CN106622115B - It is a kind of based on the potassium type heavy metal mesoporous adsorption material and its preparation method and application that molybdenum ore tailings is raw material - Google Patents
It is a kind of based on the potassium type heavy metal mesoporous adsorption material and its preparation method and application that molybdenum ore tailings is raw material Download PDFInfo
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- CN106622115B CN106622115B CN201611260596.4A CN201611260596A CN106622115B CN 106622115 B CN106622115 B CN 106622115B CN 201611260596 A CN201611260596 A CN 201611260596A CN 106622115 B CN106622115 B CN 106622115B
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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
- B01J20/16—Alumino-silicates
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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
- B01J20/28078—Pore diameter
- B01J20/28083—Pore diameter being in the range 2-50 nm, i.e. mesopores
-
- 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
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4893—Residues derived from used synthetic products, e.g. rubber from used tyres
-
- 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 belongs to Heavy-Metal-Contaminated Environments processing technology fields, disclose a kind of based on potassium type heavy metal mesoporous adsorption material and its preparation method that molybdenum ore tailings is raw material and application.The preparation method is the following steps are included: by alkaline potassium compound is added after molybdenum ore tailings pickling, the heat together in Muffle furnace, is then dissolved in water, and takes supernatant and sodium metaaluminate and waterglass is added, mixing is reacted, and after reaction purifies products therefrom up to potassium type heavy metal mesoporous adsorption material.The mesoporous adsorption material of this method preparation is very good to the adsorption effect of heavy metal, even if in heavy metal solution at concentrations up to 280mgL‑1Under, still there is 95% or more removal rate, and more stable after absorption heavy metal, there is no secondary pollution risk, can be applicable in heavy metal containing wastewater treatment.And the present invention makes full use of the characteristic of raw material molybdenum ore tailings waste, the purpose of the treatment of wastes with processes of wastes against one another is realized while improving the quality of product, and preparation process is simple, is conducive to industrial production and promotes.
Description
Technical field
The invention belongs to Heavy-Metal-Contaminated Environments processing technology field, in particular to a kind of based on molybdenum ore tailings is raw material
Potassium type heavy metal mesoporous adsorption material and its preparation method and application.
Background technique
With the increasingly shortage of water resource, the mankind are more more and more intense to the craving of water resource, however water pollution problem
Increasingly severe, this causes available water resource less.Therefore the problem of processing pollutant effluents, already becomes worldwide and asks
Topic.Especially in developing country, the environmental problem of pollutant effluents being largely discharged, or even the barrier for advancing and developing as country
Hinder.Heavy metal pollution has the characteristics that toxicity, not biodegradable and accumulation property, is present in water body environment and seriously threatens people
Health and life.Mentioned in the China Statistical yearbook that National Bureau of Statistics of the People's Republic of China writes 2014 it is Chinese
Discharge of wastewater has had reached surprising 71,617,510,000 tons.
Heavy metal classes pollutant is once discharged into water body, is merely able to by changing form or being transferred, dilute, accumulate, and
It cannot be degraded, and can be done harm to huamn body the pollution of very low concentrations.Cadmium is wherein the one of heavy metal element
Kind, it is a kind of soft metal that toxicity is very big, is not belonging to needed by human body element.Its most compound all have it is water-soluble,
And there is toxicity, therefore once enter water body, it is easy to unconsciously enter food chain, and be enriched in human body, prestige
Coerce human health.Cadmium, which enters human body, can be enriched in liver, pancreas, stomach and thyroid gland, and kidney can be made to generate irreversible disease
Become, causes osteoporosis, cardiovascular disease, nervous system and immune system are damaged.China's " integrated wastewater discharge mark
It is quasi- " and " Drinking Water hygienic quality specification " in the concentration limits of cadmium of clear stipulaties be respectively 0.1ppm and 5ppb.
The main source of heavy metal wastewater thereby includes chemical industry, the opening of Pb-Zn deposits, electroplating industry, non-ferrous metal metallurgy, system
The discharge of the waste water such as standby sulfuric acid industry, printing and dyeing textile, pesticide producing.
