CN116425135A - Ferric hydroxide modified sodium zirconium phosphate and preparation method and application thereof - Google Patents

Ferric hydroxide modified sodium zirconium phosphate and preparation method and application thereof Download PDF

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CN116425135A
CN116425135A CN202310466706.6A CN202310466706A CN116425135A CN 116425135 A CN116425135 A CN 116425135A CN 202310466706 A CN202310466706 A CN 202310466706A CN 116425135 A CN116425135 A CN 116425135A
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nahzr
feooh
adsorption
mixture
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刘军
王静
王广西
罗茂丹
舒俊翔
李超
王成
桂兵涛
常茂远
陈豪
黄雪晨
沈文晖
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Chengdu Univeristy of Technology
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
    • B01J20/048—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing phosphorus, e.g. phosphates, apatites, hydroxyapatites
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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    • C01B25/26—Phosphates
    • C01B25/37—Phosphates of heavy metals
    • C01B25/372—Phosphates of heavy metals of titanium, vanadium, zirconium, niobium, hafnium or tantalum
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    • C01—INORGANIC CHEMISTRY
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    • C01G49/00—Compounds of iron
    • C01G49/02—Oxides; Hydroxides
    • C01G49/06—Ferric oxide [Fe2O3]
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00—Treatment of water, waste water, or sewage
    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
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    • C01P2004/03—Particle morphology depicted by an image obtained by SEM

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Abstract

The invention discloses a ferric hydroxide modified sodium zirconium phosphate (FeOOH-NaHZr (PO) 4 ) 2 ·H 2 O) and preparation method and application thereof, feCl 3 ·6H 2 O, naOH and NaHZr (PO) 4 ) 2 ·H 2 O is added into a polytetrafluoroethylene lining together, ultrapure water is added and stirred on a magnetic stirrer, and then the lining is added into a stainless steel reaction kettle and put into an oven for high-temperature reaction. Cooling to room temperatureAnd then, centrifuging the sample in a high-speed centrifuge, washing twice with ultrapure water after finishing, and drying, grinding and sieving the obtained sample to obtain the sample. The invention synthesizes the novel adsorbent FeOOH-NaHZr (PO) by the first one-pot method 4 ) 2 ·H 2 And O, the adsorbent has excellent adsorption activity, and a certain information reference is provided for the treatment of nuclides in the real environment.

