CN106669590A - Heavy metal mesoporous adsorbent material with molybdenum ore tailings as raw material as well as preparation method and application thereof - Google Patents
Heavy metal mesoporous adsorbent material with molybdenum ore tailings as raw material as well as preparation method and application thereof Download PDFInfo
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- CN106669590A CN106669590A CN201611260580.3A CN201611260580A CN106669590A CN 106669590 A CN106669590 A CN 106669590A CN 201611260580 A CN201611260580 A CN 201611260580A CN 106669590 A CN106669590 A CN 106669590A
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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
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- 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
- B01J20/041—Oxides or hydroxides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- 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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- 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
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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
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Abstract
The invention belongs to the technical field of heavy metal pollution treatment for environment and discloses a heavy metal mesoporous adsorbent material with molybdenum ore tailings as raw material as well as a preparation method and an application thereof. The preparation method comprises steps as follows: an alkaline sodium compound is added after molybdenum ore tailings are subjected to acid pickling, the mixture is heated in a muffle furnace and dissolved in water, sodium metaaluminate and water glass are added to a supernatant, the mixture is uniformly mixed and transferred to a reactor to react, an obtained reaction liquid is purified after the reaction ends, and the heavy metal mesoporous adsorbent material is obtained. The mesoporous adsorbent material prepared with the method has a very good adsorption effect on heavy metals, has the removal rate of 95% or above even under the condition that the concentration of heavy metal solutions is up to 420 mg*L<-1>, is stable at adsorption, has no secondary pollution risk and can be applied to heavy metal wastewater treatment. Besides, the characteristics of the raw material, namely, molybdenum ore tailing waste, is fully utilized, waste is treated by waste while the product quality is improved, the preparation process is simple, and industrial production promotion is facilitated.
Description
Technical field
The invention belongs to Heavy-Metal-Contaminated Environments processing technology field, more particularly to a kind of is raw material based on molybdenum ore tailings
Heavy metal mesoporous adsorption material and its preparation method and application.
Background technology
With the increasingly shortage of water resource, craving of the mankind to water resource is more and more stronger, but water pollution problem
Increasingly severe, this causes available water resource less.Therefore the problem for the treatment of pollutant effluents already turns into worldwide asking
Topic.Particularly in developing country, the environmental problem of a large amount of discharges of pollutant effluents, or even the barrier for advancing as country and developing
Hinder.The features such as heavy metal pollution has toxicity, not biodegradable and accumulation property, is present in water body environment and seriously threatens people
Health and life.What National Bureau of Statistics of the People's Republic of China write《China Statistical Yearbook》In mention China in 2014
Discharge of wastewater has reached surprising 71,617,510,000 tons.
Heavy metal classes pollutant once enters water body, is merely able to by changing form or being transferred, dilute, accumulate, and
Can not be degraded, even and if the pollution of very low concentrations also can do harm to huamn body.Cadmium, is wherein the one of heavy metal element
Kind, it is a kind of very big soft metal of toxicity, it is not belonging to needed by human body element.Its most compound all have it is water-soluble,
And with toxicity, therefore once enter water body, it is easy to unconsciously entering food chain, and enrichment, prestige in human body
Coerce human health.Cadmium is enriched in liver, pancreas, stomach and thyroid gland into people's cognition, and kidney can be made to produce irreversible disease
Become, cause osteoporosis, angiocardiopathy, nervous system and immune system are damaged.China《Integrated wastewater discharge mark
It is accurate》And《Drinking Water hygienic quality specification》The concentration limit of the cadmium of middle clear stipulaties is 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 major types.Its
Middle chemical method mainly includes the precipitation method and electrolysis；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 for utilize cellular structure, is mesh
One of method of pre-treatment industrial waste water containing Cd.The key technology of absorption method is the selection of adsorbent, common sorbing material bag
Include zeolite, activated carbon etc..Activated carbon has very strong adsorption capacity, and clearance is high, but regenerating active carbon efficiency is low, and water quality treatment is difficult
Reach reuse requirement, price, using being restricted.Zeolite is natural sorbing material, and specific surface area is big, with very strong suction
Attached ability, is most already applied to the handling process of heavy metal wastewater thereby.In recent years, various suctions of adsorption capacity are gradually developed
Enclosure material.
Utilization rate of the mineral resources when developing be not substantially high, and useful constituent only accounts for small part, most thing
Matter will be as mine 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 there is the environmental risk of pollution.
