CN104525117B - Preparation method and usage of carbon-based epsilon-MnO2 high-efficiency arsenic adsorption material - Google Patents

Preparation method and usage of carbon-based epsilon-MnO2 high-efficiency arsenic adsorption material Download PDF

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CN104525117B
CN104525117B CN201410856026.6A CN201410856026A CN104525117B CN 104525117 B CN104525117 B CN 104525117B CN 201410856026 A CN201410856026 A CN 201410856026A CN 104525117 B CN104525117 B CN 104525117B
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carbon
cotton
solution
cotton gossypii
mno2
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CN104525117A (en
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卿恩平
田熙科
杨祥
杨超
周朝昕
王龙艳
罗东岳
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China University of Geosciences
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China University of Geosciences
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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
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • 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
    • 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
    • B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
    • 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2305/00—Use of specific compounds during water treatment
    • C02F2305/02—Specific form of oxidant

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Analytical Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Inorganic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Hydrology & Water Resources (AREA)
  • Engineering & Computer Science (AREA)
  • Environmental & Geological Engineering (AREA)
  • Water Supply & Treatment (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)

Abstract

The invention provides a preparation method of a carbon-based epsilon-MnO2 high-efficiency arsenic adsorption material. The preparation method comprises the steps that free water in cotton is removed in a freeze drying mode after seeds in the cotton are removed, and in an argon atmosphere, the dried cotton is placed into a tube furnace with good air tightness, and the cotton is subjected to carbonization treatment through temperature rise; the carbonized cotton is ground, the ground cotton is added into a KMnO4 solution, a H2SO4 solution is dropwise added into the KMnO4 solution, ultrasonic dispersion is conducted, and then the solution is stirred fully until ions are evenly dispersed and adsorbed on the surface and internal holes of the cotton; the dispersed solution is transferred into a flask, stirred to conduct a reaction, filtered, washed with absolute ethyl alcohol and ultrapure water and finally subjected to vacuum drying, the carbon-based epsilon-MnO2 high-efficiency arsenic adsorption material can be obtained, and the specific area of the carbon-based epsilon-MnO2 high-efficiency arsenic adsorption material can reach more than 125 m2/g. The carbon-based epsilon-MnO2 high-efficiency arsenic adsorption material can adsorb trivalent arsenic in water, thereby being applicable to water purification engineering.

