CN107970890B - Hydroxyl iron modified activated carbon composite material and preparation method thereof - Google Patents

Hydroxyl iron modified activated carbon composite material and preparation method thereof Download PDF

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CN107970890B
CN107970890B CN201711244659.1A CN201711244659A CN107970890B CN 107970890 B CN107970890 B CN 107970890B CN 201711244659 A CN201711244659 A CN 201711244659A CN 107970890 B CN107970890 B CN 107970890B
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吴锦华
苏眉
方一莉
李平
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South China University of Technology SCUT
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    • 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
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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    • 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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    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • B01J20/28064—Surface area, e.g. B.E.T specific surface area being in the range 500-1000 m2/g
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • 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
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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    • C02F1/28—Treatment of water, waste water, or sewage by sorption
    • C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
    • 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
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    • C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
    • 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
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  • Water Treatment By Sorption (AREA)
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Abstract

The invention discloses a hydroxyl iron modified activated carbon composite material and a preparation method thereof. The preparation method comprises the following steps: (1) acid washing the activated carbon under an ultrasonic condition to remove surface impurities, and drying to obtain pretreated activated carbon for later use; (2) adding pretreated activated carbon into a ferric nitrate solution, adjusting the pH value of the obtained solid-liquid mixture by using an HCl solution and an NaOH solution, reacting under a stirring condition at room temperature, and after the reaction is finished, placing the mixture into a constant-temperature oven for aging; (3) and after aging, performing centrifugal separation to obtain a solid, and performing rinsing and baking to obtain the hydroxyl iron modified activated carbon composite material. The preparation method has the advantages of cheap and easily obtained raw materials and simple preparation, and compared with the activated carbon, the prepared FeOOH modified activated carbon composite material has greatly improved heavy metal adsorption capacity.

