A preparation method of magnetic 5-hydroxytryptophan zirconium phosphate
By preparing magnetic 5-hydroxytryptophan zirconium phosphate composite material, the problem of insufficient performance of existing adsorbents in uranium wastewater repair is solved, efficient and stable adsorption effect is achieved, and the solid-liquid separation process is simplified.
Patent Information
- Application Number
- CN202411135873.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-08-19
- Publication Date
- 2025-04-15
- Estimated Expiration
- 2044-08-19
AI Technical Summary
The prior art has problems such as insufficient adsorbent performance, low adsorption capacity, and difficulty in recycling in the repair of uranium wastewater, making it difficult to effectively repair uranium-containing wastewater.
Using a preparation method of magnetic 5-hydroxytryptophan zirconium phosphate, an adsorption material with uniform particle size, high adsorption performance and chemical stability is formed by composite processing of α-ZrP with Fe3O4 nanoparticles and 5-hydroxytryptophan zirconium phosphate.
This material has a high adsorption capacity, a wide adsorption pH range and a short adsorption time, which can efficiently repair uranium-containing wastewater, and due to its magnetic properties, solid-liquid separation is more convenient.
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Figure CN119016027B_ABST
Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of new material preparation, and specifically relates to a method for preparing magnetic 5-hydroxytryptophan zirconium phosphate. Background Art
[0002] As one of the main nuclear fuels, uranium has been widely developed and used with the widespread application of nuclear energy. However, with the development and utilization of uranium, related nuclear accidents may occur during the mining, processing and use of uranium, which will produce a large amount of uranium-containing wastewater.
[0003] Uranium has strong chemical toxicity and radioactivity, and has carcinogenic and teratogenic effects on organisms. It also has an extremely long half-life and can accumulate in organisms through the food chain. In severe cases, it can directly cause the death of organisms. Among the many methods for remediating uranium-containing wastewater, the adsorption method has attracted much attention from researchers because of its simple operation, ease of operation, and economy. The performance of the adsorbent often determines the treatment effect of the adsorption method, so it is very necessary to develop an adsorbent with a stable structure, high efficiency, large capacity, and economy.
[0004] Zirconium phosphate has a stable physical and chemical structure, is acid and alkali resistant, and has adsorption and catalytic properties similar to zeolite. However, pure zirconium phosphate is still lacking in adsorption performance, such as low adsorption capacity and difficulty in recycling. Therefore, if zirconium phosphate can be improved to increase its adsorption capacity and make it easy to recycle, and then used as an adsorption material for the remediation of uranium-containing wastewater, greater benefits will be achieved. Summary of the invention
[0005] The purpose of the present invention is to provide a method for preparing magnetic 5-hydroxytryptophan zirconium phosphate in view of the problems existing in the current prior art. The method is simple and easy to implement, and has strong repeatability. The magnetic 5-hydroxytryptophan zirconium phosphate obtained by the method has uniform particle size and can efficiently repair uranium-containing wastewater. In addition, the material also has high chemical stability, high thermal stability and acid and alkali resistance. At the same time, because the material has the indole group of 5-hydroxytryptophan, its adsorption performance is improved, and it has a wider adsorption pH range and a larger adsorption capacity, which can efficiently repair uranium-containing wastewater.
[0006] In order to achieve the above invention object, the technical solution of the present invention is as follows:
[0007] A method for preparing magnetic 5-hydroxytryptophan zirconium phosphate comprises the following steps:
[0008] S1: α-ZrP is uniformly dispersed in deionized water to obtain solution a; tris(hydroxymethyl)aminomethane solution is slowly added dropwise to solution a for pre-intercalation to obtain solution b; Fe3O4 nanoparticles are then added to solution b, and then ultrasonic and room temperature oscillation are performed in sequence to obtain solution c; finally, solution c is centrifuged, solid-liquid separation is performed, and solid is taken to obtain Fe3O4@ZrP;
[0009] S2: The Fe3O4@ZrP obtained in S1 is uniformly dispersed in deionized water, 5-hydroxytryptophan zirconium phosphate is added thereto, and solution d is obtained by shaking; the substance obtained by the reaction is washed with deionized water, and then subjected to solid-liquid separation and vacuum drying to obtain magnetic 5-hydroxytryptophan zirconium phosphate - Fe3O4@5-HTP-ZrP.