CHARACTERISTICS OF TAILINGS SAND as trade waste one kind, be a kind of resource for mislaying, current its treatment approach has three
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 as building materials, light industry, Inorganic Chemicals, production such as devitrified glass, architectural pottery, building brick；Last
Plant is, as dispensing, to participate in portland cement, synthesis of mineral material etc..
The content of the invention
In order to overcome the shortcomings and deficiencies of the prior art described above, primary and foremost purpose of the invention is to provide a kind of based on molybdenum ore
Tailings is the preparation method of the heavy metal mesoporous adsorption material of raw material.
Another object of the present invention is offer above method preparation based on the mesoporous suction of heavy metal that molybdenum ore tailings is raw material
Enclosure material.
Still a further object of the present invention is that offer is above-mentioned to be weighed based on the heavy metal mesoporous adsorption material that molybdenum ore tailings is raw material
The application of metallic wastewater treatment.
The purpose of the present invention is realized by following proposal：
A kind of is the preparation method of the heavy metal mesoporous adsorption material of raw material based on molybdenum ore tailings, specifically includes following step
Suddenly：
(1) milled 200 mesh sieve of molybdenum ore tailings, adds dilute acid soln to be vibrated in shaking table, is separated by filtration, and dries, then
It is sub-packed in crucible, each crucible adds alkaline sodium compound, then the heat altogether in Muffle furnace, then takes out natural cooling, grinds
It is stand-by.
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 consumption of dilute acid soln used remains to be totally submerged molybdenum ore tailings with the dilute acid soln under oscillating condition
It is accurate.
Vibration described in step (1) refers to the 240rmin in horizontal reciprocating oscillator-112h is vibrated under speed.
Alkaline sodium compound described in step (1) can be sodium carbonate or NaOH, preferably NaOH.
In crucible described in step (1) dry after molybdenum ore tailings and alkaline sodium compound mass ratio for (0.6~
1):1。
The common heat in Muffle furnace described in step (1) refers in 1~3h of the common heat of 573K~973K.
Described in step (1) grind it is stand-by in the purpose that grinds be more thorough in order to what is dissolved in water.
(2) take step (1) product to be dissolved in water, centrifugal filtration takes supernatant, is transferred in teflon tanks, and adds inclined aluminium
Sour sodium and waterglass control material ratio, fully mix under magnetic agitation；
Addition sodium metaaluminate and waterglass control material described in step (2) is than being that the mol ratio for instigating reaction mass is
(5.5~7.5) Na2O:Al2O3:2.88SiO2:212.4H2O；
Mixing described in step (2) refers to 1~3h of mixing under 333~373K water bath conditions.
(3) reaction mass after being mixed in teflon tanks is transferred in reactor, reactor is put into Muffle furnace or baking
Reacted in case, reaction terminate after take out be cooled to room temperature, filter, washing, dry, obtained powder solid be sodium form with much money
Category mesoporous adsorption material.
The volume of the reaction mass after being mixed in the teflon tanks 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) refers to use 0.01molL-1The NaOH aqueous solution is washed.
It is a kind of by above-mentioned reaction prepare based on molybdenum ore tailings for raw material heavy metal mesoporous adsorption material.
The above-mentioned application based on the heavy metal mesoporous adsorption material that molybdenum ore tailings is raw material in heavy metal containing wastewater treatment.
Mechanism of the invention is：
Mineral wherein active constituent content ore high in ore dressing process is chosen away, and remaining mine tailing main component is two
Silica, alundum (Al2O3).Silica, alundum (Al2O3) are as the main constituents in the earth's crust it is necessary to fabulous environment
Compatibility.It is raw material present invention utilizes the silica and aluminum oxide in molybdenum ore tailings, is activated by acid-base method, by control
The factors such as material ratio processed, basicity, temperature, in the reactor under high pressure synthesis with bigger serface, pore volume aperture it is new
Mineral, make it on the premise of its outstanding environment compatibility is kept, with the characteristic for adsorbing pollutant.
The present invention has the following advantages and beneficial effect relative to prior art：
(1) adsorption effect of mesoporous adsorption material heavy metal prepared by the present invention is very good, even if in heavy metal solution
At concentrations up to 420mgL-1Under, still there is stabilization after more than 95% clearance, and absorption, there is no secondary pollution risk.
(2) primary raw material of mesoporous adsorption material is tailings, using a kind of waste material, realizes the mesh of the treatment of wastes with processes of wastes against one another
's.
