CN114797771A - Composite adsorption material for removing arsenic in water and preparation method thereof - Google Patents

Composite adsorption material for removing arsenic in water and preparation method thereof Download PDF

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Publication number
CN114797771A
CN114797771A CN202210359543.7A CN202210359543A CN114797771A CN 114797771 A CN114797771 A CN 114797771A CN 202210359543 A CN202210359543 A CN 202210359543A CN 114797771 A CN114797771 A CN 114797771A
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arsenic
hzo
water
composite
adsorbing material
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辛永光
谭平
欧宏森
陈惠婷
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Guangdong Xintailong Environmental Protection Group Co ltd
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Guangdong Xintailong Environmental Protection Group Co ltd
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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
    • B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
    • 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
    • B01J20/06—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
    • 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
    • B01J20/30—Processes for preparing, regenerating, or reactivating
    • B01J20/34—Regenerating or reactivating
    • B01J20/345—Regenerating or reactivating using a particular desorbing compound or mixture
    • B01J20/3475—Regenerating or reactivating using a particular desorbing compound or mixture in the liquid phase
    • 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
    • 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
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/42—Materials comprising a mixture of inorganic materials
    • 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
    • B01J2220/00—Aspects relating to sorbent materials
    • B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
    • B01J2220/48—Sorbents characterised by the starting material used for their preparation
    • B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/103—Arsenic compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2303/00—Specific treatment goals
    • C02F2303/16—Regeneration of sorbents, filters

Abstract

The invention discloses a composite adsorption material for removing arsenic in water and a preparation method thereof. The composite adsorbing material for removing arsenic from water is synthesized, the composite adsorbing material is composed of Hydrated Zirconia (HZO) and Graphene Oxide (GO), the efficient removal of arsenic is enhanced by the synergistic removal effect of GO and HZO in the composite adsorbing material on arsenic, namely the inner layer complexing ability of HZO on arsenic is enhanced by hydrogen bonds generated by GO on arsenic, so that the adsorption capacity of the HZO/GO composite material on arsenic is higher than the sum of the adsorption capacity of single GO or HZO on arsenic and the adsorption capacity of HZO and GO on arsenic. Meanwhile, the HZO/GO composite material has good regeneration capacity for arsenic, and the adsorption capacity of the HZO/GO composite material is only slightly reduced after circulation for a plurality of times, so that the HZO/GO composite material has a higher application prospect and a higher popularization value.