[0010] As a preferred embodiment of the present application, in step S1 of the method for preparing magnetic 5-hydroxytryptophan zirconium phosphate, the method for preparing α-ZrP has the following schemes:
[0011] The first scheme is: dissolving ZrOCl·8H2O in deionized water, slowly adding phosphoric acid solution under magnetic stirring at room temperature, washing the precipitated white solid with deionized water until neutral, separating the solid and liquid, and obtaining α-ZrP after constant temperature drying; the mass concentration of ZrOCl·8H2O dissolved in deionized water is 100g / L~1000g / L; the concentration of phosphoric acid solution is 3.4M~12M; the volume ratio of phosphoric acid solution to ZrOCl·8H2O solution is 5:1~1:5; the drying temperature is 60~85℃; the obtained α-ZrP-1 is fine particles.
[0012] The second scheme is as follows: ZrOCl·8H2O is dissolved in deionized water, phosphoric acid solution is slowly added under magnetic stirring at room temperature, the obtained mixed solution is placed in a hydrothermal reactor, and the reaction is carried out at 60-85°C for 12-24 hours. The precipitated white solid is washed with deionized water until neutral, the solid-liquid separation is carried out, and α-ZrP is obtained after constant temperature drying; the mass concentration of ZrOCl·8H2O dissolved in deionized water is 100g / L-1000g / L; the concentration of phosphoric acid solution is 3.4M-12M; the volume ratio of phosphoric acid solution to ZrOCl·8H2O solution is 5:1-1:5; the drying temperature is 60-85°C; the obtained α-ZrP-2 is fine particles.
[0013] The third scheme: dissolve ZrOCl·8H2O in deionized water, slowly add aminotrimethylenephosphonic acid solution under magnetic stirring at room temperature, stir for a certain time, place the obtained mixed solution in a hydrothermal reactor, react at 60-85°C for 12-24h, wash the precipitated white solid with deionized water until neutral, separate the solid and liquid, and dry at a constant temperature to obtain α-ZrP; the mass concentration of ZrOCl·8H2O dissolved in deionized water is 20g / L-100g / L; the concentration of the organic phosphoric acid solution is 3.4M-12M; the volume ratio of the added phosphoric acid solution to the ZrOCl·8H2O solution is 5:1-1:5; the drying temperature is 60-85°C; the obtained α-ZrP-3 is fine particles.
[0014] The fourth scheme: minimum solvent method: dissolve ZrOCl·8H2O in deionized water, slowly add a certain amount of phosphoric acid solution under room temperature magnetic stirring conditions, place the obtained mixed solution in a hydrothermal reactor, react at 60-80°C for a period of time, wash the precipitated white solid with deionized water until neutral, separate the solid and liquid, and dry at a constant temperature to obtain α-ZrP; the mass concentration of ZrOCl·8H2O dissolved in deionized water is 100g / L~1000g / L; the concentration of phosphoric acid solution is 3.4M~12M; the volume ratio of added phosphoric acid solution to ZrOCl·8H2O solution is 5:1~1:5; the drying temperature is 60~85°C; the obtained α-ZrP-4 is fine particles.
[0015] The α-ZrP obtained by the above scheme is in the form of fine particles, has a stable physical and chemical structure, is acid and alkali resistant, has ion exchange properties, and has the same adsorption and catalytic properties as zeolite.
[0016] As a preferred embodiment of the present application, in step S1 of the method for preparing magnetic 5-hydroxytryptophan zirconium phosphate, when α-ZrP is dispersed in water to form a solution, its mass concentration is 20 to 50 g / L.
[0017] As a preferred embodiment of the present application, in step S1 of the method for preparing magnetic 5-hydroxytryptophan zirconium phosphate, the concentration of tris(hydroxymethyl)aminomethane solution is 10-40 g / L; in terms of volume ratio, V α-ZrP :V Tris =3:1~1:3.
