CN112263986A - Surfactant-loaded goethite material and preparation method thereof - Google Patents

Surfactant-loaded goethite material and preparation method thereof Download PDF

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Publication number
CN112263986A
CN112263986A CN202011010576.8A CN202011010576A CN112263986A CN 112263986 A CN112263986 A CN 112263986A CN 202011010576 A CN202011010576 A CN 202011010576A CN 112263986 A CN112263986 A CN 112263986A
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China
Prior art keywords
surfactant
goethite
loaded
solution
preparing
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CN202011010576.8A
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Inventor
易筱筠
薛潮
阳月贝
杨志林
郝鑫瑞
卢桂宁
党志
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South China University of Technology SCUT
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South China University of Technology SCUT
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Priority to CN202011010576.8A priority Critical patent/CN112263986A/en
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Priority to CN202110605378.4A priority patent/CN113304723B/en
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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
    • B01J20/06—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
    • 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
    • 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
    • C02F2101/20—Heavy metals or heavy metal compounds

Abstract

The invention discloses a surfactant-loaded goethite material and a preparation method thereof. The method comprises the following steps: adding a surfactant into a solvent, and uniformly mixing to obtain a surfactant solution; mixing the activator solution with the ferric iron solution, and uniformly stirring to obtain a mixed solution; and adjusting the pH value of the mixed solution to 12.0-13.0, heating for aging, centrifuging to obtain a precipitate, washing, drying, grinding into powder, and sieving to obtain the surfactant-loaded goethite material. According to the preparation method provided by the invention, the surfactant-loaded goethite complex is prepared by a hydrothermal method, so that not only are nano-sized particles and morphology prepared, but also the introduction of the surfactant is beneficial to reducing agglomeration of goethite, and the surface of the goethite has more abundant functional groups. The goethite prepared by the coprecipitation method has uniform appearance, can be used for adsorbing heavy metal ions in an aqueous solution, and has higher removal efficiency compared with pure goethite.

