CN107970890A - A kind of hydroxyl iron-loaded modified activated carbon composite material and preparation method thereof - Google Patents
A kind of hydroxyl iron-loaded modified activated carbon composite material and preparation method thereof Download PDFInfo
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- CN107970890A CN107970890A CN201711244659.1A CN201711244659A CN107970890A CN 107970890 A CN107970890 A CN 107970890A CN 201711244659 A CN201711244659 A CN 201711244659A CN 107970890 A CN107970890 A CN 107970890A
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- activated carbon
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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
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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
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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
- B01J20/28—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
- 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
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- 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
- C02F1/00—Treatment of water, waste water, or sewage
- 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
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- 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
- C02F1/288—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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The invention discloses a kind of hydroxyl iron-loaded modified activated carbon composite material and preparation method thereof.The preparation method includes the following steps：（1）Activated carbon is dried, the activated carbon pre-processed is spare through pickling under ultrasound condition with removing surface impurity；（2）The activated carbon of pretreatment is added in iron nitrate solution, after the pH value of the solidliquid mixture adjusted with HCl solution and NaOH solution, is reacted under the conditions of being stirred at room temperature, is placed in aging in constant temperature oven again after reaction；（3）After aging, solid is centrifugally separating to obtain, through rinse, bakees, obtains the hydroxyl iron-loaded modified activated carbon composite material.Preparation method raw material of the present invention is cheap and easy to get, makes simply, and compared with activated carbon, absorption heavy metal ability is improved significantly the hydroxyl iron-loaded modified activated carbon composite material of preparation.
Description
Technical field
The present invention relates to the preparing technical field of absorbent charcoal composite material, and in particular to a kind of hydroxyl iron-loaded modified activated carbon is answered
Condensation material and preparation method thereof.
Background technology
With the fast development of the industries such as mining, smelting and plating, a large amount of discharge of wastewater are into nature, Natural Water weight
Metallic pollution getting worse, constitutes a serious threat safely to drinking water source water quality.Therefore, how low cost, efficiently remove water
Weight metal is most important to ensureing drinking water safety.
At present, conventional drink water purifying method mainly has coagulating sedimentation, electrodialysis, ion exchange and UF membrane etc..These
Although method can remove the heavy metal in drinking water, all there are certain limitation, for example coagulant sedimentation sludge yield is big；Electricity
Dialysis power consumption is high；Ion exchange and membrane separation process impact resistance difference and operating cost height.It is different from the above method, absorption
Method is because with processing method is simple, operating cost is low and the advantage such as easy to operate, being undoubtedly and effectively removing drinking water heavy metal
Method.
In numerous adsorbents, activated carbon is because its duct is enriched, specific surface area is big, high mechanical strength and particle diameter are adjustable excellent
Point, is widely used in drink water purifying.Experimental study and sector application it turns out that, although activated carbon is organic to small molecule
Thing and aromatic hydrocarbon have very strong suction-operated, but its adsorption energy to the especially negatively charged chromium of heavy metal ion, arsenic etc.
Power is very weak, and adsorption capacity is often below 10mg/g, this be primarily due to activated carbon surface functional group be mostly weak electronegative group such as
Hydroxyl, carboxyl and electric charge are weaker.In addition, activated carbon also there are poor selectivity, the rate of adsorption is slow the deficiencies of, seriously constrain activity
Charcoal plays efficiency in clean water treatment, therefore is badly in need of effective, easy and safety method and activated carbon is modified, to improve it
To the removal ability of heavy metal ion in drinking water.
Iron carbonyl is a kind of active mineral being widespread in nature, and has stable chemical property, higher ratio
Surface area and trickle grain structure, the iron epoxide and hydroxyl on its surface are to the negative heavy metal ion in water and positive heavy metal
Ion all has very strong adsorption capacity, can synchronously go negative and positive heavy metal ion in water removal, but iron carbonyl was using
Easily assemble agglomerating in journey and its activity is drastically declined, and the hydroxyl iron particle after reaction is difficult to separate from solution because tiny.