[0018] As a preferred embodiment of the present application, in step S1, stirring is required during the pre-intercalation, and the stirring time is more than 5 minutes.
[0019] As a preferred embodiment of the present application, in step S1 of the method for preparing magnetic 5-hydroxytryptophan zirconium phosphate, the amount of Fe3O4 nanoparticles added is based on the mass of Fe3O4 nanoparticles and α-ZrP, m Fe3O4 :m α-ZrP =5:1~1:5.
[0020] As a better embodiment of the present application, in step S2 of the method for preparing magnetic 5-hydroxytryptophan zirconium phosphate, the solvent of 5-hydroxytryptophan is nitrogen methyl pyrrolidone; and the concentration of 5-hydroxytryptophan is 5 g / L to 50 g / L.
[0021] In addition, the present application also protects the magnetic 5-hydroxytryptophan zirconium phosphate prepared by any of the above methods or a reasonable combination of method steps.
[0022] Thirdly, the present application also protects the use of the above-mentioned magnetic 5-hydroxytryptophan zirconium phosphate in uranium wastewater treatment.
[0023] As a better implementation in the present application, the magnetic 5-hydroxytryptophan zirconium phosphate exhibits a wider adsorption pH range and a larger adsorption capacity for uranium-containing wastewater, and the adsorption time is shorter.
[0024] Furthermore, in the treatment of uranium wastewater, the magnetic 5-hydroxytryptophan zirconium phosphate has an adsorption pH range of 3 to 8; an adsorption capacity of 642.8 mg / g; and a short adsorption time, reaching equilibrium in about 25 minutes.
[0025] The present application also provides a preferred method for preparing magnetic 5-hydroxytryptophan zirconium phosphate, which specifically comprises the following steps:
[0026] S1: 0.8 g α-ZrP was uniformly dispersed in 20 mL deionized water to obtain solution a; tris(hydroxymethyl)aminomethane solution (a solution formed by dissolving 0.4 g Tris in 20 mL deionized water) was slowly added dropwise to solution a for pre-intercalation to obtain solution b, and stirred for 5 min; then 0.8 g Fe3O4 nanoparticles were added to solution b, and then ultrasonicated for 20 min and oscillated at room temperature for 24 h to obtain solution c; finally, solution c was centrifuged and solid-liquid separated, and the solid was taken to obtain Fe3O4@ZrP;
[0027] S2: The Fe3O4@ZrP obtained in S1 was uniformly dispersed in 20 mL of deionized water, and a 5-hydroxytryptophan solution (a solution formed by dissolving 0.4 g of 5-HTP in 20 mL of NMP) was added thereto, and solution d was obtained after shaking for 24 h. The substance obtained by the reaction was washed with deionized water, and then subjected to solid-liquid separation and vacuum drying (60°C) to obtain magnetic 5-hydroxytryptophan zirconium phosphate - Fe3O4@5-HTP-ZrP.
[0028] Compared with the prior art, the present invention has the following beneficial effects:
[0029] (i) In the present application, the prepared α-ZrP is in the form of fine particles, has a stable physical and chemical structure, is acid and alkali resistant, has ion exchange properties, and has the same adsorption and catalytic properties as zeolite; it lays the foundation for the subsequent magnetic 5-hydroxytryptophan zirconium phosphate.
[0030] (ii) Tris(hydroxymethyl)aminomethane is added at this time, so that it can be used as a surfactant in this application to pre-intercalate α-ZrP and increase its interlayer spacing, thus preparing for the subsequent introduction of modified groups.
[0031] (III) In the present invention, Fe3O4 is introduced into α-ZrP, and the magnetism of Fe3O4 can be utilized to achieve solid-liquid separation of α-ZrP.
[0032] (IV) In the present invention, 5-hydroxytryptophan is used to achieve indole functionalization modification of Fe3O4@ZrP, so that it has an electron-rich group indole, thereby increasing the active sites of the material.