Description

Ferric hydroxide modified sodium zirconium phosphate and preparation method and application thereof
Technical Field
The invention belongs to the technical field of radioactive wastewater treatment, and particularly relates to iron oxyhydroxide modified sodium zirconium phosphate and a preparation method and application thereof.
Background
Compared with traditional fossil fuels, nuclear energy has the advantages of low carbon, low pollution and extremely high power density, and has been widely used worldwide. With the rapid development of nuclear power, radioactive liquid wastewater is inevitably generated in the spent fuel circulation process. 60 Co is one of the important radioactive by-product metal ions of radioactive wastewater, and can cause serious threat to human health through migration of surface water and groundwater, such as lung hypofunction, mutation, paralysis, bone defect and the like, and can have harmful influence on ecological environment. Therefore, the extraction of cobalt ions from wastewater solutions is extremely important。
Zirconium phosphate (ZrP) has attracted considerable attention as a potential adsorbent. The method has the advantages that not only can the abundant space layers be changed, the target metal can be conveniently removed from the wastewater, the acid, alkali, radiation and heat stability are excellent, but also protons in the phosphate group can be easily replaced by other cations. ZrP has been applied to treat Cs + 、Cu 2+ Radioactive waste water of plasma. But the adsorption capacity for radionuclides is low due to the lack of porous structures or interlayer spaces.
The iron oxyhydroxide (FeOOH) has rich surface hydroxyl functional groups, more active sites, environmental friendliness, rich resources, special structure and easy adsorption, and is an excellent adsorbent. With the change of pH value, the hydroxyl functional group on the surface of FeOOH can change to form-OH 2+ (OH) or-O - . As radionuclides such As As (V), cr (VI), se (IV), etc., when the radionuclides are present As anions, the-OH of FeOOH 2+ Positively charged functional groups will be attracted by electrostatic attraction. However, feOOH itself has limited active sites, and nanoparticles thereof are agglomerated under certain conditions, resulting in a decrease in adsorption capacity. The improvement of the specific surface area, charge distribution and other adsorption properties of the FeOOH complex has important significance for Co (II) adsorption.
Based on the analysis, a zirconium phosphate adsorbent with better radionuclide adsorption capability is urgently needed in the industry at present.
Disclosure of Invention
In order to solve the problems, the invention synthesizes the novel adsorbent FeOOH modified NaHZr (PO) 4 ) 2 ·H 2 O, the adsorbent has excellent adsorption activity. Scheme 1 shows that the catalyst is prepared by reacting a catalyst with NaHZr (PO 4 ) 2 ·H 2 In-situ growth of FeOOH on O, and one-pot synthesis of FeOOH-NaHZr (PO) 4 ) 2 ·H 2 O. And the morphology and the like of the nanocomposite are characterized and researched. Subsequently, the adsorption of Co (II) on the nanocomposite under different factors was studied, and the reuse and formation after Co (II) adsorption was studied. The results show that the synthesized nanocomposite material does notThe method is a good Co (II) ion adsorption material, and provides a certain information reference for the treatment of nuclides in a real environment. The invention is realized by the following technical means:
the invention firstly discloses a preparation method of ferric hydroxide modified sodium zirconium phosphate, which comprises the following steps:
(1) FeCl is added 3 ·6H 2 O, naOH and NaHZr (PO) 4 ) 2 ·H 2 Adding O together into a polytetrafluoroethylene lining, adding ultrapure water and stirring on a magnetic stirrer to obtain a first mixture;
(2) Placing the first mixture into a stainless steel reaction kettle, placing the stainless steel reaction kettle into an oven for high-temperature reaction, and cooling the stainless steel reaction kettle to room temperature to obtain a second mixture;
(3) Centrifuging the second mixture in a high-speed centrifuge, and then washing twice with ultrapure water to obtain a third mixture;
(4) And grinding and sieving the third mixture after vacuum drying to obtain the ferric hydroxide modified sodium zirconium phosphate.
Further, the FeCl in the step (1) 3 ·6H 2 O, naOH and NaHZr (PO) 4 ) 2 ·H 2 The mass ratio of O is 1.5028:2:3.23.
Further, the amount of ultrapure water used in the step (1) is 80mL, and the stirring time is 30min.
Further, the drying condition of the oven in the step (2) is 433K, and the reaction is carried out for 12 hours.
Further, the processing conditions of the high-speed centrifuge in the step (3) are as follows: rotational speed 10000rpm, centrifugation time 5min.
Further, the vacuum drying conditions in the step (4) are as follows: drying temperature 333K, drying time 24h.
Further, the sieving particle size in the step (4) is 60 meshes.
The invention also discloses FeOOH-NaHZr (PO) prepared by the preparation method 4 ) 2 ·H 2 O。
The invention also discloses a method for preparing the FeOOH-NaHZr (PO) 4 ) 2 ·H 2 O is in wasteUse in water treatment.
Further, the wastewater is radioactive liquid wastewater.
The invention has the beneficial effects that:
