CN105905974A - Application of phosphorus-modified nano flaky aluminium oxide in removal of cadmium ions in water - Google Patents
Application of phosphorus-modified nano flaky aluminium oxide in removal of cadmium ions in water Download PDFInfo
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- CN105905974A CN105905974A CN201610482923.4A CN201610482923A CN105905974A CN 105905974 A CN105905974 A CN 105905974A CN 201610482923 A CN201610482923 A CN 201610482923A CN 105905974 A CN105905974 A CN 105905974A
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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
-
- 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
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/048—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium containing phosphorus, e.g. phosphates, apatites, hydroxyapatites
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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
- B01J20/08—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 comprising aluminium oxide or hydroxide; comprising bauxite
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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
- B01J20/28014—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 form
- B01J20/28033—Membrane, sheet, cloth, pad, lamellar or mat
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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
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (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)
- Water Treatment By Sorption (AREA)
Abstract
The invention discloses application of phosphorus-modified nano flaky aluminium oxide in removal of cadmium ions in water. According to the application, aluminum sulfate and sodium metaaluminate are firstly taken as raw materials for preparing nano flaky boehmite; after that, the obtained nano flaky boehmite is dipped into disodium hydrogen phosphate and then is roasted, so that the phosphorus-modified nano flaky aluminium oxide is obtained; finally, the obtained phosphorus-modified nano flaky aluminium oxide is taken as an adsorbent for removing the cadmium ions in the water. The application is low in raw material price, simple in preparation technology and less in energy consumption, does not produce pollution waste, and is environment-friendly. The prepared phosphorus-modified nano flaky aluminium oxide has larger specific surface area and macropore volume, more negative charges and cadmium ion bonding can be provided by the surface of the phosphorus-modified nano flaky aluminium oxide, and the phosphorus-modified nano flaky aluminium oxide has the cadmium ion adsorption capacity of 355.9mg/ g; the phosphorus-modified nano flaky aluminium oxide has higher adsorption capacity, and the adsorption capacity is superior to those of adsorbing materials reported in literatures, so that the cost for treating cadmium-containing industrial waste water is further lowered.
Description
Technical field
The invention belongs to environmental technology field, particularly to a kind of P Modification nano-sheet aluminium oxide in removing water
Application in terms of cadmium ion.
Background technology
Cadmium is not the indispensable element of human body.Cadmium in human body is absorption from external environment after birth, mainly passes through
Food, water and air and enter body accumulation and get off.Respiratory tract can be produced by cadmium to stimulate, and long-term exposure can cause
Anosmia, gingiva macula lutea or gradually become Huang circle, cadmium compound is difficult to by intestinal absorption, but can through breathe by body
Interior absorption, lodges in liver or kidney works the mischief, especially with the most obvious to kidney damage.Can also result in sclerotin to dredge
Pine and softening, " itai-itai " that the thirties in 20th century, Japan occurred is exactly to be caused by serious cadmium pollution.
Cadmium is very big to harm, and can accumulate in human body, it is impossible to discharging, therefore people must strictly limit
The intake of cadmium processed.The drinking water cadmium content standard limit value of China is 0.005mg/L, World Health Organization's regulation drink
0.003mg/L is must not exceed with cadmium content in water.Cadmium element can be enriched with layer by layer along food chain, therefore in food
Cadmium content also should be severely limited, and wherein the cadmium element in irrigation water is the main source of food cadmium pollution, I
Total cadmium maximum concentration of state's regulation industrial wastewater discharge is 0.1mg/L.
At present, process both at home and abroad the method for cadmium wastewater and be mainly divided into three major types: physical-chemical process, chemical method and
Biotechnology.Physical-chemical process includes: absorption method, ion-exchange-resin process, solvent extraction, membrane separation process,
Evaporation.Absorption method mainly by the loose porous structure of adsorbing material or specific function to heavy metal in water from
Son carries out physical absorption or chemisorbed, and the selection of adsorbent is the core of absorption method.With chemical precipitation method phase
Ratio, absorption method is higher for the clearance of heavy metal ions in wastewater, heavy metal ion remaining in processed waste water
Concentration is relatively low, it is possible to reach wastewater discharge standard requirement.Compared with membrane processing method, the one-time investment of absorption method is relatively
Little, operating cost is the lowest.In prior art, report alumina composite material is removed in water as adsorbent
Cadmium ion, Yang Weichun of such as Central South University et al. has synthesized a kind of mesoporous carbon and has stablized aluminium oxide
(MC/Al2O3), the saturated extent of adsorption of divalent cadmium ion in water is reached 49.98mg/g (Applied Surface
Science,2016,369:215-223).But this method cost is higher, and the highest to the adsorbance of cadmium ion.
Summary of the invention
It is an object of the invention to the deficiency for current cadmium sorption agent adsorption effect, it is provided that a kind of P Modification thin slice
Shape alumina adsorbant, can be widely applied to the removal of cadmium ion in water, big to the saturated extent of adsorption of cadmium ion.