[0033] (V) The present invention is simple and easy to implement, and has strong repeatability. The material obtained by the present method has uniform particle size, has the common properties of zirconium phosphate layered compounds, has a stable physical and chemical structure, is acid and alkali resistant, and is suitable for the treatment of uranium-containing wastewater. It exhibits a wide adsorption pH range and a large adsorption capacity for uranium-containing wastewater, and has a short adsorption time. BRIEF DESCRIPTION OF THE DRAWINGS
[0034] Figure 1 The figure is a flow chart for preparing the magnetic 5-hydroxytryptophan zirconium phosphate in the present invention;
[0035] Figure 2 This is a sample image of α-ZrP prepared in Example 1 of the present invention;
[0036] Figure 3 This is a sample image of Fe3O4@5-HTP-ZrP-1 prepared in Example 1 of the present invention;
[0037] Figure 4 This is a graph showing the influence of different pH values on the adsorption effect of the materials prepared in Examples 1 to 4 of the present invention;
[0038] Figure 5 This is a graph showing the adsorption data of Fe3O4@5-HTP-ZrP-1 on uranium-containing wastewater over time in Example 1 of the present invention;
[0039] Figure 6This is a graph showing the adsorption data of Fe3O4@5-HTP-ZrP-1 on uranium-containing wastewater as the concentration changes in Example 1 of the present invention;
[0040] Figure 7 This is a graph showing the cyclic adsorption data of Fe3O4@5-HTP-ZrP-1 on uranium-containing wastewater in Example 1 of the present invention;
[0041] Figure 8 This is a comparison chart of the maximum adsorption capacity of uranium by α-ZrP and Fe3O4@5-HTP-ZrP-1 in Example 1 of the present invention;
[0042] Fig. 9 This is a graph showing the adsorption data of Fe3O4@5-HTP-ZrP-2 on uranium-containing wastewater over time in Example 2 of the present invention;
[0043] Fig.10 This is a graph showing the adsorption data of Fe3O4@5-HTP-ZrP-2 on uranium-containing wastewater as the concentration changes in Example 2 of the present invention;
[0044] Fig.11 This is a graph showing the adsorption data of Fe3O4@5-HTP-ZrP-3 on uranium-containing wastewater over time in Example 3 of the present invention;
[0045] Fig.12 This is a graph showing the adsorption data of Fe3O4@5-HTP-ZrP-3 on uranium-containing wastewater as the concentration changes in Example 3 of the present invention;
[0046] Fig.13 This is a graph showing the adsorption data of uranium-containing wastewater by Fe3O4@5-HTP-ZrP-4 over time in Example 4 of the present invention;
[0047] Fig.14 This is a graph showing the adsorption data of Fe3O4@5-HTP-ZrP-4 on uranium-containing wastewater as the concentration changes in Example 4 of the present invention. DETAILED DESCRIPTION
[0048] All features disclosed in this specification, or steps in all methods or processes disclosed, except mutually exclusive features and / or steps, can be combined in any manner.
[0049] Any feature disclosed in this specification (including claims and abstract), unless otherwise stated, may be replaced by other alternative features that are equivalent or have similar purposes. That is, unless otherwise stated, each feature is only an example of a series of equivalent or similar features.
[0050] The features and performance of the present invention are further described in detail below in conjunction with the embodiments.
[0051] The reagents and raw materials not specifically mentioned in the following examples are all commercially available products.
[0052] Embodiment 1:
[0053] A method for preparing magnetic 5-hydroxytryptophan zirconium phosphate specifically comprises the following steps:
[0054] S1: α-ZrP is uniformly dispersed in deionized water to form a solution a with a mass concentration of 20 g / L. Tris(hydroxymethyl)aminomethane solution is slowly added dropwise to solution a for pre-intercalation to obtain solution b, and Fe3O4 nanoparticles are added to solution b, ultrasonicated for 20 min, oscillated at room temperature for 12 h, centrifuged, separated solid and liquid, and the solid was taken to obtain Fe3O4@ZrP;
[0055] The preparation method of α-ZrP is as follows: accurately weigh 16g ZrOCl·8H2O and dissolve it in 50mL deionized water; slowly add 50mL 3.4M phosphoric acid solution under magnetic stirring at room temperature; separate the precipitated white solid by solid-liquid separation and dry it at a constant temperature of 60°C to obtain α-ZrP.