Description

Surfactant-loaded goethite material and preparation method thereof
Technical Field
The invention belongs to the field of preparation of environment functional materials, and mainly relates to a surfactant-loaded goethite material and a preparation method thereof.
Background
Goethite (alpha-FeOOH) is one of the most widely existing iron minerals in tropical and subtropical soils, has a high industrial production value, has a fine particle structure and a large specific surface area due to stable chemical properties, has a wide development and application prospect in environmental management, and is an environmental functional material with excellent performance. Goethite can stably exist in acid soil, and can remarkably influence the geochemical cycle process of pollutants in the environment through interface reactions such as migration diffusion, adsorption and desorption, precipitation and dissolution, oxidation and reduction and the like between goethite and the pollutants, thereby influencing the migration conversion capability and the toxicological ecological effect of the pollutants in the environment.
Natural goethite has a limited ability to adsorb heavy metals and organic pollutants. Similar to clay minerals, many researchers have been focusing on the modification of goethite to improve its ability to remove specific contaminants. However, the improved pollutant removal capability after modification is still not ideal no matter the goethite preparation conditions are optimized or specific chemical substances are loaded/doped in the preparation process.
The surfactant is usually used for modifying certain adsorbents, can change the interface state of a reaction system, and can enrich the surface functional groups of the original adsorbents, so that the adsorption capacity of the adsorbents can be improved. The types of the surfactants are various, and different surfactants have different chemical properties, but the modification mode by adding the surfactants in the goethite preparation process is not common.
Zhang jin Hua et al [ Zhang jin Hua, Zhu Xiao Meng, xu Fang, etc. ], a method for synthesizing surfactant-modified goethite, 2014]Sodium dodecyl sulfate (C) was added during the preparation of goethite12H25NaO4S) solution, the adsorption efficiency of the synthesized product to organic pollutants in water is improved to a certain extent. However, no report on the relevant composite material for heavy metal adsorption is yet found.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a surfactant-loaded goethite material and a preparation method thereof.
The invention aims to provide a preparation method of surfactant-loaded goethite.
The purpose of the invention is realized by at least one of the following technical solutions.
The preparation method of the surfactant-loaded goethite material provided by the invention comprises the following steps:
(1) adding a surfactant into a solvent, and uniformly mixing to obtain a surfactant solution; mixing the activator solution with the ferric iron solution, and uniformly stirring to obtain a mixed solution;
(2) and (2) adjusting the pH value of the mixed solution in the step (1) to 12.0-13.0, transferring the mixed solution into a polyethylene plastic bottle, covering the opening, heating for aging treatment (standing and aging in an oven), centrifuging to obtain a precipitate, washing, drying, grinding into powder, and sieving to obtain the surfactant-loaded goethite material.
Further, the surfactant in the step (1) is anionic polyacrylamide.
Further, the solvent in the step (1) is deionized water; the concentration of the surfactant solution is 8.0-12.0 g/L.
Further, the ferric iron solution in the step (1) is Fe (NO)3)3·9H2And the concentration of the ferric iron solution is 0.9-1.1 mol/L.
Further, the volume ratio of the surfactant solution to the ferric iron solution in the step (1) is 1:4-1: 6.
Preferably, the stirring time of step (1) is 10 min.
Further, the aging time of the step (2) is not less than 48 hours.
Further, the temperature of the aging treatment in the step (2) is 60-70 ℃.
Preferably, the aging treatment time of the step (2) is 60 h.
Preferably, in the step (2), the pH value of the mixed solution may be adjusted by using a strong alkali solution, wherein the strong alkali solution is one or more of a NaOH solution and a KOH solution. The concentration of the strong alkali solution is 5 mol/L.
Further, the size of the sieve holes of the sieve in the step (2) is 100 meshes.
Further, the drying in the step (2) is freeze-drying under vacuum condition, and the temperature of the freeze-drying is-20 ℃.
The present invention provides a surfactant-loaded goethite material (surfactant-loaded goethite complex) prepared by the above-described preparation method.
The goethite prepared by the coprecipitation method has uniform appearance, can be used for adsorbing heavy metal ions in an aqueous solution, and has higher removal efficiency compared with pure goethite.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) according to the preparation method provided by the invention, the surfactant-loaded goethite complex is prepared by a hydrothermal method, so that not only are nano-sized particles and morphology prepared, but also the introduction of the surfactant is beneficial to reducing agglomeration of goethite, and the surface of the goethite has more abundant functional groups.
(2) Compared with a pure goethite sample prepared under the same condition, the goethite material loaded with the surfactant, prepared by the invention, has a remarkable removal effect on heavy metal ions in an aqueous solution.
Drawings
Figure 1 is an XRD pattern of a sample prepared in example 1 of the present invention.
FIG. 2 is a FTIR plot of a sample prepared in example 1 of the present invention.
FIG. 3 is an SEM image of a sample prepared in example 1 of the present invention.
FIG. 4 is a SEM-EDS picture of a sample prepared in example 1 of the present invention.
Fig. 5 is a graph showing the adsorption efficiency of the sample prepared in example 1 of the present invention to the heavy metal cadmium, respectively, and the pure goethite sample prepared under the same conditions.
Detailed Description