In view of this, iron carbonyl modification activated carbon is used in research, and hydroxyl iron particle is uniformly distributed in activated carbon surface
And duct, this composite material had not only solved the problems, such as that iron carbonyl easily reunited and is difficult to separate from solution after, but also was expected to
While activated carbon specific surface area is not greatly lowered, increases substantially it by iron carbonyl and adsorb the ability of heavy metal, realize
The technique that negative and positive heavy metal ion synchronously removes.
The content of the invention
In view of the above-mentioned deficiencies in the prior art, it is an object of the present invention to provide one kind, to prepare hydroxyl iron-loaded modified activated carbon compound
The method of material.The preparation method is raw material using activated carbon that is cheap, being readily available and ferric nitrate, using activated carbon as load
Body, ferric nitrate are modifying agent, and hydroxyl iron-loaded modified activated carbon composite material is prepared through easy steps, without complicated technique bar
Part and production equipment can improve the performance of activated carbon adsorption heavy metal.
The present invention also aims to provide a kind of hydroxyl iron-loaded modified activated carbon composite material made from the preparation method.
The iron carbonyl absorbent charcoal composite material is expected to the place for being applied to drinking water treatment, even burst mode tra nsmitter on a large scale
Reason, to ensure that drinking water safety provides new method.
The purpose of the present invention is achieved through the following technical solutions.
A kind of preparation method of hydroxyl iron-loaded modified activated carbon composite material, includes the following steps：
(1) by activated carbon through pickling under ultrasound condition to remove surface impurity, dry, the activated carbon pre-processed is standby
With；
(2) activated carbon of pretreatment is added in iron nitrate solution, after the pH value of the solidliquid mixture adjusted, in
Reacted under the conditions of being stirred at room temperature, be placed in aging in constant temperature oven again after reaction；
(3) after aging, solid is centrifugally separating to obtain, through rinse, is bakeed, is obtained the hydroxyl iron-loaded modified activated carbon and answer
Condensation material.
Further, in step (1), the particle diameter of the activated carbon is 150 mesh.
Further, in step (1), the solution of the pickling is 0.1mol/L HCl solutions.
Further, in step (1), the time of pickling is 15min under the ultrasound condition.
Further, in step (1), the temperature of the drying is 100 DEG C.
Further, in step (2), the activated carbon of the pretreatment and the solid-liquid ratio of iron nitrate solution are 4.48：100g/
mL。
Further, in step (2), the concentration of the iron nitrate solution is 0.1~1.0mol/L, is preferably 0.1mol/
L。
Further, in step (2), described to adjust the obtained pH of solidliquid mixture to be with concentration be 0.1mol/L
HCl solution and NaOH solution are adjusted；.
Further, in step (2), the adjusting pH value is to adjust pH value as 7.
Further, in step (2), the time of the reaction is 12h.
Further, in step (2), the temperature of the aging is 70 DEG C, and the time of aging is 12h.
Further, in step (3), the rinse is that rinse to cleaning solution is in neutrality.
Further, in step (3), the baking is to dry 12h at 70 DEG C.
A kind of hydroxyl iron-loaded modified activated carbon composite material as made from the preparation method described in any of the above-described, with activated carbon
For carrier loaded inorganic material hydroxyl iron particle, specific surface area 770m2The content of/g, Fe are 2.3wt%.
Compared with the existing prior art, the invention has the advantages that and beneficial effect：
(1) present invention can be efficiently used iron carbonyl and carry out modification to activated carbon, and iron carbonyl modification is prepared
Absorbent charcoal composite material；The absorbent charcoal composite material being modified by iron carbonyl not only remains the huge specific surface area of activated carbon,
Chemical stability is also enhanced, the ability of its absorption heavy metal has compared with activated carbon before modified to be greatly improved；
(2) present invention is using activated carbon that is cheap, being readily available and ferric nitrate as raw material, by simple technique system
Standby to obtain hydroxyl iron-loaded modified activated carbon composite material, low to the equipment and technological requirement of production, of low cost, production efficiency is high,
Industrialized production easy to implement；
(3) preparation process of the present invention is simple, and the loading process of iron carbonyl, only in an oven can be complete without high-temperature roasting
Into.