[0056] The concentration of the added tris(hydroxymethyl)aminomethane solution is 20 g / L, V α-ZrP :V Tris =2:1.
[0057] Fe3O4 nanoparticle addition amount: the mass ratio of Fe3O4 nanoparticles to α-ZrP is 1:1; that is, m Fe3O4 :m α-ZrP =1:1.
[0058] S2: All the Fe3O4@ZrP obtained in S1 was evenly dispersed in 20 mL of deionized water, 10 mL of 5-hydroxytryptophan solution was added thereto, and the mixture was shaken for 24 h. The mixture was first washed with acetone, and then washed with deionized water until the acetone was clean and the washing filtrate was close to neutral. The mixture was separated into solid and liquid, and dried under vacuum at 60 °C to obtain magnetic 5-hydroxytryptophan zirconium phosphate - Fe3O4@5-HTP-ZrP-1 (such as Figure 3 shown).
[0059] The concentration of 5-hydroxytryptophan solution is 20 g / L; the preparation method is: accurately weigh 5-hydroxytryptophan and dissolve it in nitrogen-methylpyrrolidone.
[0060] The adsorption data of Fe3O4@5-HTP-ZrP-1 on uranium-containing wastewater are as follows Figure 4-7As shown in the figure, its optimum pH is 3-8, the maximum adsorption capacity is 642.8 mg / g, and the adsorption equilibrium is reached in 25 minutes; after 4 adsorption-desorption cycles, the removal rate of Fe3O4@5-HTP-ZrP-1 for 10 mg / L uranium solution can still reach 70%, and it has good adsorption performance for uranium. The maximum adsorption capacity of α-ZrP and Fe3O4@5-HTP-ZrP-1 for uranium obtained from S1 is shown in Figure 8 As shown, the adsorption performance of the modified magnetic 5-hydroxytryptophan zirconium phosphate is significantly improved; at the same time, the material has magnetism, and using it for the remediation of uranium-containing wastewater will bring huge benefits.
[0061] Embodiment 2:
[0062] A method for preparing magnetic 5-hydroxytryptophan zirconium phosphate specifically comprises the following steps:
[0063] S1: Disperse α-ZrP uniformly in deionized water to form a solution a with a mass concentration of 20 g / L. Slowly drop tris(hydroxymethyl)aminomethane solution into solution a for pre-intercalation, with a stirring time of 6 min during pre-intercalation; add Fe3O4 nanoparticles, ultrasonicate for 20 min, oscillate at room temperature for 12 h, centrifuge, separate solid and liquid, and take the solid to obtain Fe3O4@ZrP;
[0064] The preparation method of α-ZrP is as follows: accurately weigh 1g ZrOCl·8H2O and dissolve it in 10mL deionized water; slowly add 4mL concentrated phosphoric acid solution under room temperature magnetic stirring; place it in a hydrothermal kettle at 75°C for 24h to obtain a white solid; wash it with deionized water until it is neutral; separate the solid from the liquid; and dry it at a constant temperature of 60°C to obtain α-ZrP.
[0065] The concentration of the added tris(hydroxymethyl)aminomethane solution is 20 g / L, V α-ZrP :V Tris =2:1.
[0066] Fe3O4 nanoparticle addition amount: the mass ratio of Fe3O4 nanoparticles to α-ZrP is 1:1; that is, m Fe3O4 :m α-ZrP =1:1.
[0067] S2: All the Fe3O4@ZrP obtained in S1 was evenly dispersed in 20 mL of deionized water, and 10 mL of 5-hydroxytryptophan solution was added thereto. The mixture was shaken for 24 h, and then washed with acetone. The acetone was washed clean with deionized water and the washing filtrate was nearly neutral. The mixture was separated from the solid and the liquid was dried under vacuum at 60 °C to obtain magnetic 5-hydroxytryptophan zirconium phosphate - Fe3O4@5-HTP-ZrP-2.
[0068] The concentration of 5-hydroxytryptophan solution is 20 g / L; the preparation method is: accurately weigh 5-hydroxytryptophan and dissolve it in nitrogen-methylpyrrolidone.
