CN106311130A - Modified attapulgite material and its preparation and application methods - Google Patents

Modified attapulgite material and its preparation and application methods Download PDF

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Publication number
CN106311130A
CN106311130A CN201610821169.2A CN201610821169A CN106311130A CN 106311130 A CN106311130 A CN 106311130A CN 201610821169 A CN201610821169 A CN 201610821169A CN 106311130 A CN106311130 A CN 106311130A
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attapulgite
activation
modified
modified attapulgite
manganese ions
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CN106311130B (en
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王君
魏新涛
张宏森
刘琦
刘婧媛
宋大雷
李茹民
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Harbin Engineering University
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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
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/12—Naturally occurring clays or bleaching earth
    • 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
    • G—PHYSICS
    • G21—NUCLEAR PHYSICS; NUCLEAR ENGINEERING
    • G21F—PROTECTION AGAINST X-RADIATION, GAMMA RADIATION, CORPUSCULAR RADIATION OR PARTICLE BOMBARDMENT; TREATING RADIOACTIVELY CONTAMINATED MATERIAL; DECONTAMINATION ARRANGEMENTS THEREFOR
    • G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
    • G21F9/04—Treating liquids
    • G21F9/06—Processing
    • G21F9/12—Processing by absorption; by adsorption; by ion-exchange

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  • Chemical & Material Sciences (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • High Energy & Nuclear Physics (AREA)
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  • General Engineering & Computer Science (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Water Treatment By Sorption (AREA)

Abstract

The invention provides a modified attapulgite material and its preparation and application methods. The modified attapulgite is prepared by: ultrasonically treating attapulgite in HCL solution, filtering, washing, drying, heating to 350+/-5 DEG C for activation, and cooling to room temperature to obtain intermediate A; dissolving MnCl2.4H2O in isopropanol, adding the intermediate A, stirring and ultrasonically processing, adding potassium permanganate solution, refluxing at 87+/-2 DEG C, cooling to room temperature, filtering by suction, washing with isopropanol solution until a clear liquid is formed, and drying at 80-100 DEG C. Through acid activation and thermal activation, specific surface area is enlarged, attachment active sites for bivalent manganese ions are increased; the activated attapulgite can adsorb bivalent manganese ions under anhydrous condition, and it is possible to effectively avoid the competition between water and the bivalent manganese ions; the number of the bivalent manganese ions is under control, it is guaranteed that post-adsorbing solution contains few bivalent manage ions, and no influence is caused to further reaction.