The following description of the embodiments of the present invention is provided in connection with the accompanying drawings and examples, but the invention is not limited thereto. It is noted that the processes described below, if not specifically described in detail, are all realizable or understandable by those skilled in the art with reference to the prior art. The reagents or apparatus used are not indicated to the manufacturer, and are considered to be conventional products available by commercial purchase.
Example 1
20.2 g Fe (NO) are weighed out3)3·9H2O was placed in a beaker and 0.05L of distilled water was added to make a 1M solution. 810 g/L Anionic Polyacrylamide (APAM) solution with the volume of 0.01L is poured into the ferric nitrate solution, and the mixture is fully stirred and mixed to form uniform suspension. Subsequently, a 5M KOH solution was poured into the mixed suspension solution in portions while stirring, and the pH of the homogeneous suspension was adjusted to 13.0. And transferring the mixed solution into a polyethylene plastic bottle, sealing, and standing and aging in an oven at 60 ℃ for 60 hours. Standing, aging, centrifuging, washing with deionized water for 5 times, freeze drying, and grinding with 100 mesh sieve to obtain goethite complex (surfactant-loaded goethite material) loaded with anionic polyacrylamide. XRD, FT-IR, SEM-EDS, and adsorption curves of the surfactant-loaded goethite material samples prepared are shown in FIGS. 1 to 5, respectively. XRD patterns andthe result of the SEM image shows that the prepared goethite complex sample is long rod acicular nanoparticles with uniform appearance and smooth surface. It can be seen in the FT-IR chart that at 789 cm-1And 883cm-1The two nearby peaks are characteristic peaks of goethite, namely stretching vibration of surface-OH and bending vibration of surface hydroxyl of Fe-OH-Fe, and the peak shapes are sharp and symmetrical, which indicates that the synthesized goethite complex is good in crystallization. 1371 cm-1The nearby absorption peak is bending vibration of free hydroxyl, and the goethite complex loaded with anionic polyacrylamide absorbs Cd2After + here the intensity of the absorption peak is clearly reduced. 1656 cm-1The nearby absorption peak is the O-H bending vibration of the crystal water. 3100 cm-1Nearby stretching vibrations are goethite free-OH and hydrated hydroxyl-OH2+ and Cd adsorbed by the complex2After + here too the absorption peak intensity is significantly reduced, meaning Cd2+ may react with surface hydroxyl groups, causing a reduction in the intensity of the absorption peak there. The results of SEM-EDS and adsorption curves show that the complex sample is paired with Cd2The removal efficiency of + is very significant.
Example 2
20.2 g Fe (NO) are weighed out3)3·9H2O was placed in a beaker and 0.05L of distilled water was added to make a 1M solution. 10 g/L Anionic Polyacrylamide (APAM) solution with the volume of 0.01L is poured into the ferric nitrate solution, and the mixture is fully stirred and mixed to form uniform suspension. Subsequently, while pouring a 5M NaOH solution into the mixed suspension solution in portions, the pH of the homogeneous suspension was adjusted to 12.0 to 13.0 by stirring. And transferring the mixed solution into a polyethylene plastic bottle, sealing, and standing and aging in an oven at 70 ℃ for 48 hours. Centrifuging after 48h, washing for 5 times by using deionized water, freeze-drying, and grinding and sieving by using a 100-mesh sieve to obtain the goethite complex (surfactant-loaded goethite material) loaded with the anionic polyacrylamide. The sample material prepared in example 2 has the same adsorption capacity for heavy metals as the material of example 1, and the surface physical and chemical properties thereof can be shown in fig. 1 to 5.
Example 3
20.2 g Fe (NO) are weighed out3)3·9H2O was placed in a beaker and 0.05L of distilled water was added to make a 1M solution. 10 g/L Anionic Polyacrylamide (APAM) solution with the volume of 0.01L is poured into the ferric nitrate solution, and the mixture is fully stirred and mixed to form uniform suspension. Subsequently, a 5M KOH solution was poured into the mixed suspension solution in portions while stirring, and the pH of the homogeneous suspension was finally adjusted to 12.0 to 13.0. And transferring the mixed solution into a polyethylene plastic bottle, sealing, and standing and aging in an oven at 60 ℃ for 48 hours. Centrifuging after 48h, washing for 5 times by using deionized water, freeze-drying, and grinding and sieving by using a 100-mesh sieve to obtain the goethite complex (surfactant-loaded goethite material) loaded with the anionic polyacrylamide. The sample material prepared in example 3 has the same adsorption capacity for heavy metals as the material of example 1, and the surface physical and chemical properties thereof can be shown in fig. 1 to 5.
Comparative example
20.2 g Fe (NO) are weighed out3)3·9H2O was placed in a beaker and 0.05L of distilled water was added to make a 1M solution. Subsequently, a 5M KOH solution was poured into the ferric nitrate solution in portions while stirring, and the pH of the mixed solution was finally adjusted to 13.0. And transferring the mixed solution into a polyethylene plastic bottle, adding deionized water to dilute to 1L, sealing, and standing and aging in an oven at 60 ℃ for 48 h. Centrifuging after 48h, washing for 5 times by using deionized water, freeze-drying, grinding and sieving by using a 100-mesh sieve to obtain the pure goethite.
Application example
The goethite complex prepared in examples 1 to 3 and the pure goethite prepared in the comparative example were used for adsorbing heavy metal cadmium, the initial concentration of cadmium was 20mg/L, the mineral addition amount was 0.5g/L, the pH was 5.0, the reaction temperature was 30 ℃, and the reaction system was 40mL, respectively. The experimental result proves that the absorption efficiency of the goethite complex prepared in the example on cadmium is more than 80%, while the absorption rate of the comparative example is only 48.9%, as shown in fig. 5.
The above examples are only preferred embodiments of the present invention, which are intended to be illustrative and not limiting, and those skilled in the art should understand that they can make various changes, substitutions and alterations without departing from the spirit and scope of the invention.