[0069] The adsorption data of Fe3O4@5-HTP-ZrP-2 on uranium-containing wastewater are as follows Figure 4 , Figure 9-10 As shown in the figure, it can be seen that the optimal pH is 7, the maximum adsorption capacity is 127.2 mg / g, and the adsorption equilibrium is reached in 10 minutes.
[0070] Embodiment 3:
[0071] A method for preparing magnetic 5-hydroxytryptophan zirconium phosphate specifically comprises the following steps:
[0072] S1: Disperse α-ZrP uniformly in deionized water to obtain solution a with a mass concentration of 20 g / L. Slowly add tris(hydroxymethyl)aminomethane solution to solution a to form solution b, and perform pre-intercalation for 7 min. Add Fe3O4 nanoparticles, perform ultrasound for 20 min, and oscillate at room temperature for 24 h to obtain solution c. Centrifuge solution c to separate the solid and liquid, and take the solid to obtain Fe3O4@ZrP.
[0073] The preparation method of α-ZrP is as follows: 1 mL of aminotrimethylenephosphonic acid (ATMPA) is dissolved in 120 ml of deionized water, and the mixture is fully mixed and stirred for 2 h; 0.76 g of ZrOCl·8H2O is accurately weighed and dissolved in 30 mL of deionized water, and 120 mL of aminotrimethylenephosphonic acid solution is slowly added under magnetic stirring at room temperature. The precipitated white solid is washed with deionized water until it is neutral, and α-ZrP is obtained after solid-liquid separation and constant temperature drying at 60°C.
[0074] The concentration of the added tris(hydroxymethyl)aminomethane solution is 20 g / L, V α-ZrP :V Tris =2:1. Fe3O4 nanoparticle addition amount: the mass ratio of Fe3O4 nanoparticles to α-ZrP is 1:1; that is, m Fe3O4 :m α-ZrP =1:1.
[0075] S2: All the Fe3O4@ZrP obtained in S1 was evenly dispersed in 20 mL of deionized water to obtain solution d. 10 mL of 5-hydroxytryptophan solution was added to solution d, shaken for 24 h, washed with deionized water for several times, separated the solid and liquid, and dried under vacuum at 60 °C to obtain magnetic 5-hydroxytryptophan zirconium phosphate - Fe3O4@5-HTP-ZrP-3.
[0076] The concentration of 5-hydroxytryptophan solution is 20 g / L; the preparation method is: accurately weigh 5-hydroxytryptophan and dissolve it in nitrogen-methylpyrrolidone.
[0077] The adsorption data of Fe3O4@5-HTP-ZrP-3 on uranium-containing wastewater are as follows Figure 4 , Figure 11-12 As shown in the figure, it can be seen that the optimal pH is 5-6, the maximum adsorption capacity is 127.2 mg / g, and the adsorption equilibrium is reached in 90 minutes.
[0078] Embodiment 4:
[0079] A method for preparing magnetic 5-hydroxytryptophan zirconium phosphate specifically comprises the following steps:
[0080] S1: α-ZrP was uniformly dispersed in deionized water with a mass concentration of 20 g / L. Tris(hydroxymethyl)aminomethane solution was slowly added dropwise for pre-intercalation, and Fe3O4 nanoparticles were added. Ultrasonic treatment was performed for 20 min, and oscillation was performed at room temperature for 12 h. Centrifugation was performed for solid-liquid separation, and the solid was obtained to obtain Fe3O4@ZrP.
[0081] The preparation method of α-ZrP is as follows: accurately weigh 4.83g ZrOCl·8H2O and dissolve it in a certain amount of deionized water; slowly add a certain amount of concentrated phosphoric acid solution under room temperature magnetic stirring conditions; react at 80°C for 24h to obtain a white solid; wash the white solid with deionized water to neutrality; separate the solid from the liquid; and dry at 60°C to obtain α-ZrP.
[0082] The concentration of the added tris(hydroxymethyl)aminomethane solution is 20 g / L, V α-ZrP :V Tris =2:1.
[0083] Fe3O4 nanoparticle addition amount: the mass ratio of Fe3O4 nanoparticles to α-ZrP is 1:1; that is, m Fe3O4 :m α-ZrP =1:1.