Description

A kind of Preparation method and use of the efficient arsenic adsorbent material of carbon-based ε type manganese dioxide
Technical field
The invention provides a kind of nanometer titanium dioxide manganese material, the efficient arsenic of more particularly, to a kind of carbon-based ε type manganese dioxide is inhaled Enclosure material, belongs to water technology and application.
Background technology
Arsenic pollution problem has become as a global environmental problem, especially Mongolia, Chile, inland of China platform The ground such as gulf have all occurred in that the Arsenic Contamination in Groundwater of geographic coverage.
Inorganic arsenic existing forms in water body are mainly as () and as ().As () is bigger, more compared with as () toxicity Difficult removal, conventional absorption method has reasonable Adsorption effect to as (), but common adsorbents are straight to as () Connect adsorption effect poor, it usually needs add oxidant such as hydrogen peroxide, free chlorine, as () is oxidized to as by hypochlorous acid etc. (), then pass through Adsorption.This processing mode complex steps, in actual use because water condition is different, using Can be usually limited, the use of simultaneous oxidation agent will also result in secondary pollution for environment.ε type manganese dioxide has relatively low oxidation electricity Gesture, can effectively aoxidize as (), and carbon-based ε type manganese dioxide has higher specific surface, can as () have preferably simultaneously Absorption property.
China's number of applying for a patent: 201210075132.1 publication numbers: cn 102616859a provides a kind of δ type titanium dioxide The method of manganese Adsorption as (), this patent is prepared δ type manganese dioxide for reactant and is used for potassium permanganate and manganese sulfate Arsenious adsorption treatment, the method has a preferable eliminating rate of absorption, but δ type manganese dioxide is to the adsorbance of as () relatively Low, adsorbent service efficiency is relatively low.
The present invention makes full use of the oxidability to as () for the ε type manganese dioxide, makes full use of carbon-based ε type manganese dioxide High-ratio surface, the as () that as () oxidation is obtained has good adsorption capacity, and conventional absorbtion technique than before is simpler Single, cost-effective, and there is more obvious Adsorption effect.
Content of the invention
The invention provides efficient arsenic adsorbent material of a kind of carbon-based ε type manganese dioxide and preparation method thereof, this material removes Trivalent arsenic efficiency high, process is simple, adsorption capacity is big, and adsorbent service efficiency is high.Meanwhile, the synthesis material of this material be easy to get, Inexpensively, preparation process is simple, meets needs of production.
Realizing the technical scheme that above-mentioned purpose of the present invention adopted is:
A kind of preparation method of the efficient arsenic adsorbent material of carbon-based ε type manganese dioxide, comprises the following steps: (1): Cotton Gossypii is gone Remove the free water of Cotton Gossypii after seed using cryodesiccated mode, under argon atmosphere, dried Cotton Gossypii is placed in air-tightness In good tube furnace, be warming up to 800～1100 DEG C with the heating rate of 5～10 DEG C/min, and at this temperature insulation 2～ 5h；
(2): the Cotton Gossypii after carbonization is ground, is added to the kmno that concentration is 0.2～0.4mol/l4Among solution, added The quality of the Cotton Gossypii entering is: 2～5mg/ml, then the h that Deca mass concentration is 20%～40%2so4Solution, the sulphuric acid of institute's Deca Solution and kmno4The volume ratio of solution is 1:5～15, ultrasonic disperse 0.5～1h, is then sufficiently stirred for until uniform ion disperses Absorption is in the surface of Cotton Gossypii and internal void；
(3): the solution after dispersion is transferred in flask, in 120～140 DEG C of stirring reaction 10～15h, with no after filtration Water-ethanol and ultra-pure water cyclic washing, to neutral, be finally vacuum dried at 50～70 DEG C and can be prepared by carbon-based ε type manganese dioxide Efficiently arsenic adsorbent material, its specific surface area reaches 125m2/ more than g.
The efficient arsenic adsorbent material of carbon-based ε type manganese dioxide provided in the present invention can adsorb the trivalent arsenic in water, because This can apply in Water warfare engineering.
Compared with prior art, reaction raw material used in this application is Cotton Gossypii, potassium permanganate and sulphuric acid, all inexpensive easy ?；Meanwhile, synthetic route is simple, controlled, and the yield of carbon-based ε type manganese bioxide material is higher, easily realizes commercial production.Made Standby carbon-based ε type manganese dioxide has preferable oxidation effectiveness to as (), has good adsorptivity, carbon-based ε type two to as () Manganese oxide oxidation-adsorption processes as (), and adsorption capacity is big, and adsorbent service efficiency is high.
Brief description
Fig. 1 is the fesem figure of the Cotton Gossypii after carbonization in the embodiment of the present invention；
Fig. 2 is the tem figure of the Cotton Gossypii after carbonization in the embodiment of the present invention；
Fig. 3 is the xrd diffraction pattern of prepared carbon-based ε type manganese dioxide in the embodiment of the present invention；
Fig. 4 is the bet figure of prepared carbon-based ε type manganese dioxide in the embodiment of the present invention.
Specific embodiment
With reference to specific embodiment, detailed specific description is done to the present invention, but protection scope of the present invention not office It is limited to following examples.
Embodiment 1
Prepare the efficient arsenic adsorbent material method of carbon-based ε type manganese dioxide in the present embodiment, comprise the following steps: Cotton Gossypii is gone Remove the free water of Cotton Gossypii after seed using cryodesiccated mode, under argon atmosphere, dried Cotton Gossypii is placed in air-tightness In good tube furnace, it is warming up to 800 DEG C with the heating rate of 7 DEG C/min, and be incubated 2h at this temperature.