The method of heavy metal containing wastewater treatment can substantially be divided into physical treatment process, chemical method, biological treatment three categories.Its
Middle chemical method mainly includes the precipitation method and electrolysis method；Physical treatment process includes solvent extraction and separation method, ion-exchange, film point
From and absorption method；Biological treatment includes biosorption process, bio-flocculation process, phytoremediation.
Absorption method is a kind of effective ways of heavy metal ion in the material Adsorption water using cellular structure, is mesh
One of the method for pre-treatment industrial waste water containing Cd.The key technology of absorption method is the selection of adsorbent, common adsorbent material packet
Include zeolite, active carbon etc..Active carbon has very strong adsorption capacity, and removal rate is high, but regenerating active carbon low efficiency, water quality treatment are difficult
Reach reuse requirement, price, using being restricted.Zeolite is natural adsorbent material, and large specific surface area has very strong suction
Attached ability is most already applied to the treatment process of heavy metal wastewater thereby.In recent years, a variety of suctions of adsorption capacity are gradually developed
Enclosure material.
Utilization rate of the mineral resources in development and utilization be not substantially high, and useful constituent only accounts for small part, most object
Matter will become tailing.So resource of tailings is all constantly being accumulated every year, a large amount of CHARACTERISTICS OF TAILINGS SANDs are deposited in Tailings Dam, do not only take up soil
Ground, waste of resource, and polluted environmental risk.
The one kind of CHARACTERISTICS OF TAILINGS SAND as trade waste is a kind of resource mislayed, its treatment approach has three at present
Kind.The first is that with the continuous progress of science and technology, the tailings of fraction can extract useful mineral resources by selecting again；
Second is to produce such as devitrified glass, architectural pottery, building brick as building materials, light industry, Inorganic Chemicals；Last
Kind is to participate in portland cement, synthesis of mineral material etc. as ingredient.
Summary of the invention
In order to overcome the shortcomings and deficiencies of the prior art described above, the primary purpose of the present invention is that providing a kind of based on molybdenum ore
Tailings is the preparation method of the potassium type heavy metal mesoporous adsorption material of raw material.
Another object of the present invention is to provide being situated between based on the potassium type heavy metal that molybdenum ore tailings is raw material for above method preparation
Hole adsorbent material.
Still a further object of the present invention is to provide the above-mentioned potassium type heavy metal mesoporous adsorption material based on molybdenum ore tailings for raw material
Application in heavy metal containing wastewater treatment.
The purpose of the present invention is realized by following proposal:
A kind of preparation method based on the potassium type heavy metal mesoporous adsorption material that molybdenum ore tailings is raw material, specifically includes following
Step:
(1) milled 200 mesh of molybdenum ore tailings is added dilute acid soln and vibrates in shaking table, be separated by filtration, dries, then
It is sub-packed in crucible, alkaline potassium compound, then the heat together in Muffle furnace is added in each crucible, then takes out natural cooling, grinds
For use；
Dilute acid soln described in step (1) can be dilute sulfuric acid aqueous solution or diluted hydrochloric acid aqueous solution, the concentration of dilute acid soln
Preferably 1mol/L；The dosage of dilute acid soln used remains to be totally submerged molybdenum ore tailings with dilute acid soln under oscillating condition
It is quasi-.
Oscillation described in step (1) refers to the 240rmin in horizontal reciprocating oscillator-112h is vibrated under speed.
Alkaline potassium compound described in step (1) can be potassium carbonate or potassium hydroxide, preferably potassium hydroxide.
In crucible described in step (1) dry after molybdenum ore tailings and alkaline potassium compound mass ratio be (0.6~
1):1。
Heat together refers in 1~3h of 573K~973K heat together in Muffle furnace described in step (1).
It is more thorough in order to what is dissolved in water that the purpose ground in stand-by is ground described in step (1).