Brief description of the drawings
Fig. 1 is hydroxyl iron-loaded modified activated carbon composite material scanning electron microscope (SEM) figure prepared by embodiment 1；
Fig. 2 is hydroxyl iron-loaded modified activated carbon composite material X-ray diffraction (XRD) figure prepared by embodiment 1.
Embodiment
Technical solution of the present invention is described in further detail below in conjunction with specific embodiment and attached drawing, but the present invention
Embodiment and protection domain not limited to this.
Embodiment 1
The preparation of hydroxyl iron-loaded modified activated carbon composite material, comprises the following steps：
(1) it is particle diameter is miscellaneous to remove surface with 0.1mol/L HCl solutions ultrasound pickling 15min for the activated carbon of 150 mesh
Matter, is dried for standby at 100 DEG C.
(2) weigh the activated carbons of the 4.48g after step (1) processing and to add 100mL 0.1mol/L ferric nitrates molten
In liquid, obtain solidliquid mixture, with concentration be 0.1mol/L HCl solution and NaOH solution adjust mixture pH value be 7；
Solidliquid mixture is then reacted into 12h with magnetic stirrer at ambient temperature, then is positioned over aging in 70 DEG C of baking ovens
12h。
(3) solid after step (2) aging is centrifuged, rinse to neutrality obtains hydroxyl after bakeing 12h at 70 DEG C
Iron-loaded modified activated carbon composite material.
The scanning electron microscope (SEM) photograph (SEM) of the hydroxyl iron-loaded modified activated carbon of preparation is as shown in Figure 1, as shown in Figure 1, hydroxyl iron particle
Particle diameter be 0.1-1 μm, be evenly distributed in activated carbon surface and duct.
The hydroxyl iron-loaded modified activated carbon composite material of preparation is that specific surface area is 770m2The content of/g, Fe are 2.3wt%.
Since iron load capacity is less than 3%, activated carbon itself specific surface area and adsorption site quantity do not have to be decreased obviously, this will make work
Property charcoal absorption small molecule organic pollution and the ability of aromatic hydrocarbon be maintained, and assign its new function, make removing heavy metals
Ability be improved significantly.
The X-ray diffractogram (XRD) of the hydroxyl iron-loaded modified activated carbon of preparation is as shown in Fig. 2, as shown in Figure 2, preparation is answered
Occur the characteristic peak of iron carbonyl in condensation material, illustrate that activated carbon surface has iron carbonyl generation.
By the hydroxyl iron-loaded modified activated carbon composite material of preparation and activated carbon respectively to chromium ion (sexavalence), cadmium ion (two
Valency) carry out simulated solution Static Adsorption contrast experiment.
0.2g/L hydroxyl iron-loaded modified activated carbon composite materials and 0.2g/L activated carbons are separately added into chromium ion solution and cadmium
In solion, wherein the concentration of chromium ion solution is 2.5mg/L, and the concentration of cadmium-ion solution is 3.0mg/L, and experimental result is such as
Shown in table 1.
The absorption property comparative test result of 1 hydroxyl iron-loaded modified activated carbon composite material of table and activated carbon
As known from Table 1, the activated carbon being modified by iron carbonyl is before modified respectively to the adsorbance of chromium ion and cadmium ion
5 times and 4 times, by iron carbonyl be modified activated carbon can greatly improve adsorption capacity of the activated carbon to heavy metal.