[0084] S2: The Fe3O4@ZrP obtained in S1 was uniformly dispersed in deionized water, 10 mL of 5-hydroxytryptophan solution was added thereto, shaken for 24 h, washed with deionized water for several times, separated the solid and the liquid, and dried under vacuum at 60°C to obtain magnetic 5-hydroxytryptophan zirconium phosphate - Fe3O4@5-HTP-ZrP-4.
[0085] The concentration of 5-hydroxytryptophan solution is 20 g / L; the preparation method is: accurately weigh 5-hydroxytryptophan and dissolve it in nitrogen-methylpyrrolidone.
[0086] The adsorption data of Fe3O4@5-HTP-ZrP-4 on uranium-containing wastewater are as follows Figure 4 , Figure 13-14As shown in the figure, it can be seen that the optimal pH is 7, the maximum adsorption capacity is 64.9 mg / g, and the adsorption equilibrium is reached in 30 minutes.
[0087] The above-mentioned embodiments only express the specific implementation methods of the present application, and the descriptions thereof are relatively specific and detailed, but they cannot be understood as limiting the protection scope of the present application. It should be pointed out that, for ordinary technicians in this field, several variations and improvements can be made without departing from the technical solution concept of the present application, and these all belong to the protection scope of the present application.
[0088] This background section is provided to generally present the context of the invention, and the work of the presently named inventors, the work to the extent described in this background section, and aspects of this section that did not constitute prior art at the time of application are neither explicitly nor implicitly admitted to be prior art to the present invention.
Claims
1. A method for preparing magnetic 5-hydroxytryptophan zirconium phosphate, characterized in that: The following steps are involved: S1: Disperse α-ZrP uniformly in deionized water to obtain solution a; Slowly drop tris(hydroxymethyl)aminomethane solution into solution a for pre-intercalation to obtain solution b; then add Fe3O4 nanoparticles into solution b, and then successively subject to ultrasound and room temperature oscillation to obtain solution c; finally, centrifuge solution c, perform solid-liquid separation, and take solid to obtain Fe3O4@ZrP; S2: The Fe3O4@ZrP obtained in S1 is uniformly dispersed in deionized water, and 5-hydroxytryptophan solution is added thereto, and the mixture is shaken; the substance obtained by the reaction is washed with deionized water, and then subjected to solid-liquid separation and vacuum drying to obtain magnetic 5-hydroxytryptophan zirconium phosphate Fe3O4@5-HTP-ZrP.
2. The method for preparing magnetic 5-hydroxytryptophan zirconium phosphate according to claim 1, characterized in that: In step S1, α-ZrP is dispersed in deionized water to form a solution with a mass concentration of 20 to 50 g / L.
3. The method for preparing the magnetic 5-hydroxytryptophan zirconium phosphate according to claim 1 or 2, characterized in that: In step S1, the concentration of the tris(hydroxymethyl)aminomethane solution is 10-40 g / L; in terms of volume ratio, V α-ZrP :V Tris =3:1~1:
3.
4. The method for preparing magnetic 5-hydroxytryptophan zirconium phosphate according to claim 3, characterized in that: In step S1, stirring is required during the pre-intercalation, and the stirring time is more than 5 minutes.
5. The method for preparing the magnetic 5-hydroxytryptophan zirconium phosphate according to claim 1, 2 or 4, characterized in that: In step S1, the amount of Fe3O4 nanoparticles added is measured by mass, m Fe3O4 :m α-ZrP =5:1~1:
5.
6. The method for preparing a magnetic 5-hydroxytryptophan zirconium phosphate according to claim 5, characterized in that In step S2, the solvent of 5-hydroxytryptophan is N-methylpyrrolidone; the concentration of 5-hydroxytryptophan is 10 g / L to 50 g / L.
7. The magnetic 5-hydroxytryptophan zirconium phosphate obtained according to the method of claim 1, 2, 4 or 6.
8. Use of the magnetic 5-hydroxytryptophan zirconium phosphate according to claim 7 in uranium wastewater treatment.
Citation Information
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