(2) it takes and grinds stand-by product in step (1) and be dissolved in water, centrifugal filtration takes supernatant, is transferred to teflon tank
In, and sodium metaaluminate and waterglass control material ratio is added, it is mixed well under magnetic agitation；
Addition sodium metaaluminate described in step (2) and waterglass control material ratio are to instigate the molar ratio of reaction mass to be
(4.0~6.0) K2O:(0.5~1.8) Na2O:2.88SiO2:212.4H2O；
Mixing described in step (2) refers to 1~3h of mixing under 333~373K water bath condition.
(3) reaction mass after mixing in teflon tank is transferred in reactor, reactor is put into Muffle furnace or baking
It is reacted in case, is filtered after being cooled to room temperature after reaction, washed, dry, powder solid obtained, that is, potassium type heavy metal
Mesoporous adsorption material.
The volume of reaction mass after mixing in teflon tank described in step (3) is the 2/3 of reactor volume.
Reaction described in step (3) refers to 8~36h of reaction under the conditions of 353~473K.
Washing described in step (3), which refers to, uses 0.01molL-1The washing of NaOH aqueous solution.
A kind of potassium type heavy metal mesoporous adsorption material based on molybdenum ore tailings for raw material being prepared by above-mentioned reaction.
It is above-mentioned based on the potassium type heavy metal mesoporous adsorption material that molybdenum ore tailings is raw material in heavy metal containing wastewater treatment
Using.
Mechanism of the invention are as follows:
Wherein the high ore of active constituent content is chosen away mineral in ore dressing process, and remaining tailing main component is two
Silica, aluminum oxide.Silica, aluminum oxide are as the main constituents in the earth's crust it is necessary to fabulous environment
Compatibility.Present invention utilizes in molybdenum ore tailings silica and aluminium oxide be raw material, activated by acid-base method, pass through control
The factors such as material ratio processed, basicity, temperature, there is bigger serface, hole to hold the novel of aperture for synthesis under high pressure in the reactor
Mineral make it under the premise of keeping its outstanding environment compatibility, have the characteristic of absorption pollutant.
The present invention compared with the existing technology, have the following advantages and the utility model has the advantages that
(1) mesoporous adsorption material prepared by the present invention is very good to the adsorption effect of heavy metal, even if in heavy metal solution
At concentrations up to 280mgL-1Under, still there is 95% or more removal rate, and more stable after mesoporous material absorption heavy metal, does not have
Secondary pollution risk.
(2) primary raw material of mesoporous adsorption material is tailings, using a kind of waste material, the mesh that realizes waste treatment and waste
's.
(3) present invention makes full use of the characteristic of former molybdenum ore tailings waste, improves the quality of product.Have very in molybdenum ore tailings
Good aluminum and siliceous source, and contain a small amount of K2O、Na2O, conducive to the stabilization of mesoporous material under alkaline condition.
(4) preparation process is simple, is conducive to industrial production and promotes.
Detailed description of the invention
Fig. 1 is that the heavy metal mesoporous adsorption material for preparing removes Cd in the solution containing Cd under various concentration in embodiment 1
Except rate figure.
Specific embodiment
Below with reference to embodiment and attached drawing, the present invention is described in further detail, but embodiments of the present invention are unlimited
In this.
Agents useful for same can routinely be bought unless otherwise specified from market in embodiment.
The molybdenum ore tailings used in example is from Guangdong Province, Wuhua, Meizhou, main chemical compositions (wt%) are as follows:
| Molybdenum ore tailings component | SiO2 | Al2O3 | Fe2O3 | TiO3 | Na2O | K2O | MgO | CaO | P2O5 | CuO |
| Content | 78.35 | 10.95 | 1.54 | 0.46 | 1.65 | 3.40 | 0.42 | 0.64 | 0.12 | 0.01 |
Embodiment 1: the preparation of potassium type heavy metal mesoporous adsorption material
(1) milled 200 mesh of 15g molybdenum ore tailings is taken, 30mL, the H of 1mol/L is added2SO4It vibrates, filters in shaking table
Separation, drying；Be sub-packed in crucible, the KOH for the quality such as each crucible is added, molybdenum ore tailings after being dried in each crucible and
The mass ratio of KOH is 0.85:1, the heat together 3h in the Muffle furnace of 823K, takes out natural cooling, is ground stand-by；
(2) it takes 5g step (1) to grind stand-by product and adds 90ml deionized water dissolving, centrifugal filtration takes supernatant, transfer
Into teflon tank, and 5.4g sodium metaaluminate and 15.75g waterglass is added, adjusts material ratio, magnetic agitation under the conditions of 343K
1h。
(3) reaction mass after stirring in teflon tank is transferred in reactor, is reacted under the conditions of 373K, instead
It answers to take out after 8h and be cooled to room temperature, filter, wash, it is dry, powder solid, that is, potassium type heavy metal mesoporous adsorption material is made.