The present invention is that raw material prepares nano-sheet boehmite, then through phosphoric acid initially with aluminum sulfate and sodium metaaluminate
After disodium hydrogen dipping, roasting obtains P Modification nano-sheet aluminium oxide, finally removes in water as adsorbent
Cadmium ion.
The preparation method of P Modification nano-sheet aluminium oxide of the present invention is: by nano-sheet boehmite in matter
Measure in the disodium phosphate soln that concentration is 10-20% and soak 2-12h, after drying at 400-800 DEG C of roasting temperature
2-6h, obtains P Modification nano-sheet aluminium oxide.
The preparation method of described nano-sheet boehmite is: be the aluminum sulfate solution of 10-20% in mass concentration
Middle instillation mass concentration is the sodium aluminate solution of 20-30%, and regulation to pH value is 9-11, the white that will obtain
Suspension is transferred in autoclave, crystallization 6-20h at 90-150 DEG C;It is cooled to room temperature after having reacted, spends
Ionized water washs the white depositions obtained, and is dried to obtain nano-sheet boehmite at 60-100 DEG C.
The thickness of described nano-sheet boehmite is less than 1.5 nanometers.
The thickness of described P Modification nano-sheet aluminium oxide is less than 2.4 nanometers.
Using the P Modification nano-sheet aluminium oxide of above-mentioned preparation as the application of cadmium sorption agent.
Described P Modification nano-sheet aluminium oxide as the using method of cadmium sorption agent is: by 0.001-0.1g
P Modification nano-sheet alumina dispersion, in 100mL water, is stirred at room temperature 2-4h, filters, i.e. gets rid of
Divalent cadmium ion in aqueous solution.
The low in raw material price that the present invention uses, preparation technology is simple, and energy resource consumption is few, and it is useless not produce pollution
Gurry, environmental protection.The P Modification nano-sheet aluminium oxide prepared has large specific surface area and big hole body
Long-pending, its surface is provided that more negative charge and cadmium ion bonding, reaches the adsorption capacity of cadmium ion
355.9mg/g, has relatively high-adsorption-capacity to cadmium ion, is better than the adsorbing material reported in document, drops the most further
The low cost processing industrial waste water containing Cd.
Accompanying drawing explanation
Fig. 1 is the XRD spectra of the P Modification nano-sheet aluminium oxide of the embodiment of the present invention 1 preparation.
Fig. 2 is the transmission electron microscope picture of the P Modification nano-sheet aluminium oxide of the embodiment of the present invention 1 preparation.
Fig. 3 is the saturating of the P Modification aluminium oxide prepared of industrial boehmite that produces of comparative example 1 Shandong Aluminum Plant
Radio mirror figure.
Detailed description of the invention
Embodiment 1
(1) weigh aluminum sulfate solution that 50.0g mass concentration is 10% in beaker, under stirring, be added dropwise over matter
Amount concentration is the sodium aluminate solution of 30%, until pH value is 9;
(2) the uniform white suspension obtained is encapsulated in autoclave, puts into 150 DEG C of baking oven crystallization
6 hours, being cooled to room temperature after having reacted, products therefrom filters, and after being washed with deionized, does in 60 DEG C
Dry;
(3) taking the dried product of 5.0g, immersing 10.0g mass concentration is the disodium phosphate soln of 10%
In, take out after 12h and be dried 2 hours in 60 DEG C;400 DEG C of roasting 2h, obtain P Modification nano-sheet aluminium oxide
P1, testing its specific surface area is 210.2m2/ g, thickness is 2.40nm, and pore volume is 0.71cm3/g;
(4) accurately weigh 0.02gP1, be dispersed in the divalent cadmium ion solution of 100mL100mg/L, magnetic force
Stirring 2h, filters, and is 59.82mg/L with the concentration of cadmium ions in ICP-AES detection filtrate, and adsorption capacity is
200.9mg/g。
Embodiment 2
(1) weigh aluminum sulfate solution that 30.0g mass concentration is 20% in beaker, under stirring, be added dropwise over matter
Amount concentration is the sodium aluminate solution of 30%, until pH value is 11;
(2) the uniform white suspension obtained is encapsulated in autoclave, puts into 130 DEG C of baking oven crystallization
20 hours, being cooled to room temperature after having reacted, products therefrom filters, and after being washed with deionized, does in 80 DEG C
Dry;
(3) taking the dried product of 5.0g, immersing 10.0g mass concentration is the disodium phosphate soln of 10%
In, take out after 12h and be dried 2 hours in 60 DEG C;800 DEG C of roasting 2h, obtain P Modification nano-sheet aluminium oxide
P2, testing its specific surface area is 298.5m2/ g, thickness is 1.69nm, and pore volume is 0.95cm3/g;
(4) accurately weigh 0.02gP2, be dispersed in the divalent cadmium ion solution of 100mL100mg/L, magnetic force
Stirring 2h, filters, and is 56.25mg/L with the concentration of cadmium ions in ICP-AES detection filtrate, and adsorption capacity is
218.8mg/g。
Embodiment 3
(1) weigh aluminum sulfate solution that 30.0g mass concentration is 20% in beaker, under stirring, be added dropwise over matter