Claims (10)

1. A preparation method of a surfactant-loaded goethite material is characterized by comprising the following steps:
(1) adding a surfactant into a solvent, and uniformly mixing to obtain a surfactant solution; mixing the activator solution with the ferric iron solution, and uniformly stirring to obtain a mixed solution;
(2) and (2) adjusting the pH value of the mixed solution obtained in the step (1) to 12.0-13.0, heating for aging, centrifuging to obtain a precipitate, washing, drying, grinding into powder, and sieving to obtain the surfactant-loaded goethite material.
2. The method for preparing the surfactant-loaded goethite material according to claim 1, wherein the surfactant in the step (1) is anionic polyacrylamide.
3. The method for preparing a surfactant-loaded goethite material as claimed in claim 1, wherein the solvent in the step (1) is deionized water; the concentration of the surfactant solution is 8.0-12.0 g/L.
4. The method of preparing surfactant-loaded goethite material according to claim 1, wherein the ferric iron solution of step (1) is Fe (NO)3)3·9H2And the concentration of the ferric iron solution is 0.9-1.1 mol/L.
5. The method for preparing a surfactant-loaded goethite material according to claim 1, wherein the volume ratio of the surfactant solution to the ferric iron solution in the step (1) is 1:4 to 1: 6.
6. The method for preparing a surfactant-loaded goethite material according to claim 1, wherein the aging treatment of the step (2) is carried out for not less than 48 hours.
7. The method for preparing a surfactant-loaded goethite material according to claim 1, wherein the aging temperature in the step (2) is 60 to 70 ℃.
8. The method for preparing a surfactant-loaded goethite material according to claim 1, wherein the size of the mesh of the screen in the step (2) is 100 mesh.
9. The method for preparing the surfactant-loaded goethite material according to claim 1, wherein the drying in the step (2) is freeze-drying under vacuum at a temperature of-20 ℃.
10. A surfactant-loaded goethite material produced by the production method according to any one of claims 1 to 9.
CN202011010576.8A 2020-09-23 2020-09-23 Surfactant-loaded goethite material and preparation method thereof Pending CN112263986A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114618442A (en) * 2022-01-27 2022-06-14 华南理工大学 Organic modified ferrihydrite composite material and preparation method and application thereof

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US20130015398A1 (en) * 2010-01-29 2013-01-17 Jinneng Science & Technology Co., Ltd. Method for preparing modified micronized particles
CN103599765A (en) * 2013-11-19 2014-02-26 南京理工大学 Method for synthesizing surfactant-modified goethite
CN105056719B (en) * 2015-07-30 2017-10-10 福州大学化肥催化剂国家工程研究中心 The preparation method and desulfurizing agent obtained by this method of a kind of FeOOH low-temp desulfurization agent
CN105217772A (en) * 2015-10-10 2016-01-06 贵州万山兴隆锰业有限公司 A kind of additive for manganese ore wastewater treatment and preparation method thereof
DE102018130744A1 (en) * 2018-12-03 2020-06-25 Universität Duisburg-Essen Use of iron oxide particles in waste water to eliminate contamination
CN109626493B (en) * 2019-01-04 2021-08-31 三峡大学 Application of surfactant modified goethite in removing microcystis aeruginosa

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Publication number Priority date Publication date Assignee Title
CN114618442A (en) * 2022-01-27 2022-06-14 华南理工大学 Organic modified ferrihydrite composite material and preparation method and application thereof

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Inventor after: Yin Hua

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Application publication date: 20210126