Embodiment 2
With 0.05molL-1For NaCl solution as supporting electrolyte solution, preparation Cd solution concentration is 100mgL-1's
Heavy metal ion solution.The heavy metal ion solution of the above-mentioned concentration of 25mL is measured, addition fills to be prepared in 0.1g embodiment 1
Heavy metal mesoporous adsorption material 50mL centrifuge tube in, each processing is repeated 3 times, and is averaged.Excellent centrifuge tube will be added
It covers, in 250rmin-1, vibrate for 24 hours under the conditions of (25 ± 2) DEG C, be then 6000rmin in revolving speed-1Lower centrifugation 30min,
Filtering, with the concentration of the Cd ion in solution after atomic absorption spectrophotometry (AAS) measurement balance.
Adsorbent material obtained the results show that balance after supernatant C d concentration be 1.39mgL-1, illustrate that handling rate can
Up to 98.65%.
Embodiment 3
With 0.05molL-1For NaCl solution as supporting electrolyte solution, the metal ion for preparing following concentration respectively is molten
Liquid, Cd solution concentration: 20,30,60,100,140,190,280,420mgL-1；The metal ion for measuring the above-mentioned concentration of 25mL is molten
Liquid is added in the 50mL centrifuge tube for filling 0.1g adsorbent material, and each processing is repeated 3 times, and is averaged.Excellent centrifugation will be added
Pipe covers, in 250rmin-1, vibrate for 24 hours under the conditions of (25 ± 2) DEG C, be then 6000rmin in revolving speed-1Lower centrifugation
30min, filtering, with the concentration of the Cd ion in solution after atomic absorption spectrophotometry (AAS) measurement balance.
The potassium type heavy metal mesoporous adsorption material that embodiment 1 is prepared removes the Cd in the Cd solution under various concentration
Except rate as shown in Figure 1, from figure 1 it appears that being lower than 420mgL in Cd concentration-1When, the heavy metal prepared in embodiment 1 is situated between
Hole adsorbent material has reached 77% or more to its removal rate, and preceding 7 concentration (20,30,60,100,140,190,
280mg·L-1) handling rate all reached 95% or more.Illustrate suction of the heavy metal mesoporous adsorption material prepared by the present invention to Cd
Attached effect is very good.
Embodiment 4
In order to probe into potassium type heavy metal mesoporous material that embodiment 1 is prepared after adsorbing heavy metal, in the environment
Risk.Simulated Acid Rain solution is configured according to condition elements such as the acid rain constituent of In Guangzhou Area many years, pH value, to an absorption huge sum of money
Material after category carries out desorption experiment.
Configuring S/N ingredient ratio (mass ratio) is 3: 1, the Simulated Acid Rain solution that pH value is 3.5.Take 25mL acid rain solution and reality
Applying Cd concentration in example 3 is 280mgL-1、420mg·L-1Residue after lower absorption mixes (solid-to-liquid ratio 1g:250mL),
250r·min-1, vibrate for 24 hours under the conditions of (25 ± 2) DEG C, be then 6000rmin in revolving speed-1Lower centrifugation 30min is filtered, and is used
The concentration of Cd ion after atomic absorption spectrophotometry (AAS) measurement balance in solution.