(3) characteristic of former molybdenum ore tailings discarded object is made full use of, the quality of product is improved.There is good aluminium in molybdenum ore tailings
Matter and siliceous source, and contain a small amount of K2O、Na2O, beneficial to the stabilization of mesoporous material under alkalescence condition.
(4) preparation process is simple, promotes beneficial to industrial production.
Brief description of the drawings
Fig. 1 is the clearance of the heavy metal mesoporous adsorption material to Cd in the solution containing Cd of various concentrations of the preparation of embodiment 1
Figure.
Specific embodiment
With reference to embodiment and accompanying drawing, the present invention is described in further detail, but embodiments of the present invention are not limited
In this.
Agents useful for same can routinely be bought from market unless otherwise specified in embodiment.
The molybdenum ore tailings used in example comes from Guangdong Province Meizhou Wuhua, and its main chemical compositions (wt%) is：
| 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：It is the preparation of the heavy metal mesoporous adsorption material of raw material based on molybdenum ore tailings
(1) milled 200 mesh sieve of 15g molybdenum ore tailings is taken, the H of 30ml, 1mol/L is added2SO4Vibrated in shaking table, filtering
Separate, drying；It is sub-packed in crucible, the NaOH of the quality such as each crucible addition is warm altogether in the Muffle furnace of 823K, is taken out after 3h
Natural cooling, grinds stand-by.
(2) 5g steps (1) are taken and grinds stand-by product plus 90ml deionized water dissolvings, centrifugal filtration takes supernatant, shifted
Into teflon tanks, and add 5.4g sodium metaaluminates and 15.75g waterglass regulation material ratio, the magnetic agitation under the conditions of 343K
1h。
(3) reaction mass after being stirred in teflon tanks is transferred in reactor, is reacted under the conditions of 373K, instead
Taking-up is cooled to room temperature after answering 8h, filters, and washing is dried, and prepared powder solid is sodium form heavy metal mesoporous adsorption material.
Embodiment 2
With 0.05molL-1Used as supporting electrolyte solution, it is 100mgL to prepare Cd solution concentrations to NaCl solution-1's
Heavy metal ion solution.The metal ion solution of the above-mentioned concentration of 25mL is measured, addition fills the heavy metal of the preparation of 0.1g embodiments 1
In the 50mL centrifuge tubes of sorbing material, each treatment is repeated 3 times, and averages.Excellent centrifuge tube will be added to cover, in 250r
min-1, vibrate 24h under the conditions of (25 ± 2) DEG C, be then 6000rmin in rotating speed-1Lower centrifugation 30min, filtering, is inhaled with atom
Receive the concentration of the Cd ions after AAS (AAS) measure is balanced in solution.
Supernatant C d concentration is 0.25mgL after showing the balance surveyed with the result of sorbing material obtained in NaOH-1,
I.e. handling rate is up to 99.76%.
Embodiment 3
With 0.05molL-1NaCl solution is used as supporting electrolyte solution, and the metal ion that following concentration is prepared respectively is molten
Liquid, Cd solution concentrations:20、30、60、100、140、190、280、420mg·L-1；The metal ion for measuring the above-mentioned concentration of 25mL is molten
Liquid, addition is filled in the 50mL centrifuge tubes of the heavy-metal adsorption material of the preparation of 0.1g embodiments 1, and each treatment is repeated 3 times, and makes even
Average.Excellent centrifuge tube will be added to cover, in 250rmin-1, vibrate 24h under the conditions of (25 ± 2) DEG C, be then in rotating speed
6000r·min-1Lower centrifugation 30min, filtering determines the Cd ions in solution after balancing with atomic absorption spectrophotometry (AAS)
Concentration, so as to draw clearance.
Clearance figure of the heavy-metal adsorption material prepared in embodiment 1 to Cd in the solution containing Cd under various concentrations
As shown in figure 1, being as can be seen from Figure 1 less than 420mgL in Cd concentration-1When, the heavy metal that embodiment 1 is prepared is mesoporous
Sorbing material has all reached more than 98.5% to the clearance of Cd, and preceding 7 concentration (20,30,60,100,140,190,
280mg·L-1) handling rate all reached more than 99.6%, illustrate the present invention preparation sodium form heavy metal mesoporous adsorption material pair
Cd has preferable adsorption effect.
Embodiment 4
In order to probe into heavy metal mesoporous material that embodiment 1 prepares after Adsorption of Heavy Metals, risk in the environment.
Simulated Acid Rain solution is configured according to condition elements such as In Guangzhou Area acid rain constituent, pH value for many years, after Adsorption of Heavy Metals
Material carry out desorption experiment.