Description

Hydroxyl iron modified activated carbon composite material and preparation method thereof
Technical Field
The invention relates to the technical field of preparation of activated carbon composite materials, in particular to a hydroxyl iron modified activated carbon composite material and a preparation method thereof.
Background
With the rapid development of industries such as mining, smelting, electroplating and the like, a large amount of wastewater is discharged into nature, heavy metal pollution of natural water is increasingly serious, and the water quality safety of drinking water sources is seriously threatened. Therefore, how to remove heavy metals in water with low cost and high efficiency is important for ensuring the safety of drinking water.
At present, the conventional drinking water purification methods mainly comprise coagulation precipitation, electrodialysis, ion exchange, membrane separation and the like. Although the methods can remove heavy metals in drinking water, the methods have certain limitations, such as large sludge yield in a coagulating sedimentation method; the electrodialysis method has high power consumption; ion exchange and membrane separation processes have poor impact resistance and high operating costs. Different from the method, the adsorption method is undoubtedly a method for effectively removing heavy metals in drinking water due to the advantages of simple treatment method, low operation cost, simple and convenient operation and the like.
Among the adsorbents, activated carbon is widely used for purifying drinking water due to its advantages of rich pore passages, large specific surface area, high mechanical strength and adjustable particle size. Experimental research and industrial application results show that although the activated carbon has strong adsorption effect on small molecular organic matters and aromatic hydrocarbons, the activated carbon has weak adsorption capacity on heavy metal ions, particularly negatively charged chromium, arsenic and the like, and the adsorption capacity is usually less than 10mg/g, mainly because the surface functional groups of the activated carbon are mostly weak electronegative groups such as hydroxyl and carboxyl and the charges are weak. In addition, the active carbon has the defects of poor selectivity, slow adsorption rate and the like, and the performance of the active carbon in water purification treatment is seriously restricted, so that an effective, simple and safe method for modifying the active carbon is urgently needed to improve the removal capacity of the active carbon on heavy metal ions in drinking water.
The hydroxyl iron is an active mineral widely existing in nature, has stable chemical properties, higher specific surface area and fine particle structure, has strong adsorption capacity on negative heavy metal ions and positive heavy metal ions in water by ferric oxide groups and hydroxyl groups on the surface, can synchronously remove the negative heavy metal ions and the positive heavy metal ions in the water, but is easy to agglomerate in the using process to cause the activity to be rapidly reduced, and the reacted hydroxyl iron particles are fine and difficult to separate from the solution.
In view of the above, the research on modifying the activated carbon by using the hydroxyl iron to uniformly distribute the hydroxyl iron particles on the surface and the pore channels of the activated carbon solves the problems that the hydroxyl iron is easy to agglomerate and is difficult to separate from the solution after use, and is expected to greatly improve the heavy metal adsorption capacity of the activated carbon by means of the hydroxyl iron while not greatly reducing the specific surface area of the activated carbon, so as to realize the process for synchronously removing the negative and positive heavy metal ions.
Disclosure of Invention
The invention aims to provide a method for preparing a hydroxyl iron modified activated carbon composite material aiming at the defects of the prior art. According to the preparation method, the active carbon and ferric nitrate which are low in price and easy to obtain are used as raw materials, the active carbon is used as a carrier, the ferric nitrate is used as a modifier, the hydroxyl iron modified active carbon composite material is prepared through simple steps, and the heavy metal adsorption performance of the active carbon can be improved without complex process conditions and production equipment.
The invention also aims to provide the hydroxyl iron modified activated carbon composite material prepared by the preparation method. The hydroxyl iron activated carbon composite material is expected to be applied to drinking water treatment on a large scale, even treatment of sudden environmental pollution events, and a new method is provided for ensuring the safety of drinking water.
The purpose of the invention is realized by the following technical scheme.
A preparation method of a hydroxyl iron modified activated carbon composite material comprises the following steps:
(1) acid washing the activated carbon under an ultrasonic condition to remove surface impurities, and drying to obtain pretreated activated carbon for later use;
(2) adding the pretreated activated carbon into a ferric nitrate solution, adjusting the pH value of the obtained solid-liquid mixture, reacting under the condition of stirring at room temperature, and aging in a constant-temperature oven after the reaction is finished;
(3) and after aging, performing centrifugal separation to obtain a solid, and performing rinsing and baking to obtain the hydroxyl iron modified activated carbon composite material.
Further, in the step (1), the particle size of the activated carbon is 150 meshes.
Further, in the step (1), the acid-washing solution is 0.1mol/L HCl solution.
Further, in the step (1), the time for pickling under the ultrasonic condition is 15 min.
Further, in the step (1), the drying temperature is 100 ℃.
Further, in the step (2), the feed-liquid ratio of the pretreated activated carbon to the ferric nitrate solution is 4.48: 100 g/mL.
Further, in the step (2), the concentration of the ferric nitrate solution is 0.1-1.0 mol/L, preferably 0.1 mol/L.
Further, in the step (2), the pH value of the solid-liquid mixture obtained by adjusting is adjusted by using HCl solution and NaOH solution with the concentration of 0.1 mol/L; .
Further, in the step (2), the pH value is adjusted to be 7.
Further, in the step (2), the reaction time is 12 h.
Further, in the step (2), the aging temperature is 70 ℃, and the aging time is 12 h.
Further, in the step (3), the rinsing is performed until the washing solution is neutral.
Further, in the step (3), the baking is performed at 70 ℃ for 12 h.
The hydroxyl iron modified activated carbon composite material prepared by the preparation method takes activated carbon as a carrier to load inorganic material hydroxyl iron particles, and the specific surface area is 770m 2 In terms of/g, the Fe content is 2.3 wt.%.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) according to the invention, the hydroxyl iron can be effectively used for modifying the active carbon to prepare the hydroxyl iron modified active carbon composite material; the active carbon composite material modified by the hydroxyl iron not only reserves the huge specific surface area of the active carbon, but also enhances the chemical stability, and the heavy metal adsorption capacity of the active carbon composite material is greatly improved compared with that of the active carbon before modification;
(2) according to the invention, the active carbon and ferric nitrate which are low in price and easy to obtain are used as raw materials, and the hydroxyl iron modified active carbon composite material is prepared by a simple process, so that the production equipment and process requirements are low, the cost is low, the production efficiency is high, and the industrial production is easy to realize;
(3) the preparation process is simple, and the loading process of the hydroxyl iron can be finished only in an oven without high-temperature roasting.
Drawings
FIG. 1 is a Scanning Electron Microscope (SEM) image of a FeOOH-modified activated carbon composite prepared in example 1;
fig. 2 is an X-ray diffraction (XRD) pattern of the iron oxyhydroxide-modified activated carbon composite prepared in example 1.
Detailed Description
The technical solution of the present invention is further described in detail below with reference to specific examples and drawings, but the embodiments and the scope of the present invention are not limited thereto.
Example 1
The preparation method of the hydroxyl iron modified activated carbon composite material comprises the following steps:
(1) and ultrasonically pickling the active carbon with the particle size of 150 meshes for 15min by using 0.1mol/L HCl solution to remove surface impurities, and drying at 100 ℃ for later use.
(2) Weighing 4.48g of the activated carbon treated in the step (1), adding the activated carbon into 100mL of 0.1mol/L ferric nitrate solution to obtain a solid-liquid mixture, and adjusting the pH value of the mixture to be 7 by using HCl solution and NaOH solution with the concentrations of 0.1 mol/L; and then stirring the solid-liquid mixture for reaction for 12 hours at room temperature by using a magnetic stirrer, and then placing the mixture in an oven at 70 ℃ for aging for 12 hours.
(3) And (3) centrifugally separating the aged solid in the step (2), rinsing to be neutral, and baking at 70 ℃ for 12h to obtain the hydroxyl iron modified activated carbon composite material.
The Scanning Electron Microscope (SEM) of the prepared hydroxyl iron modified activated carbon is shown in figure 1, and as can be seen from figure 1, the particle size of the hydroxyl iron particles is 0.1-1 μm and is uniformly distributed on the surface and in the pore channels of the activated carbon.
The prepared hydroxyl iron modified active carbon composite material has the specific surface area of 770m 2 In terms of/g, the Fe content is 2.3 wt.%. Because the iron loading is less than 3 percent, the specific surface area and the number of adsorption sites of the activated carbon are not obviously reduced, so that the capability of the activated carbon for adsorbing small-molecule organic pollutants and aromatic hydrocarbons is maintained, a new function is given to the activated carbon, and the capability of removing heavy metals is greatly improved.
The X-ray diffraction pattern (XRD) of the prepared iron oxyhydroxide-modified activated carbon is shown in fig. 2, and it can be seen from fig. 2 that characteristic peaks of iron oxyhydroxide appear in the prepared composite material, indicating that iron oxyhydroxide is generated on the surface of the activated carbon.
The prepared hydroxyl iron modified activated carbon composite material and activated carbon are used for respectively carrying out a simulated solution static adsorption comparison experiment on chromium ions (hexavalent) and cadmium ions (divalent).
0.2g/L of hydroxyl iron modified activated carbon composite material and 0.2g/L of activated carbon are respectively added into a chromium ion solution and a cadmium ion solution, wherein the concentration of the chromium ion solution is 2.5mg/L, the concentration of the cadmium ion solution is 3.0mg/L, and the experimental results are shown in Table 1.
TABLE 1 comparative test results of adsorption properties of FeOH-modified activated carbon composite and activated carbon
Figure BDA0001490514950000061
As can be seen from table 1, the adsorption amounts of the activated carbon modified by iron hydroxide to chromium ions and cadmium ions were 5 times and 4 times, respectively, that were not modified, and the adsorption capacity of the activated carbon modified by iron hydroxide to heavy metals was greatly improved.
The above embodiments are merely preferred embodiments of the present invention, which are intended to be illustrative and not limiting, and any changes, substitutions, combinations, simplifications, modifications, etc. made by those skilled in the art without departing from the spirit and principle of the present invention shall be included in the scope of the present invention.