The fesem figure of the Cotton Gossypii after carbonization and tem scheme as depicted in figs. 1 and 2.
Cotton Gossypii after carbonization is ground, is added to the kmno that 50ml concentration is 0.2mol/l4Among solution, the cotton that added The quality of flower is 100mg, then the h that Deca 5ml mass concentration is 30%2so4Solution, ultrasonic disperse 0.8h, then it is sufficiently stirred for straight To uniform ion scattered adsorption in the surface of Cotton Gossypii and internal void；
Solution after dispersion is transferred in flask, in 120 DEG C of stirring reactions 12h, after filtration, uses dehydrated alcohol and ultrapure Water washing, finally at 60 DEG C, vacuum drying can be prepared by the efficient arsenic adsorbent material of carbon-based ε type manganese dioxide, and its specific surface area reaches 125.580m2/g.
The obtained xrd diffraction pattern of the efficient arsenic adsorbent material of ε type manganese dioxide in the present embodiment and bet figure such as Fig. 3 With shown in Fig. 4.
The obtained efficient arsenic adsorbent material of ε type manganese dioxide in the present embodiment, the example processing arsenic-containing water sample is as follows: takes 20ml contains as () 10ppm, the pending water sample of ph6, adds carbon-based ε type manganese dioxide by the adsorbent amount of 0.25g/l, At 25 DEG C, 24h is adsorbed with the speed oscillation of 200rpm, filter to take filtrate and measure as () concentration, calculate carbon-based ε type manganese dioxide Adsorption capacity be 37.04mg/g.
Embodiment 2
Prepare the efficient arsenic adsorbent material method of carbon-based ε type manganese dioxide in the present embodiment, comprise the following steps: Cotton Gossypii is gone Remove the free water of Cotton Gossypii after seed using cryodesiccated mode, under argon atmosphere, dried Cotton Gossypii is placed in air-tightness In good tube furnace, it is warming up to 900 DEG C with the heating rate of 5 DEG C/min, and be incubated 3h at this temperature.
Cotton Gossypii after carbonization is ground, is added to the kmno that 50ml concentration is 0.4mol/l4Among solution, the cotton that added The quality of flower is 250mg, then the h that Deca 10ml mass concentration is 20%2so4Solution, ultrasonic disperse 0.5h, then it is sufficiently stirred for Until uniform ion scattered adsorption is in the surface of Cotton Gossypii and internal void；
Solution after dispersion is transferred in flask, in 140 DEG C of stirring reactions 10h, after filtration, uses dehydrated alcohol and ultrapure Water washing, finally at 50 DEG C, vacuum drying can be prepared by the efficient arsenic adsorbent material of carbon-based ε type manganese dioxide.
Take 20ml to contain as () 8ppm, the pending water sample of ph6, add carbon-based ε type two by the adsorbent amount of 0.25g/l Manganese oxide, adsorbs 24h with the speed oscillation of 200rpm at 25 DEG C, filters to take filtrate and measures as () concentration, calculates carbon-based ε type The adsorption capacity of manganese dioxide is 14.96mg/g.
Embodiment 3
Prepare the efficient arsenic adsorbent material method of carbon-based ε type manganese dioxide in the present embodiment, comprise the following steps: Cotton Gossypii is gone Remove the free water of Cotton Gossypii after seed using cryodesiccated mode, under argon atmosphere, dried Cotton Gossypii is placed in air-tightness In good tube furnace, it is warming up to 1000 DEG C with the heating rate of 8.5 DEG C/min, and be incubated 4h at this temperature.
Cotton Gossypii after carbonization is ground, is added to the kmno that 50ml concentration is 0.3mol/l4Among solution, the cotton that added The quality of flower is 200mg, then the h that Deca 7ml mass concentration is 30%2so4Solution, ultrasonic disperse 0.7h, then it is sufficiently stirred for straight To uniform ion scattered adsorption in the surface of Cotton Gossypii and internal void；
Solution after dispersion is transferred in flask, in 130 DEG C of stirring reactions 15h, after filtration, uses dehydrated alcohol and ultrapure Water washing, finally at 70 DEG C, vacuum drying can be prepared by the efficient arsenic adsorbent material of carbon-based ε type manganese dioxide.
Take 20ml to contain as () 6ppm, the pending water sample of ph6, add carbon-based ε type two by the adsorbent amount of 0.25g/l Manganese oxide, adsorbs 24h with the speed oscillation of 200rpm at 25 DEG C, filters to take filtrate and measures as () concentration, calculates carbon-based ε type The adsorption capacity of manganese dioxide is 11.00mg/g.
Embodiment 4
Prepare the efficient arsenic adsorbent material method of carbon-based ε type manganese dioxide in the present embodiment, comprise the following steps: Cotton Gossypii is gone Remove the free water of Cotton Gossypii after seed using cryodesiccated mode, under argon atmosphere, dried Cotton Gossypii is placed in air-tightness In good tube furnace, it is warming up to 1100 DEG C with the heating rate of 10 DEG C/min, and be incubated 5h at this temperature.
Cotton Gossypii after carbonization is ground, is added to the kmno that 50ml concentration is 0.3mol/l4Among solution, the cotton that added The quality of flower is 150mg, then the h that Deca 4ml mass concentration is 40%2so4Solution, ultrasonic disperse 1h, be then sufficiently stirred for until Uniform ion scattered adsorption is in the surface of Cotton Gossypii and internal void；
Solution after dispersion is transferred in flask, in 130 DEG C of stirring reactions 13h, after filtration, uses dehydrated alcohol and ultrapure Water washing, finally at 60 DEG C, vacuum drying can be prepared by the efficient arsenic adsorbent material of carbon-based ε type manganese dioxide.
Take 20ml to contain as () 4ppm, the pending water sample of ph6, add carbon-based ε type two by the adsorbent amount of 0.25g/l Manganese oxide, adsorbs 24h with the speed oscillation of 200rpm at 25 DEG C, filters to take filtrate and measures as () concentration, calculates carbon-based ε type The adsorption capacity of manganese dioxide is 8.75mg/g.