Configuration S/N compositions ratio (mass ratio) is 3: 1, and pH value is 3.5 Simulated Acid Rain solution.In taking 25mL and embodiment 3
Cd concentration is 280mgL-1、420mg·L-1Residue mixing (solid-to-liquid ratio 1g after lower absorption:250mL), in 250rmin-1、
24h is vibrated under the conditions of (25 ± 2) DEG C, is then 6000rmin in rotating speed-1Lower centrifugation 30min, filtering, uses atomic absorption spectrophotometry
Photometry (AAS) determines the concentration of the Cd ions in solution after balancing.
Result shows, is 280mgL in Cd concentration-1Residue desorption efficiency after lower absorption is 0.06%, is in Cd concentration
420mg·L-1Residue desorption efficiency is 0.07% after lower absorption.Therefore, material will not be deposited substantially after high concentration heavy metal is adsorbed
Desorbing the possibility that causes secondary pollution.
Above-described embodiment is the present invention preferably implementation method, but embodiments of the present invention are not by above-described embodiment
Limitation, it is other it is any without departing from Spirit Essence of the invention and the change, modification, replacement made under principle, combine, simplification,
Equivalent substitute mode is should be, is included within protection scope of the present invention.
Claims (8)
1. a kind of is the preparation method of the heavy metal mesoporous adsorption material of raw material based on molybdenum ore tailings, it is characterised in that specifically included
Following steps：
(1) milled 200 mesh sieve of molybdenum ore tailings, adds dilute acid soln to be vibrated in shaking table, is separated by filtration, and dries, and then dispenses
In crucible, each crucible adds alkaline sodium compound, then the heat altogether in Muffle furnace, then takes out natural cooling, grinds stand-by；
(2) take step (1) product to be dissolved in water, centrifugal filtration takes supernatant, is transferred in teflon tanks, and add sodium metaaluminate
With waterglass control material ratio, fully mixed under magnetic agitation；
(3) reaction mass after being mixed in teflon tanks is transferred in reactor, during reactor is put into Muffle furnace or baking oven
Reacted, reaction is taken out after terminating and is cooled to room temperature, is filtered, washing is dried, and obtained powder solid is the mesoporous suction of heavy metal
Enclosure material.
2. according to claim 1 is the preparation method of the heavy metal mesoporous adsorption material of raw material based on molybdenum ore tailings, its
It is characterised by：
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 consumption of dilute acid soln used is remained to be totally submerged molybdenum ore tailings and is defined by the dilute acid soln under oscillating condition；
Vibration described in step (1) refers to the 240rmin in horizontal reciprocating oscillator-112h is vibrated under speed.
3. according to claim 1 is the preparation method of the heavy metal mesoporous adsorption material of raw material based on molybdenum ore tailings, its
It is characterised by：
Alkaline sodium compound described in step (1) is sodium carbonate or NaOH；
The mass ratio of molybdenum ore tailings and alkaline sodium compound after being dried in the crucible described in step (1) is (0.6~1):1；
The common heat in Muffle furnace described in step (1) refers in 1~3h of the common heat of 573K~973K.
4. according to claim 3 is the preparation method of the heavy metal mesoporous adsorption material of raw material based on molybdenum ore tailings, its
It is characterised by：
Alkaline sodium compound described in step (1) is NaOH.
5. according to claim 1 is the preparation method of the heavy metal mesoporous adsorption material of raw material based on molybdenum ore tailings, its
It is characterised by：
Addition sodium metaaluminate and waterglass control material described in step (2) are than being that to instigate the mol ratio of reaction mass be (5.5
~7.5) Na2O:Al2O3:2.88SiO2:212.4H2O；
Mixing described in step (2) refers to 1~3h of mixing under 333~373K water bath conditions.
6. according to claim 1 is the preparation method of the heavy metal mesoporous adsorption material of raw material based on molybdenum ore tailings, its
It is characterised by：
The volume of the reaction mass after being mixed in the teflon tanks 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) refers to use 0.01molL-1The NaOH aqueous solution is washed.
7. what a kind of method according to any one of claim 1~6 was prepared is a huge sum of money for raw material based on molybdenum ore tailings
Category mesoporous adsorption material.
8. it is according to claim 7 based on molybdenum ore tailings for raw material heavy metal mesoporous adsorption material at heavy metal wastewater thereby
Application in reason.
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| CN106669590B (en) | 2019-05-07 |
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