The results show that being 280mgL in Cd concentration-1Residue desorption efficiency after lower absorption is 0.28%, is in Cd concentration
420mg·L-1Residue desorption efficiency is 0.25% after lower absorption.Therefore, material will not be deposited substantially after adsorbing high concentration heavy metal
Desorbing the possibility for causing secondary pollution.
The above embodiment is a preferred embodiment of the present invention, but embodiments of the present invention are not by above-described embodiment
Limitation, other any changes, modifications, substitutions, combinations, simplifications made without departing from the spirit and principles of the present invention,
It should be equivalent substitute mode, be included within the scope of the present invention.
Claims (8)
1. a kind of preparation method based on the potassium type heavy metal mesoporous adsorption material that molybdenum ore tailings is raw material, it is characterised in that specific
The following steps are included:
(1) milled 200 mesh of molybdenum ore tailings is added dilute acid soln and vibrates in shaking table, be separated by filtration, dries, then dispense
In crucible, alkaline potassium compound, then the heat together in Muffle furnace is added in each crucible, then takes out natural cooling, is ground stand-by；
(2) it taking and grinds stand-by product in step (1) and be dissolved in water, centrifugal filtration takes supernatant, it is transferred in teflon tank, and
Sodium metaaluminate is added and waterglass controls material ratio, is mixed well under magnetic agitation；
(3) reaction mass after mixing in teflon tank is transferred in reactor, reactor is put into Muffle furnace or baking oven
It is reacted, is filtered after being cooled to room temperature after reaction, washed, dry, powder solid obtained, that is, potassium type heavy metal is mesoporous
Adsorbent material；
Described in step (2) addition sodium metaaluminate and waterglass control material ratio be instigate reaction mass molar ratio be (4.0
~6.0) K2O:(0.5~1.8) Na2O:2.88SiO2:212.4H2O。
2. the preparation side according to claim 1 based on the potassium type heavy metal mesoporous adsorption material that molybdenum ore tailings is raw material
Method, it is characterised in that:
Dilute acid soln described in step (1) is dilute sulfuric acid aqueous solution or diluted hydrochloric acid aqueous solution, and the concentration of dilute acid soln is 1mol/
L；The dosage of dilute acid soln used is subject to dilute acid soln under oscillating condition and remains to be totally submerged molybdenum ore tailings；
Oscillation described in step (1) refers to the 240rmin in horizontal reciprocating oscillator-112h is vibrated under speed.
3. the preparation side according to claim 1 based on the potassium type heavy metal mesoporous adsorption material that molybdenum ore tailings is raw material
Method, it is characterised in that:
Alkaline potassium compound described in step (1) is potassium carbonate or potassium hydroxide；
The mass ratio of molybdenum ore tailings and alkaline potassium compound after drying in crucible described in step (1) is (0.6~1): 1；
Heat together refers in 1~3h of 573K~973K heat together in Muffle furnace described in step (1).
4. the preparation side according to claim 3 based on the potassium type heavy metal mesoporous adsorption material that molybdenum ore tailings is raw material
Method, it is characterised in that:
Alkaline potassium compound described in step (1) is potassium hydroxide.
5. the preparation side according to claim 1 based on the potassium type heavy metal mesoporous adsorption material that molybdenum ore tailings is raw material
Method, it is characterised in that:
Mixing described in step (2) refers to 1~3h of mixing under 333~373K water bath condition.
6. the preparation side according to claim 1 based on the potassium type heavy metal mesoporous adsorption material that molybdenum ore tailings is raw material
Method, it is characterised in that:
The volume of reaction mass after mixing in teflon tank described in step (3) is the 2/3 of reactor volume；
Reaction described in step (3) refers to 8~36h of reaction under the conditions of 353~473K；
Washing described in step (3), which refers to, uses 0.01molL-1The washing of NaOH aqueous solution.
7. what a kind of methods described in any item according to claim 1~6 were prepared is the potassium type of raw material based on molybdenum ore tailings
Heavy metal mesoporous adsorption material.
8. according to claim 7 useless in heavy metal based on the potassium type heavy metal mesoporous adsorption material that molybdenum ore tailings is raw material
Application in water process.
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