Description

Composite adsorption material for removing arsenic in water and preparation method thereof
Technical Field
The invention relates to the technical field of water treatment, in particular to a composite adsorption material for removing arsenic in water and a preparation method thereof.
Background
The pollution of high-toxicity arsenic in water bodies is a worldwide problem troubling human beings, the pollution can be accumulated in human bodies, irreversible damage can be caused to human organs, and the high-efficiency removal of the arsenic in the water bodies is vital to human health. At present, the adsorption method for removing arsenic is widely used due to the characteristics of simple operation, economy, effectiveness and the like. For this reason, various transition metal hydroxides have been developed for arsenic removal in water bodies, such as fe (iii), zr (iv), la (iii), cu (ii), and exhibit strong affinity for arsenic. Among them, Hydrous Zirconia (HZO) is widely used for removing arsenic in water because of its advantages of low cost, no toxicity, strong stability, strong corrosion resistance, etc. However, HZO is easily agglomerated in the adsorption system, resulting in a low arsenic adsorption capacity of HZO. The adsorption capacity is influenced by a plurality of factors such as the specific surface area, the dispersity and the functional group of the adsorbent. In recent years, researchers have utilized synergistic adsorption strategies of complex and hydrogen bonds to achieve efficient removal of phosphorus as the oxyanion, e.g., UiO-66-NH, respectively 2 The material and the magnesium oxide/biochar composite adsorption material realize the efficient removal of phosphorus by the synergistic adsorption effect of complexation and hydrogen bonds formed by phosphorus. Given the similar physicochemical properties of the oxoanions phosphorus and arsenic, and the high efficiency of the complexation and hydrogen bonding cooperative adsorption strategy for oxoanion removal, we expected that the complexation and hydrogen bonding cooperative adsorption strategy would be applied to the high efficiency removal of arsenic.
Graphene Oxide (GO) is surface functionalized graphene with a 2D crystal form independent lamellar structure, the surface of the graphene oxide contains a large number of hydroxyl groups, carboxyl groups, aldehyde groups and the like, and the groups can adsorb and remove oxygen-containing anions (such as phosphorus and arsenic) in a water body through hydrogen bond action. In addition to that, GO is a metal oxide (MnFe) 2 O 4 、Fe 3 O 4 ) A good support material. Therefore, the HZO is loaded on the surface of GO through hydrogen bonds and oxygen vacancy repairing action to form an HZO/GO composite material, and then the inner layer complexing ability of the HZO to arsenic is strengthened by utilizing the hydrogen bonds of GO to arsenic, so that the arsenic is efficiently removed.
Disclosure of Invention
In view of this, one of the objectives of the present invention is to provide a composite adsorbing material for removing arsenic from water, which can be recycled.
The invention also aims to provide a preparation method of the composite adsorbing material for removing arsenic in water.
The invention also aims to provide a regeneration method of the composite adsorbing material for removing arsenic from water.
In order to achieve the above object, the present invention provides the following technical solutions:
the utility model provides a compound adsorption material for aquatic removes arsenic, compound adsorption material comprises Hydrous Zirconia (HZO) and oxidized Graphene (GO), GO in the compound adsorption material and HZO remove the effect in coordination to arsenic and have strengthened the high-efficient of arsenic and get rid of, GO has strengthened the inlayer complex ability to arsenic to HZO to the hydrogen bond that arsenic produced promptly for compound adsorption material is higher than GO alone or HZO to the adsorption capacity of arsenic and the sum of HZO and GO to the adsorption capacity of arsenic. Meanwhile, the composite adsorption material has good regeneration capacity for arsenic.
The invention provides a preparation method of a composite adsorption material for removing arsenic in water, which comprises the following steps:
(1) mixing graphite with NaNO 3 Adding 95% H into a flask with ice temperature (0-5℃) 2 SO 4 Forming a suspension, adding KMnO slowly to the suspension with continuous stirring 4 After the addition is finished, stirring is continued for 12 hours, and the stirring temperature is controlled at 25 ℃;