1. the invention adopts a one-pot method to synthesize the iron oxyhydroxide modified sodium zirconium phosphate (FeOOH-NaHZr (PO) 4 ) 2 ·H 2 O) adsorbing material, the synthetic route is simple and environment-friendly, and excessive use of phosphoric acid and zirconium chloride is avoided, so that adverse effects of reactant loss, scattering and volatilizing of harmful medicines and the like generated in the multi-step synthetic method are reduced.
2. The raw material sodium zirconium phosphate used in the present invention (NaHZr (PO) 4 ) 2 ·H 2 O) can be purchased from related companies, has low cost and high environmental protection benefit, and has lower cost as a whole than multi-step synthesis. The method not only finds a way for the sales of sodium zirconium phosphate of companies, but also can be applied to the removal of nuclides in various waste liquids, and has multiple purposes.
Drawings
FIG. 1 is a synthetic route diagram of the iron oxyhydroxide-modified sodium zirconium phosphate of the present invention.
FIG. 2 shows pH vs. NaHZr (PO 4 ) 2 ·H 2 O、FeOOH-NaHZr(PO 4 ) 2 ·H 2 The effect of the adsorption of cobalt ions by O.
FIG. 3 is a graph of time versus NaHZr (PO) 4 ) 2 ·H 2 O、FeOOH-NaHZr(PO 4 ) 2 ·H 2 The effect of the adsorption of cobalt ions by O.
FIG. 4 is a graph of time versus NaHZr (PO) 4 ) 2 ·H 2 O、FeOOH-NaHZr(PO 4 ) 2 ·H 2 The effect of the adsorption of cobalt ions by O.
FIG. 5 shows temperature versus NaHZr (PO) 4 ) 2 ·H 2 O、FeOOH-NaHZr(PO 4 ) 2 ·H 2 The effect of the adsorption of cobalt ions by O.
FIG. 6 shows the effect of re-adsorption after eluting with different eluents.
FIG. 7 adsorption of cobalt by the adsorbent after various cycles.
FIG. 8 is a sample scanning electron microscope image; wherein (a) and (c) areNaHZr(PO 4 ) 2 ·H 2 O, (b) and (d) are FeOOH-NaHZr (PO) 4 ) 2 ·H 2 O. (a) and (b) represent one cycle, and (c) and (d) represent ten cycles.
Detailed Description
In order that the above objects, features and advantages of the invention will be readily understood, a more particular description of the invention will be rendered by reference to the appended drawings. The following is merely illustrative and explanatory of the principles of the invention, as various modifications and additions may be made to the specific embodiments described, or similar thereto, by those skilled in the art, without departing from the principles of the invention or beyond the scope of the appended claims.
The experimental procedure used in the examples below was a solvothermal synthesis; the experimental reagents, materials, etc. used in the examples described below are commercially available unless otherwise specified.
Example 1
In connection with the synthetic route of fig. 1, example 1 provides a method for preparing iron oxyhydroxide-modified sodium zirconium phosphate, comprising the steps of:
1.5028g FeCl 3 ·6H 2 O,2g NaOH and 3.23g NaHZr (PO) 4 ) 2 ·H 2 O was added together to 100mL of the inner liner of polytetrafluoroethylene, followed by 80mL of ultrapure water, and stirred on a magnetic stirrer for 30 minutes, and then the inner liner was added to a stainless steel reaction vessel, and placed in an oven, and reacted at 433K for 12 hours. Cooling to room temperature, centrifuging in a high-speed centrifuge at 10000rpm for 5min, washing the centrifuged sample with 80mL of ultrapure water twice, drying the obtained sample in 333K vacuum drying oven for 24 hr, grinding the dried sample, and sieving with 60 mesh sieve to obtain powder which is ferric hydroxide modified sodium zirconium phosphate (FeOOH-NaHZr (PO) 4 ) 2 ·H 2 O)。
Test example 1
Based on the exact same chemical properties of the Co isotopes, the present invention uses non-radioactive 59 Co asIs that 60 Alternatives to Co. The experimental procedure was as follows:
under normal temperature, 10mg of FeOOH-NaHZr (PO) 4 ) 2 ·H 2 O and NaHZr (PO) 4 ) 2 ·H 2 O was added separately to 100mL Erlenmeyer flasks. Next, 50mL of the Co (II) solution of the desired concentration was transferred to the bottle. Then, the bottles were placed in a water bath constant temperature shaking box at 150rpm for shaking adsorption. In addition, the influence of factors such as initial solution pH, contact time, initial Co (II) concentration, temperature and reusability was examined by the same method. By HNO 3 And NaOH solution to adjust the pH value of Co (II) ion solution. After shaking for several hours, 1mL of supernatant was taken to measure the remaining Co (II) concentration and the lower precipitate was dried for characterization analysis. The initial, residual and equilibrium concentrations of Co (II) were determined using an ultraviolet 752 spectrophotometer. Briefly, 1mL of supernatant, 4mL of HAc-NaAc solution (ph=5.5) and 5mL of xylenol orange solution (0.25 mg/mL) were added to a 25mL volumetric flask, and then the volume was fixed with ultrapure water. Co (II) concentration was measured on an ultraviolet 752 spectrophotometer at a wavelength of 581 nm.
NaHZr(PO 4 ) 2 ·H 2 O、FeOOH-NaHZr(PO 4 ) 2 ·H 2 Adsorption quantity q of O to Co (II) e (Eq. (1)) the calculation formula is as follows:
Figure BDA0004202494550000041
wherein q is e Mg/g, C O And C e The initial concentration and equilibrium concentration (mg/L) of the Co (II) solution, respectively. V is the volume of the solution (mL), m is the adsorbent dosage (g).
(1) Influence of initial pH