Above example is only preferrred embodiment of the present invention, is only used for explaining the present invention, is not intended to limit the present invention, this
Field technology personnel without departing from spirit of the invention with made under principle any change, replacement, combine, simplification, modification
Deng should be equivalent substitute mode, should be included within the scope of the present invention.
Claims (10)
1. a kind of preparation method of hydroxyl iron-loaded modified activated carbon composite material, it is characterised in that include the following steps：
（1）Activated carbon is dried, the activated carbon pre-processed is spare through pickling under ultrasound condition with removing surface impurity；
（2）The activated carbon of pretreatment is added in iron nitrate solution, after the pH value of the solidliquid mixture adjusted, in room temperature
Reacted under stirring condition, be placed in aging in constant temperature oven again after reaction；
（3）After aging, solid is centrifugally separating to obtain, through rinse, bakees, obtains the hydroxyl iron-loaded modified activated carbon composite wood
Material.
A kind of 2. preparation method of hydroxyl iron-loaded modified activated carbon composite material according to claim 1, it is characterised in that step
Suddenly（1）In, the solution of the pickling is 0.1 mol/L HCl solutions；The time of pickling is 15min under the ultrasound condition.
A kind of 3. preparation method of hydroxyl iron-loaded modified activated carbon composite material according to claim 1, it is characterised in that step
Suddenly（1）In, the particle diameter of the activated carbon is 150 mesh；The temperature of the drying is 100 DEG C.
A kind of 4. preparation method of hydroxyl iron-loaded modified activated carbon composite material according to claim 1, it is characterised in that step
Suddenly（2）In, the activated carbon of the pretreatment and the solid-liquid ratio of iron nitrate solution are 4.48：100 g/mL；The iron nitrate solution
Concentration be 0.1 ~ 1.0 mol/L.
A kind of 5. preparation method of hydroxyl iron-loaded modified activated carbon composite material according to claim 1, it is characterised in that step
Suddenly（2）In, HCl solution and NaOH solution that it is 0.1 mol/L with concentration that the pH for the solidliquid mixture that the adjusting obtains, which is,
It is adjusted；The adjusting pH value is to adjust pH value as 7.
A kind of 6. preparation method of hydroxyl iron-loaded modified activated carbon composite material according to claim 1, it is characterised in that step
Suddenly（2）In, the time of the reaction is 12 h.
A kind of 7. preparation method of hydroxyl iron-loaded modified activated carbon composite material according to claim 1, it is characterised in that step
Suddenly（2）In, the temperature of the aging is 70 DEG C, and the time of aging is 12 h.
A kind of 8. preparation method of hydroxyl iron-loaded modified activated carbon composite material according to claim 1, it is characterised in that step
Suddenly（3）In, the rinse is that rinse to cleaning solution is in neutrality.
A kind of 9. preparation method of hydroxyl iron-loaded modified activated carbon composite material according to claim 1, it is characterised in that step
Suddenly（3）In, the baking is that 12 h are dried at 70 DEG C.
10. a kind of hydroxyl iron-loaded modified activated carbon composite material made from claim 1 ~ 9 any one of them preparation method, it is special
Sign is, using activated carbon as carrier loaded inorganic material hydroxyl iron particle, specific surface area is 770 m2The content of/g, Fe is
2.3wt%。
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Cited By (4)
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| CN109967134A (en) * | 2019-03-14 | 2019-07-05 | 华南理工大学 | A kind of Nano ferric hydroxide modified anion resin composite materials and the preparation method and application thereof |
| CN111111615A (en) * | 2019-12-27 | 2020-05-08 | 扬州大学 | Preparation method of coralline-like charcoal/hydrated iron oxide composite arsenic removal agent |
| KR20210054208A (en) * | 2019-11-05 | 2021-05-13 | 나노화인 주식회사 | Process for Preparation Arsenic Adsorption Activated Carbons and Activated Carbons Prepared Thereby |
| 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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| 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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| Publication number | Publication date |
|---|---|
| CN107970890B (en) | 2022-09-20 |
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