(2) adding deionized water into the mixed solution obtained in the step (1) twice, slowly adding the deionized water into the mixed solution when the ionized water is added for the first time, diluting the mixed solution when the ionized water is added for the second time, and then adding H 2 O 2 Stirring the solution for 0.5 h, centrifuging the mixed solution obtained by the reaction to obtain a centrifugal precipitate, washing the centrifugal precipitate for a plurality of times by using a 5% HCl solution to remove metal ions, washing the centrifugal precipitate for a plurality of times by using deionized water until the centrifugal precipitate is neutral, and finally cooling the centrifugal precipitateDrying in a freeze-drying oven to obtain GO;
(3) putting the GO obtained in the step (2) into deionized water, performing ultrasonic treatment to form GO dispersion liquid, and adding Zr 4+ Stirring the solution, and then mixing the obtained GO and Zr 4+ The mixed solution is put into a high-pressure reaction kettle for reaction, the reaction product is repeatedly washed to be neutral by deionized water, and finally, a freeze drying oven is used for drying to obtain the HZO/GO composite material.
Further, the suspension is mixed with KMnO 4 The reaction temperature of (a) cannot be higher than 10 ℃.
Further, the temperature is controlled to be 97-99 ℃ when the ionized water is added for the first time, and then the temperature is reduced to 60 ℃.
Further, said H 2 O 2 The concentration of the solution was 30 wt%.
Further, said Zr 4+ The concentration of the solution was 1 g/L.
Further, GO and Zr 4+ The reaction temperature of the mixed solution in the high-pressure reaction kettle is 120 ℃, and the reaction time is 24 hours.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
(1) according to the invention, a hydrothermal method is adopted to synthesize a hydrous zirconia/graphene oxide (HZO/GO) composite material, the Hydrous Zirconia (HZO) is loaded on the surface of Graphene Oxide (GO), wherein GO contains a large amount of hydroxyl, carboxyl, aldehyde group, epoxy group and the like, and the groups can perform hydrogen bond action with arsenic, so that arsenic is adsorbed. In addition, the HZO in the HZO/GO composite material also contains a large amount of-OH and H 2 O, As substituted for-OH and H in HZO 2 The O-containing composite material and Zr have complexation, so that inner layer complexation is generated on arsenic, and the hydrogen bond action can not only absorb arsenic, but also strengthen the inner layer complexation between Zr and arsenic, so as to enhance the adsorption capacity on arsenic, so that the adsorption capacity of the HZO/GO composite material on arsenic is obviously larger than the sum of the adsorption capacity of GO alone or HZO on arsenic and the adsorption capacity of HZO and GO on arsenic.
(2) The composite adsorbing material for removing motherland in water prepared by the invention has better regeneration capacity, and has good application prospect and popularization value.
Drawings
Fig. 1 is an SEM image, an enlarged SEM image of the HZO/GO composite material prepared in example 1, and an SEM image of the GO prepared in comparative example 1.
Fig. 2 is an XRD pattern of HZO/GO composite prepared in example 1, GO prepared in comparative example 1, and HZO.
FIG. 3 is an FTIR plot of HZO/GO composite prepared in example 1, GO prepared in comparative example 1, and HZO.
Fig. 4 is a graph of adsorption capacity of HZO/GO composite prepared in example 1, GO prepared in comparative example 1, and HZO for As at different equilibrium concentrations.
FIG. 5 is a graph of the recycling effect of As for the HZO/GO composite material prepared in example 1.
Detailed Description
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
4 g of graphite and 4 g of NaNO 3 300 mL of 95% H was added to an ice-warm (0-5 ℃ C.) flask 2 SO 4 A suspension is formed and 18 g of KMnO are added with continuous stirring 4 Slowly adding the mixture into the suspension to ensure that the reaction temperature cannot be higher than 10 ℃, increasing the temperature to 25 ℃ after the addition is finished, keeping the temperature for 12 hours under continuous stirring, then slowly adding 200 mL of deionized water into the mixed solution, controlling the temperature to be 97-99 ℃, then reducing the temperature to 60 ℃, then adding 500 mL of deionized water into the mixed solution again for dilution, and then adding 12 mL of 30 wt% H 2 O 2 Stirring for 0.5 h, centrifuging the mixed solution after reaction, washing the centrifuged precipitate with 5% HCl solution for several times to remove metal ions, washing with deionized water for several times until neutral, and coolingAnd drying by a freeze dryer to obtain GO.
Adding 1 g of GO into 500 ml of deionized water, performing ultrasonic treatment to form GO dispersion, and adding 1 g/L of Zr with certain volume 4+ The solution was stirred and then GO and Zr 4+ And putting the mixed solution into a high-pressure reaction kettle, reacting for 24 hours at 120 ℃, repeatedly cleaning the reaction product to be neutral by using deionized water, and finally freezing and drying to obtain the HZO/GO composite material.
Comparative example 1