Description

A kind of modified attapulgite soil material and methods for making and using same thereof
Technical field
The present invention relates to a kind of uranium adsorbing material, the present invention also relates to the preparation method of a kind of uranium adsorbing material, this Invention further relates to the application process of a kind of uranium adsorbing material.
Background technology
Attapulgite is again Paligorskite, be a kind of have chain layer structure containing Shuifu County's magnesium silicate clay mineral, at mineral Sepiolite group is belonged on.Attapulgite contains the crystal lattice structure on certain both sides, there is variable amount of Ca2+、Fe3+、Mg2+、 Al3+, its chemical molecular formula substantially is: Mg5Si8O20(OH)2(OH2)4·4H2O.The concrete structure of attapulgite is by 8 four Face body composition, Si therein4+Can be by Al3+And Fe3+Plasma is replaced, Mg2+Can also be on a small quantity by Fe2+And Al3+Ion generation Replace.
The crystal of attapulgite is nano-scale fiber shape, needle-like or fiber collection shape, and specific surface is big, belongs to natural nano knot Structure material, low cost.And there are certain plasticity and a cohesive force, especially in terms of to the sewage disposal containing heavy metal ion There is important application prospect.But attapulgite self is susceptible to reunite, and the absorption property of self is limited, generally will be by modification Mode improve its absorption property.
Summary of the invention
It is an object of the invention to provide the modified attapulgite soil material that a kind of adsorption capacity is big, the purpose of the present invention also exists In the preparation method of a kind of modified attapulgite soil material of offer, the present invention also aims to provide a kind of attapulgite modified material The application process of material.
The modified attapulgite soil material of the present invention is uniformly to wrap up one layer of manganese dioxide nano layer on the surface of attapulgite.
The preparation method of the modified attapulgite soil material of the present invention is:
Attapulgite is placed in supersound process in HCl solution, and after filtering and cleaning up, 80 ± 5 DEG C are dried, intensification 350 ± 5 DEG C of activation processing, are cooled to room temperature, obtain intermediate A；
By MnCl2·4H2O is dissolved in isopropanol, adds described intermediate A, adds potassium permanganate after stirring and being ultrasonic Solution, after 87 ± 2 DEG C reflux 30～60min, be cooled to room temperature, after sucking filtration, with aqueous isopropanol clean to liquid clarify, 80～ 100 DEG C are dried, and obtain the attapulgite of modification.
The modified attapulgite soil material of the present invention is used for adsorption uranium.
The main object of the present invention is on the basis of making full use of the feature that attapulgite specific surface area is big, equal on its surface One layer of manganese dioxide nano layer of even parcel.But attapulgite is nanoscale club shaped structure, existing mode is difficult on its surface Realize one layer of nanometer layer manganese dioxide of homoepitaxial.
The Technology Ways of the present invention is first to adhere to bivalent manganese on its surface by absorption, electrostatic, ion exchange Ion, further by dismutation reaction, manganese dioxide nano layer in the growth of its surface in situ.
But complete this invention path, it is necessary to solve two technical problems: the first, attapulgite's surface to have and fills The avtive spot of the attachment divalent manganesetion divided, this guarantee shows to adhere to divalent manganesetion.The second, in dismutation reaction solution Divalent manganesetion concentration low, on the one hand if divalent manganesetion concentration is high, the dioxy not wrapping up attapulgite can be generated On the other hand change manganese, also result in manganese dioxide layer in uneven thickness, sunburner or manganese dioxide granule occurs on surface Phenomenon.
Based on the understanding to above-mentioned technical problem, the technological means that technical scheme is taked specifically includes that
(1) acid activation, thermal activation.
On the one hand acid activation, the purpose of thermal activation increase specific surface area, on the other hand activate the surface of attapulgite, increase The avtive spot of the attachment of divalent manganesetion.
(2) anhydrous condition absorption divalent manganesetion
Attapulgite after activation adsorbs divalent manganesetion at anhydrous condition, can be prevented effectively from water and divalent manganesetion pair Competition in avtive spot.Absorption will substantially reduce the activation effect of thermal activation in aqueous.Therefore anhydrous condition absorption It is an entirety with early stage activation.
(3) divalent manganesetion quantity is controlled
Control divalent manganesetion quantity, it is ensured that after absorption, in solution, divalent manganesetion quantity is relatively low, not to reaction further Impact.
Three above technological means mutually restricts, and influences each other, and collectively forms an entirety, it is ensured that the reality of goal of the invention Existing.Thermal activation and anhydrous absorption have obvious connection；Fully activation and also do not have the competition guarantee of water do not have manganese from The residue of son.
Accompanying drawing explanation
Fig. 1 be before modified after attapulgite XPS figure；
Fig. 2 a to Fig. 2 d is the TEM collection of illustrative plates of modified attapulgite；
Fig. 3 is the XPS collection of illustrative plates of different sample；
Fig. 4 a to Fig. 4 d is the TEM figure of the attapulgite after adsorption uranium；
Fig. 5 is the XRD figure spectrum of different sample.
Detailed description of the invention
Illustrate below and the present invention is described in more detail.
1g attapulgite is placed in the HCl solution of 15ml, 0.2mol/L, ultrasonic 10-30min, filters, use deionized water Cleaning, after filtration, 80 DEG C of dry 4h, heat up 350 DEG C of activation 2-10h, is cooled to room temperature, it is thus achieved that intermediate A；