Amount concentration is the sodium aluminate solution of 20%, until pH value is 11;
(2) the uniform white suspension obtained is encapsulated in autoclave, puts into 100 DEG C of baking oven crystallization
20 hours, products therefrom filtered, and after being washed with deionized, was dried in 100 DEG C;
(3) taking the dried product of 5.0g, immersing 10.0g mass concentration is the disodium phosphate soln of 20%
In, take out after 12h and be dried 2 hours in 60 DEG C;600 DEG C of roasting 4h, obtain P Modification nano-sheet aluminium oxide
P3, testing its specific surface area is 351.3m2/ g, thickness is 1.43nm, and pore volume is 1.09cm3/g;
(4) accurately weigh 0.02gP3, be dispersed in the divalent cadmium ion solution of 100mL100mg/L, magnetic force
Stirring 4h, filters, and is 42.35mg/L with the concentration of cadmium ions in ICP-AES detection filtrate, and adsorption capacity is
288.2mg/g。
Embodiment 4
(1) weigh aluminum sulfate solution that 50.0g mass concentration is 10% in beaker, under stirring, be added dropwise over matter
Amount concentration is the sodium aluminate solution of 30%, until pH value is 10;
(2) the uniform white suspension obtained is encapsulated in autoclave, puts into 90 DEG C of baking oven crystallization
12 hours, products therefrom filtered, and after being washed with deionized, was dried in 90 DEG C;
(3) take the dried product of 5g, immerse in the disodium phosphate soln that 10g mass concentration is 20%,
Take out after 2h and be dried 2 hours in 60 DEG C;400 DEG C of roasting 6h, obtain P Modification nano-sheet aluminium oxide P4, survey
Trying its specific surface area is 420.1m2/ g, thickness is 1.25nm, and pore volume is 1.20cm3/g;
(4) accurately weigh 0.02gP4, be dispersed in the divalent cadmium ion solution of 100mL100mg/L, magnetic force
Stirring 2h, filters, and is 28.82mg/L with the concentration of cadmium ions in ICP-AES detection filtrate, and adsorption capacity is
355.9mg/g。
Comparative example 1
(1) taking the industrial boehmite PB 5.0g that Shandong Aluminum Plant produces, immersing 10.0g mass concentration is 20%
Disodium phosphate soln in, take out after 12h in 60 DEG C be dried 2 hours;500 DEG C of roasting 4h, obtain P Modification
Aluminium oxide P5, testing its specific surface area is 34.4m2/ g, pore volume is 0.06cm3/g;
(2) accurately weigh 0.02g P5, be dispersed in the divalent cadmium ion solution of 100mL100mg/L, magnetic force
Stirring 4h, filters, and is 97.59mg/L with the concentration of cadmium ions in ICP-AES detection filtrate, and adsorption capacity is
12.05mg/g。
Claims (6)
1. the preparation method of a P Modification nano-sheet aluminium oxide, it is characterised in that it concretely comprises the following steps: will
Nano-sheet boehmite soaks 2-12h in the disodium phosphate soln that mass concentration is 10-20%, after drying
At 400-800 DEG C of roasting temperature 2-6h, obtain P Modification nano-sheet aluminium oxide.
Preparation method the most according to claim 1, it is characterised in that described nano-sheet boehmite
Preparation method be: in the aluminum sulfate solution that mass concentration is 10-20% instill mass concentration be the inclined of 20-30%
Sodium aluminate solution, regulation is 9-11 to pH value, transfers in autoclave by the white suspension obtained,
Crystallization 6-20h at 90-150 DEG C;It is cooled to room temperature after having reacted, is washed with deionized the white precipitate obtained
Thing, is dried to obtain nano-sheet boehmite at 60-100 DEG C.
Preparation method the most according to claim 1, it is characterised in that described nano-sheet boehmite
Thickness less than 1.5 nanometers.
Preparation method the most according to claim 1, it is characterised in that described P Modification nano-sheet oxygen
Change the thickness of aluminum less than 2.4 nanometers.
5. the P Modification nano-sheet aluminium oxide prepared according to claim 1-4 either method is as cadmium ion
The application of adsorbent.
Application the most according to claim 5, it is characterised in that described P Modification nano-sheet aluminium oxide
Using method as cadmium sorption agent is: existed by 0.001-0.1g P Modification nano-sheet alumina dispersion
In 100mL water, it is stirred at room temperature 2-4h, filters, i.e. get rid of the divalent cadmium ion in aqueous solution.
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Cited By (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN115364809A (en) * | 2022-08-23 | 2022-11-22 | 长春工业大学 | Modified alumina adsorbent and preparation method thereof |
CN115611299A (en) * | 2021-07-15 | 2023-01-17 | 北京化工大学 | Nano fibrous boehmite and preparation method thereof |
CN116328714A (en) * | 2023-05-15 | 2023-06-27 | 北京化工大学 | Silicon-phosphorus modified alumina and application thereof to adsorption and regeneration of anionic dye |
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Cited By (4)
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CN116328714A (en) * | 2023-05-15 | 2023-06-27 | 北京化工大学 | Silicon-phosphorus modified alumina and application thereof to adsorption and regeneration of anionic dye |
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