4 g of graphite and 4 g of NaNO 3 300 mL of 95% H was added to an ice-warm (0-5 ℃ C.) flask 2 SO 4 A suspension is formed and 18 g of KMnO are added with continuous stirring 4 Slowly adding the mixture into the suspension to ensure that the reaction temperature cannot be higher than 10 ℃, increasing the temperature to 25 ℃ after the addition is finished, keeping the temperature for 12 hours under continuous stirring, slowly adding 200 mL of deionized water into the mixed solution, controlling the temperature to be 97-99 ℃, reducing the temperature to 60 ℃, adding 500 mL of deionized water into the mixed solution again for dilution, and adding 12 mL of 30 wt% H 2 O 2 Stirring for 0.5 h, centrifuging the mixed solution after the reaction is finished, washing the centrifuged precipitate for several times by using a 5% HCl solution to remove metal ions, then washing the precipitate for several times by using deionized water until the precipitate is neutral, and finally drying the precipitate by using a freeze dryer to obtain GO.
SEM images of GO prepared in comparative example 1 are shown in fig. 1 (a), and SEM images and magnified SEM images of HZO/GO composite material prepared in example 1 are shown in fig. 1 (b) and fig. 1 (c), respectively.
XRD patterns of the HZO/GO composite material prepared in example 1, GO prepared in comparative example 1, and HZO are shown in fig. 2. As can be seen from fig. 2, HZO shows a typical peak of amorphous hydrous zirconia at 2 θ =27 °, while HZO/GO composite also shows a diffraction peak at 2 θ =27 °, indicating successful loading of HZO to the GO surface.
The FTIR plots of HZO/GO composite material prepared in example 1, GO prepared in comparative example 1) and HZO are shown in fig. 3. As can be seen from FIG. 3, the characteristic peak of GO appears at 3420 cm -1 （-OH），1740 cm -1 (C = O) and 1625 cm -1 (C = C), indicating that GO contains abundant oxygenAn oxygen-rich group. HZO at 3410, 1567, 1347, 474 cm -1 Characteristic peaks appear at the positions, and the corresponding groups are respectively-OH (stretching vibration), -OH (bending vibration), Zr-OH and Zr-O-Zr. After the HZO loads GO, the-OH peak in the HZO/GO composite material shifts to 3465 cm -1 Indicating that hydrogen bonding occurs between HZO and GO, indicating that HZO is loaded to the GO surface through hydrogen bonding. Meanwhile, the HZO/GO composite material is 1740 cm -1 The peak at C = O disappears, indicating that C = O and Zr in GO 4+ Crosslinking occurs. At the same time, 1360 cm -1 And 474 cm -1 Peaks of Zr-OH and Zr-O-Zr appear respectively, and further confirms the existence of HZO in the composite adsorbing material.
The adsorption capacities of HZO/GO composite material prepared in example 1, GO prepared in comparative example 1, and HZO for As at different equilibrium concentrations are shown in fig. 4. As can be seen from FIG. 4, the adsorption capacity of HZO/GO composite material to arsenic is significantly larger than the adsorption capacity of GO or HZO to arsenic and the sum of the adsorption capacities of HZO and GO to arsenic, which indicates that the composite material formed by HZO and GO is more favorable for arsenic adsorption, and this is mainly related to the adsorption mechanism of HZO/GO composite material to arsenic. In the HZO/GO composite material, GO contains a large number of carboxyl, hydroxyl, epoxy, aldehyde groups and the like, and the groups can form hydrogen bond action with arsenic, so that arsenic is adsorbed. Further, the HZO in the HZO/GO composite material contains a large amount of-OH and H 2 O and arsenic are subjected to complexation with Zr after replacing-OH and H2O in HZO, so that the arsenic is adsorbed. Besides the adsorption effect on arsenic, the hydrogen bond effect can also strengthen the complexation effect between Zr and arsenic, so that the adsorption capacity on arsenic is enhanced. Therefore, the adsorption capacity of the HZO/GO composite material on arsenic through the synergistic adsorption effect of hydrogen bonds and complexation is far higher than that of GO or HZO on arsenic through single hydrogen bonds or complexation.
Example 2
The composite adsorption material related by the invention can be simply regenerated, and has good recycling performance, and the specific process is as follows:
and (3) immersing the HZO/GO composite material after absorbing As into a 5 wt% NaOH solution for elution and regeneration.
The adsorption capacity and regeneration capacity of the HZO/GO composite material for As are shown in fig. 5. As shown in FIG. 5, the adsorption capacity of the HZO/GO composite material for As gradually decreases As the number of cycles increases. Compared with the first adsorption, after 5 cycles, the adsorption capacity of the HZO/GO composite material to As is only reduced by 21%. The results show that the HZO/GO composite material has better regeneration capability in the aspect of As adsorption.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.