0.2g MnCl2·4H2O is added in 100mL isopropanol, adds intermediate A, stirring ultrasonic 10-after dissolving 30min, stirs 30-120min, adds the potassium permanganate solution of 10-20mL0.04mol/L, stirring, and reflux after 87 DEG C 30- 60min, is cooled to room temperature；Sucking filtration, the aqueous isopropanol with 30% cleans to liquid clarification；80-100 DEG C of baking oven is dried 1.5- 2h, it is thus achieved that modified attapulgite.
The feature of above-mentioned steps is described as follows:
(1) acid activation: attapulgite is after acid soak, and internal structure can be partly dissolved, and undissolved part plays a supportive role, Making duct number increase, specific surface area increases.Meanwhile, often containing the impurity such as carbonate, acidification one in attapulgite duct Aspect can remove the impurity being distributed in attapulgite duct, makes duct dredge, and strengthens permeability；On the other hand, due to concavo-convex The cation interchangeability of rod soil, the H that radius is less+Attapulgite stone interlayer portion K can be displaced+、Na+、Ca2+And Mg2+Deng Ion, increases pore volume so that it is absorption property is higher.
(2) thermal activation: owing to containing the structure in absorption water, zeolite water, partially crystallizable water, octahedron in attapulgite Water, can be sloughed by high-temperature roasting, can remove the water of different conditions in crystal structure when heating, and internal structure becomes Loose porous, thus increase specific surface area, increase avtive spot, strengthen absorption affinity.But activation temperature 350 DEG C will not be to structure Produce impact.
(3) acid activation and conventional treatment mode that thermal activation is attapulgite, the feature of the application is by after activation Mesosome A is placed in the aqueous isopropanol of bivalent manganese, the most activated after attapulgite there is substantial amounts of avtive spot, can be direct Bivalent manganese is adsorbed, it is to avoid water is for the impact of absorption.Therefore acid activation, thermal activation and Non-aqueous processing have collaborative Effect.
(4)0.2g MnCl 2·4H2O is added in 100mL isopropanol, adds intermediate A, stirring ultrasonic 10-after dissolving 30min, stirs 30-120min.Early stage stirring ultrasonic 10-30min purpose be attapulgite after on the one hand making activation with On the other hand divalent manganesetion is fully contacted, and avoids occurring attapulgite to reunite, when intermediate A the most fully adsorb bivalent manganese from After son, can effectively suppress agglomeration to occur, remove ultrasonic, adsorb remaining divalent manganesetion further.Experiment detection table Bright: the adsorption ratio of divalent manganesetion is more than 92%.
(5) pretreatment and the synergism of divalent manganesetion quantity.Divalent manganesetion quantity is very few, and modified effect is paid no attention to Think；Divalent manganesetion quantity is too much, can cause residue, causes not wrapping up attapulgite containing substantial amounts of in the material of final production The manganese dioxide of soil, the activation of early stage can improve the absorbability for bivalent manganese with increasing specific surface area simultaneously.In the application On the one hand divalent manganesetion quantity can meet the modified requirement for attapulgite, on the other hand avoids divalent manganesetion Residue.
(6) adding the potassium permanganate solution of 10-20mL0.04mol/L, stirring, reflux after 87 DEG C 30-60min.Add height Potassium manganate, so that sexavalence manganese ion and the absorption divalent manganesetion generation dismutation reaction on attapulgite, generates titanium dioxide Manganese.Backflow is so that reaction carries out more abundant.
(7) clean to liquid clarification with the aqueous isopropanol of 30%；80-100 DEG C of baking oven is dried 1.5-2h.30% different Propanol solution can remove the remaining potassium permanganate of reaction, is prone to dry simultaneously.Obtain after 80-100 DEG C of baking oven is dried 1.5-2h Obtain the attapulgite material of manganese dioxide parcel.
Fig. 1 be before modified after attapulgite XPS figure, wherein A be attapulgite, B be modified attapulgite.This figure Show to show to have wrapped up manganese dioxide at attapulgite.
Fig. 2 a to Fig. 2 d is the TEM collection of illustrative plates of modified attapulgite, and this figure shows to show to have wrapped up nanoscale two at attapulgite Manganese oxide layer.
The modified attapulgite soil material of the present invention is used for adsorption uranium, and this is attapulgite modified in uranium capacity and adsorption mechanism side Mask has an unexpected effect.
The first, adsorption capacity aspect
Attapulgite modified solution ph be 6,298K time uranium adsorption capacity be 2844.87mg/g；Recessed to relevant modification The effectiveness comparison of the uranium absorption of convex rod soil is as shown in the table:
The second, the absorption property to low concentration
The absorption of low concentration uranium has important value in terms of the later stage process of nuclear waste water, and the present invention have chosen 5.0, and 10.0, Uranium solution under 50.0,100.0ppb tetra-variable concentrations is at pH=8.0, and under the conditions of 25 DEG C, the clearance to uranium is ground Study carefully.The uranium solution of variable concentrations being poured into conical flask 50ml respectively, adds the modified attapulgite of 20mg wherein, vibrate 24h, from The heart, takes supernatant, measures residue uranium concentration.It can be seen that modified attapulgite to the uranium clearance of low concentration more than 70.This table Bright low concentration wastewater is processed after reach discharge standard aspect there is important using value.
3rd, adsorption mechanism aspect
Fig. 3 is the XPS collection of illustrative plates of different sample, and wherein, A is modified attapulgite, and B is the attapulgite after adsorption uranium.Figure 4a to Fig. 4 d is the TEM figure of the attapulgite after adsorption uranium.Fig. 5 is the XRD figure spectrum of different sample, and wherein, A is modified concavo-convex Rod, B is the modified attapulgite after adsorption uranium.
The structure of the attapulgite after adsorption uranium and pattern all there occurs the change of essence, and this shows that modified attapulgite uranium adsorbs During there occurs obvious chemical reaction, this is the main cause of adsorption capacity super large, the dioxy that its basic reason is ultra-thin Change the structure of manganese layer.