Claims (4)

1. Application of hydroxyl iron modified activated carbon composite material in Cr 6+ Or Cd 2+ The application of adsorption is characterized by comprising the following steps:
(1) acid washing the active carbon with the particle size of 150 meshes under the ultrasonic condition to remove surface impurities, and drying at 100 ℃ to obtain pretreated active carbon for later use; the solution of the acid washing is 0.1mol/L HCl solution; the pickling time under the ultrasonic condition is 15 min;
(2) adding pretreated activated carbon into a ferric nitrate solution, wherein the feed-liquid ratio of the pretreated activated carbon to the ferric nitrate solution is 4.48: 100 g/mL; the concentration of the ferric nitrate solution is 0.1-1.0 mol/L, the obtained solid-liquid mixture is subjected to reaction under the condition of stirring at room temperature after the pH value of the obtained solid-liquid mixture is adjusted, and the obtained solid-liquid mixture is placed in a constant-temperature oven for aging after the reaction is finished, wherein the aging temperature is 70 ℃, and the aging time is 12 hours; the pH value of the solid-liquid mixture obtained by adjustment is adjusted by HCl solution and NaOH solution with the concentration of 0.1 mol/L; the pH value is adjusted to be 7;
(3) after aging is finished, performing centrifugal separation to obtain a solid, rinsing and baking to obtain the hydroxyl iron modified activated carbon composite material, wherein the specific surface area of the prepared hydroxyl iron modified activated carbon composite material is 770m 2 The Fe content was 2.3 wt./g.
2. The FeOOH modified activated carbon composite material used for Cr according to claim 1 6+ Or Cd 2+ The application of adsorption is characterized in that in the step (2), the reaction time is 12 h.
3. The FeOOH modified activated carbon composite material used for Cr according to claim 1 6+ Or Cd 2+ The application of adsorption is characterized in that in the step (3), the rinsing is performed until the rinsing liquid is neutral.
4. The application of the FeOOH-modified activated carbon composite material in Cr (chromium) according to claim 1 6+ Or Cd 2+ Use of adsorption, characterized in that in step (3), the baking is at 70 ℃ for 12 h.
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CN115121006A (en) * 2022-07-05 2022-09-30 科立鑫(珠海)新能源有限公司 Method for removing nickel and cadmium impurities from cobalt sulfate solution

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