NaHZr (PO) at pH 2-13 was examined with 50mL of Co (II) solution and 10mg or more of the adsorbent under 298K 4 ) 2 ·H 2 O、FeOOH-NaHZr(PO 4 ) 2 ·H 2 Influence of O on Co (II) ion adsorption. As shown in FIG. 2, the adsorption amount of cobalt gradually increases with the increase of pH, but when the pH is greater than8.5, cobalt ions start to hydrolyze and precipitate, so that at pH=8, the Co (II) concentration is 50mg/L, and the adsorption amounts of the cobalt ions and the Co (II) are about 60 mg/g and 90mg/g, respectively.
(2) Influence of contact time
Contact time vs. NaHZr (PO) 4 ) 2 ·H 2 O and FeOOH-NaHZr (PO) 4 ) 2 ·H 2 The effect of O is shown in FIG. 3. As can be seen from fig. 3, the adsorption amount of Co (II) by both adsorbents increases rapidly from the first few hours to 24 hours, because many adsorption sites of the adsorbents can be occupied by Co (II) during this period, almost equilibrium is reached at 24 hours, and the adsorption of Co (II) does not significantly change from 24 hours to 72 hours. Over time, the sites for adsorption of Co (II) decrease. Therefore, in subsequent experiments, we selected the optimal t=24 h. With NaHZr (PO) 4 ) 2 ·H 2 O compared with FeOOH-NaHZr (PO 4 ) 2 ·H 2 The adsorption rate of O is faster because the latter has a variety of structures and more adsorption sites.
(3) Influence of initial cobalt ion concentration on adsorption
NaHZr(PO 4 ) 2 ·H 2 O、FeOOH-NaHZr(PO 4 ) 2 ·H 2 Co (II) adsorption of O to various initial concentrations is shown in FIG. 4, and the results indicate that NaHZr (PO 4 ) 2 ·H 2 O、FeOOH-NaHZr(PO 4 ) 2 ·H 2 The adsorption capacity (qe equilibrium adsorption amount) of O and Co (II) increases with the initial concentration of Co (II), and the maximum q of Co (II) is 60mg/L e The values were about 70mg/g and 97mg/g, respectively.
(4) Influence of temperature on adsorption
Temperature vs. NaHZr (PO) 4 ) 2 ·H 2 O、FeOOH-NaHZr(PO 4 ) 2 ·H 2 The effect of O on Co (II) adsorption is shown in FIG. 5. As can be seen from the results of FIG. 5, from 288K to 318K, co (II) is found in NaHZr (PO 4 ) 2 ·H 2 O and FeOOH-NaHZr (PO) 4 ) 2 ·H 2 The amount of adsorption on O increases significantly with increasing temperature. Indicating that the adsorption of the cobalt by the two adsorbents is endothermic. As the temperature increases from 298K to 318K, the adsorption of cobalt increases by about 20mg/g. The subsequent experimental temperature was chosen to be 298K, considering that continued operation at high temperatures would result in unnecessary energy loss without significant increase in adsorption capacity.
Test example 2
Whether the adsorbent can be repeatedly used has great significance in practical application. In this work, different solvents, e.g. HCl, naCl, naHCO 3 ，CH 3 COOH and NaOH solutions were used for elution as shown in table 1.
The reusability study of Co (II) was performed as follows:
first, a Co (II) adsorption experiment was performed, the residual Co (II) concentration was detected 24h after adsorption equilibrium, and all precipitates were retained after centrifugation. 50mL of HCl, naCl, naHCO at various concentrations were then added 3 ，CH 3 The COOH and NaOH solutions were added to a 100mL Erlenmeyer flask, and the above precipitate was added to the eluate and shaken with shaking for 24h, respectively. The adsorption capacity of the different eluents after two cycle times is shown in figure 6. The results show that other eluents besides NaOH solution have little regeneration capacity for the adsorbent. As a result, the optimal eluent was a NaOH solution of 0.2 mol/L. Co (II) is adsorbed on FeOOH-NaHZr (PO) 4 ) 2 ·H 2 O and NaHZr (PO) 4 ) 2 ·H 2 As shown in fig. 7, the repeated adsorption study on O shows that the adsorption capacity of both adsorbents did not significantly decrease after ten cycles. The scanning electron microscope of fig. 8 shows that the surface morphology of the samples (a and b) after one adsorption and the samples (c and d) after the corresponding ten elution and adsorption is not greatly changed, and the electron microscope result shows that the surface of the sample after ten adsorption has no change except that the particles become compact from dispersion, which is probably because the material can withstand proper alkalinity and has a stable substance structure.
TABLE 1 major eluent in the regeneration study
Eluent Concentration (mol/L)
HCl 0.1
NaCl 0.1
NaHCO 3 0.1
CH 3 COOH 0.1
NaOH 0.1 and 0.2
In conclusion, the invention synthesizes a novel mesoporous FeOOH-NaHZr (PO 4) for the first time 2 ·H 2 O nanocomposite. Batch experiments on factors such as contact time, temperature, initial cobalt concentration and initial pH are carried out, and the results show that NaHZr (PO) 4 ) 2 ·H 2 O and NaHZr (PO) 4 ) 2 ·H 2 The maximum adsorption amount of O to Co (II) is 65+ -5 mg/g and 95+ -5 mg/g respectively. The adsorption of Co (II) by the two adsorbents is spontaneous endothermic adsorption, and belongs to quasi-secondary chemical adsorption. Next, naHZr (PO) after 10 regeneration cycles 4 ) 2 ·H 2 O and FeOOH-NaHZr (PO) 4 ) 2 ·H 2 O still maintains excellent adsorption performance. The research of the invention shows that NaHZr (PO 4 ) 2 ·H 2 O and FeOOH-NaHZr (PO) 4 ) 2 ·H 2 O can efficiently adsorb Co (II) in aqueous solution, and FeOOH-NaHZr (PO) is synthesized by one-pot method 4 ) 2 ·H 2 O can provide reference information for treating radionuclides such as cobalt (II) in actual nuclear wastewater.