Claims (3)

1. a modified attapulgite soil material, is characterized in that: be uniformly to wrap up one layer of manganese dioxide to receive on the surface of attapulgite Rice layer.
2. a preparation method for the modified attapulgite soil material described in claim 1, is characterized in that:
Attapulgite is placed in supersound process in HCl solution, and after filtering and cleaning up, 80 ± 5 DEG C are dried, heat up 350 ± 5 DEG C Activation processing, is cooled to room temperature, obtains intermediate A；
By MnCl2·4H2O is dissolved in isopropanol, adds described intermediate A, stirring ultrasonic rear addition potassium permanganate molten Liquid, after 87 ± 2 DEG C reflux 30～60min, be cooled to room temperature, after sucking filtration, with aqueous isopropanol clean to liquid clarify, 80～ 100 DEG C are dried, and obtain the attapulgite of modification.
3. an application for the modified attapulgite soil material described in claim 1, is characterized in that for adsorption uranium.
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Cited By (7)

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Publication number Priority date Publication date Assignee Title
CN106622113A (en) * 2017-01-18 2017-05-10 湖南大学 Preparation and application of attapulgite stabilizing delta-MnO2
CN108525640A (en) * 2017-03-03 2018-09-14 沈金池 A kind of modified technique improving attapulgite absorption property
CN108587566A (en) * 2018-07-24 2018-09-28 东莞市兆荣节能科技有限公司 A kind of preparation method of phase-change material suspension agent aid
CN109289761A (en) * 2018-10-24 2019-02-01 山西新华化工有限责任公司 The method for preparing formaldehyde protective materials is modified to recessed soil
CN109847716A (en) * 2018-12-10 2019-06-07 哈尔滨工程大学 It is a kind of using natural minerals be base extraction of uranium from seawater adsorbent and preparation method thereof
CN110205132A (en) * 2019-05-28 2019-09-06 安徽大学 A kind of preparation method and application of PERFORMANCE OF MODIFIED VERMICULITE-montmorillonite composite material
CN110575812A (en) * 2019-09-25 2019-12-17 西南石油大学 environment-friendly adsorbing material for efficient phosphorus removal of argil/pyrolusite and preparation method thereof

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CN102709057A (en) * 2012-05-23 2012-10-03 天津大学 Method for preparing composite of grapheme with different oxidation degrees and manganese dioxide
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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106622113A (en) * 2017-01-18 2017-05-10 湖南大学 Preparation and application of attapulgite stabilizing delta-MnO2
CN108525640A (en) * 2017-03-03 2018-09-14 沈金池 A kind of modified technique improving attapulgite absorption property
CN108587566A (en) * 2018-07-24 2018-09-28 东莞市兆荣节能科技有限公司 A kind of preparation method of phase-change material suspension agent aid
CN108587566B (en) * 2018-07-24 2021-03-23 东莞市兆荣节能科技有限公司 Preparation method of phase-change material suspending agent assistant
CN109289761A (en) * 2018-10-24 2019-02-01 山西新华化工有限责任公司 The method for preparing formaldehyde protective materials is modified to recessed soil
CN109847716A (en) * 2018-12-10 2019-06-07 哈尔滨工程大学 It is a kind of using natural minerals be base extraction of uranium from seawater adsorbent and preparation method thereof
CN109847716B (en) * 2018-12-10 2021-12-24 哈尔滨工程大学 Natural mineral-based uranium extraction adsorbent from seawater and preparation method thereof
CN110205132A (en) * 2019-05-28 2019-09-06 安徽大学 A kind of preparation method and application of PERFORMANCE OF MODIFIED VERMICULITE-montmorillonite composite material
CN110575812A (en) * 2019-09-25 2019-12-17 西南石油大学 environment-friendly adsorbing material for efficient phosphorus removal of argil/pyrolusite and preparation method thereof
CN110575812B (en) * 2019-09-25 2022-03-22 西南石油大学 Environment-friendly adsorbing material for efficient phosphorus removal of argil/pyrolusite and preparation method thereof

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