Claims (7)

1. The utility model provides a compound adsorption material for aquatic removes arsenic, a serial communication port, compound adsorption material comprises Hydrous Zirconia (HZO) and Graphite Oxide (GO), and HZO forms compound adsorption material through hydrogen bond and oxygen vacancy restoration effect load to GO surface, GO strengthens HZO to the inlayer complex ability of arsenic among the compound adsorption material to the hydrogen bond of arsenic to realize the high-efficient of arsenic and get rid of.
2. The preparation method of the composite adsorbing material for removing arsenic in water as claimed in claim 1, which comprises the following steps:
(1) mixing graphite with NaNO 3 Adding 95% H into a flask with ice temperature (0-5℃) 2 SO 4 Forming a suspension, adding KMnO slowly to the suspension with continuous stirring 4 After the addition is finished, stirring is continued for 12 hours, and the stirring temperature is controlled at 25 ℃;
(2) adding deionized water into the mixed solution obtained in the step (1) twice, slowly adding the deionized water into the mixed solution when the ionized water is added for the first time, diluting the mixed solution when the ionized water is added for the second time, and then adding H 2 O 2 Stirring the solution for 0.5 h, centrifuging the mixed solution obtained by the reaction to obtain a centrifugal precipitate, washing the centrifugal precipitate for a plurality of times by using a 5% HCl solution to remove metal ions, washing the centrifugal precipitate for a plurality of times by using deionized water until the centrifugal precipitate is neutral, and finally cooling the centrifugal precipitateDrying in a freeze-drying oven to obtain GO;
(3) putting the GO obtained in the step (2) into deionized water, performing ultrasonic treatment to form GO dispersion liquid, and adding Zr 4+ Stirring the solution, and then mixing the obtained GO and Zr 4+ The mixed solution is put into a high-pressure reaction kettle for reaction, the reaction product is repeatedly washed to be neutral by deionized water, and finally the composite adsorbing material is obtained by drying by a freeze drying box.
3. The method for preparing the composite adsorbing material for removing arsenic in water as claimed in claim 2, wherein the suspension is mixed with KMnO 4 The reaction temperature of (a) cannot be higher than 10 ℃.
4. The preparation method of the composite adsorbing material for removing arsenic from water as claimed in claim 2, wherein the temperature is controlled to 97-99 ℃ when the ionized water is added for the first time, and then the temperature is reduced to 60 ℃.
5. The method for preparing the composite adsorbing material for removing arsenic in water as claimed in claim 2, wherein the H is 2 O 2 The concentration of the solution was 30 wt%.
6. The method for preparing the composite adsorbing material for removing arsenic in water as claimed in claim 2, wherein Zr is used 4+ The concentration of the solution was 1 g/L.
7. The method for preparing the composite adsorbing material for removing arsenic in water as claimed in claim 2, wherein the GO and the Zr are used 4+ The reaction temperature of the mixed solution in the high-pressure reaction kettle is 120 ℃, and the reaction time is 24 hours.
CN202210359543.7A 2022-04-07 2022-04-07 Composite adsorption material for removing arsenic in water and preparation method thereof Pending CN114797771A (en)

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Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112973656A (en) * 2021-02-07 2021-06-18 重庆工商大学 Preparation method of renewable composite material for efficiently removing arsenic in wastewater

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112973656A (en) * 2021-02-07 2021-06-18 重庆工商大学 Preparation method of renewable composite material for efficiently removing arsenic in wastewater

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
张丹慧等: "《贵金属-石墨烯纳米复合材料的合成及性能》", 北京：国防工业出版社, pages: 1 - 8 *

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