Claims (10)

1. FeOOH-NaHZr (PO 4 ) 2 ·H 2 The preparation method of O comprises the following steps:
(1) FeCl is added 3 ·6H 2 O, naOH and NaHZr (PO) 4 ) 2 ·H 2 Adding O together into a polytetrafluoroethylene lining, adding ultrapure water and stirring on a magnetic stirrer to obtain a first mixture;
(2) Placing the first mixture into a stainless steel reaction kettle, placing the stainless steel reaction kettle into an oven for high-temperature reaction, and obtaining a second mixture after the reaction kettle is cooled to room temperature;
(3) Centrifuging the second mixture in a high-speed centrifuge, and then washing twice with ultrapure water to obtain a third mixture;
(4) Vacuum drying the third mixture, grinding, and sieving to obtain FeOOH-NaHZr (PO) 4 ) 2 ·H 2 O。
2. The method of manufacturing according to claim 1, wherein:
step (1) the FeCl 3 ·6H 2 O, naOH and NaHZr (PO) 4 ) 2 ·H 2 The mass ratio of O is 1.5028:2:3.23.
3. The method of manufacturing according to claim 1, wherein:
the dosage of the ultrapure water in the step (1) is 80mL, and the stirring time is 30min.
4. The method of manufacturing according to claim 1, wherein:
the drying conditions of the oven in the step (2) are as follows: the reaction is carried out for 12h at 433K.
5. The method of manufacturing according to claim 1, wherein:
the processing conditions of the high-speed centrifuge in the step (3) are as follows: rotational speed 10000rpm, centrifugation time 5min.
6. The method of manufacturing according to claim 1, wherein:
the vacuum drying conditions in the step (4) are as follows: drying temperature 333K, drying time 24h.
7. The method of manufacturing according to claim 1, wherein:
and (3) sieving the powder in the step (4) to obtain the powder with the particle size of 60 meshes.
8. FeOOH-NaHZr (PO) prepared by the preparation method according to any one of claims 1 to 7 4 ) 2 ·H 2 O。
9. A FeOOH-NaHZr (PO) according to claim 8 4 ) 2 ·H 2 O is applied to wastewater treatment.
10. The use of claim 9, wherein: the waste water is radioactive liquid waste water.
CN202310466706.6A 2023-04-27 2023-04-27 Ferric hydroxide modified sodium zirconium phosphate and preparation method and application thereof Pending CN116425135A (en)

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Citations (3)

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Publication number Priority date Publication date Assignee Title
US7052532B1 (en) * 2000-03-09 2006-05-30 3M Innovative Properties Company High temperature nanofilter, system and method
CN101970099A (en) * 2008-01-31 2011-02-09 协和化学工业株式会社 Selective adsorbent material, and method for production thereof
CN110024202A (en) * 2016-12-02 2019-07-16 旭化成株式会社 Nonaqueous electrolyte battery inorganic particle

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US7052532B1 (en) * 2000-03-09 2006-05-30 3M Innovative Properties Company High temperature nanofilter, system and method
CN101970099A (en) * 2008-01-31 2011-02-09 协和化学工业株式会社 Selective adsorbent material, and method for production thereof
CN110024202A (en) * 2016-12-02 2019-07-16 旭化成株式会社 Nonaqueous electrolyte battery inorganic particle

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
曾光石 等: "磁记录材料锶、钡铁氧体的穆斯堡尔研究", 华中科技大学学报(自然科学版), vol. 18, no. 03, 30 March 1990 (1990-03-30), pages 97 - 101 *

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