Claims (2)

1. a kind of preparation method of the efficient arsenic adsorbent material of carbon-based ε type manganese dioxide is it is characterised in that comprise the following steps:
(1): the free water of Cotton Gossypii will be removed after Cotton Gossypii remove seed using cryodesiccated mode, under argon atmosphere, after being dried Cotton Gossypii be placed in the good tube furnace of air-tightness, be warming up to 800～1100 DEG C with the heating rate of 5～10 DEG C/min, and It is incubated 2～5h at a temperature of this；
(2): the Cotton Gossypii after carbonization is ground, is added to the kmno that concentration is 0.2～0.4mol/l4Among solution, the cotton that added The quality of flower is: 2～5mg/ml, then the h that Deca mass concentration is 20%～40%2so4Solution, the sulfuric acid solution of institute's Deca with kmno4The volume ratio of solution is 1:5～15, and then ultrasonic disperse 0.5～1h is sufficiently stirred for until uniform ion scattered adsorption exists The surface of Cotton Gossypii and internal void；
(3): the solution after dispersion is transferred in flask, in 120～140 DEG C of stirring reaction 10～15h, after filtration, uses anhydrous second Alcohol and ultra-pure water cyclic washing to neutral, finally at 50～70 DEG C vacuum drying to can be prepared by carbon-based ε type manganese dioxide efficient Arsenic adsorbent material, its specific surface area reaches 125m2/ more than g.
2. application in Water warfare engineering for the efficient arsenic adsorbent material of carbon-based ε type manganese dioxide described in claim 1, for inhaling Trivalent arsenic in attached water.
CN201410856026.6A 2014-12-31 2014-12-31 Preparation method and usage of carbon-based epsilon-MnO2 high-efficiency arsenic adsorption material Expired - Fee Related CN104525117B (en)

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CN105879830A (en) * 2016-06-29 2016-08-24 广西桂柳化工有限责任公司 Method for preparing manganese dioxide adsorbent
CN112058232B (en) * 2020-09-21 2021-10-22 河南大学 Manganese dioxide modified activated carbon composite adsorbent, preparation method thereof and application thereof in arsenic removal

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