CN106311123A - Preparation method of water body molybdate adsorbent based on solid waste steel slag - Google Patents
Preparation method of water body molybdate adsorbent based on solid waste steel slag Download PDFInfo
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- CN106311123A CN106311123A CN201610977861.4A CN201610977861A CN106311123A CN 106311123 A CN106311123 A CN 106311123A CN 201610977861 A CN201610977861 A CN 201610977861A CN 106311123 A CN106311123 A CN 106311123A
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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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- 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
- 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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- Organic Chemistry (AREA)
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- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a preparation method of a water body molybdate adsorbent based on solid waste steel slag, belonging to the field of water body pollutant adsorbing materials. The preparation method comprises the following steps: (1) grinding steel slag, rinsing and naturally drying; (2) carrying out particle size screening, and modifying the obtained solid respectively with sulfuric acid, lanthanum chloride and cetyl trimethylammonium bromide (CTMAB); and (3) cleaning with deionized water, and drying to obtain the La-CTMAB-modified steel slag adsorbing material. After the ground surface sewage with the molybdate concentration of 5 mg/L is treated by the adsorbing material, the water body molybdate content reaches the Groundwater Quality Standard (GB/T14848-9) Class IV (<=0.5 mg/L). The method has the characteristics of low cost, high adsorption efficiency, wide applicability and the like, implements waste recycling, and brings in favorable social benefits and economic benefits.
Description
Technical field
The invention belongs to water body pollutant adsorbing material field, be specifically related to a kind of molybdate sewage disposal adsorbing material
Preparation, be related specifically to a kind of composite adsorbing material based on solid waste and preparation method thereof.
Background technology
Molybdenum is one of necessary trace element of animals and plants existence, is also strategy money important in the national economic development simultaneously
Source.The chemical form of heavy metal molybdenum has changeableness, generally exists with two oxides form in nature, and one is tetravalence
State molybdenum, one is hexavalent state molybdenum.In sour environment, molybdate is easily concentrated fixing, and under alkalescence and oxidation environment, molybdic acid
Salt can be re-released in environment.Owing to molybdenum ore production technique is the most backward, alkalescence molybdic tailing management intensity is inadequate, causes part
Area water body molybdenum polution is the most serious.Molybdenum exceeds standard not only to know from experience people and produces serious harm, as comprehensive in produced headache, gout
The symptom such as disease, arteriosclerosis, and animals and plants are also had obvious toxic action.To this end, China is to subsoil water and life drink
It is strict with respectively with the molybdenum concentration in water, subsoil water IV class molybdenum concentration≤0.5mg/L, drinking water molybdenum concentration < 0.07mg/
L.And the most efficient, the molybdate removed in water of low cost, solve the surrounding area surface water huge sum of money that molybdic tailing draining causes
Belong to molybdenum polution, it has also become one of current water environment pollution prevention emphasis research direction.
Currently the minimizing technology to molybdate sewage mainly has chemical precipitation, ion exchange, membrane filtration, and absorption four kinds
Type.Chemical precipitation method is easily generated secondary pollution, and ion exchange and membrane filtration typically require the highest operation expense, and later stage
Operation easier is bigger.Therefore, the molybdate using absorption method to remove in sewage has the most wide application prospect.It is typically used as
Inorganic, the organic material of adsorbent are often difficult to reach eco-friendly requirement.Such as the ceramsite carrier in inorganic adsorbing material,
May require that a large amount of clay in preparation process, not only the industrial land with present tense clashes, and sintering preparation process is also simultaneously
Mass energy can be consumed；And organic adsorption material is typically from petroleum derivation product, it is non-renewable resources.
In adsorbing material investigative technique, some technology utilizing prepared from steel slag for adsorbing material are there are.As, Chinese patent
Application number 201210425931.7, authorized announcement date on October 31st, 2012.Which disclose a entitled " a kind of utilization
The method of slag processing dyeing waste water " patent document；Chinese Patent Application No. 201310119161.8, authorized announcement date 2014
On December 17,.Which disclose the patent literary composition of a entitled " a kind of novel C r (VI) adsorbent and preparation method thereof "
Part；Chinese Patent Application No. 201510764403.8, January 20 2016 Shen Qing Publication day.Which disclose a title
For the patent document of " a kind of subsoil water Compound Heavy Metals repair materials ", this preparation method of restoration materials is to be lived by Exocarpium cocois (Cocos nucifera L)
Property charcoal, zeolite, slag, bentonite and sharp state type nano titanium oxide is baking mixed obtains, although preparation process is simple, but former
Expect relatively costly.Separately, Chinese Patent Application No. 201610275611.6, August 17 2016 Shen Qing Publication day.This patent is open
The patent document of a entitled " a kind of method utilizing solid waste slag processing polluted-water ", this patent adsorbing material is main
It is through nitric acid, sulphuric acid, hydrochloric acid or the acetum of 10-98% by slag, carries out according to the ratio of slag with acid volume 1:1-1:5
Modification, dries at a temperature of 40-150 DEG C after rinsing with clear water and is prepared from.This processing method is mainly for eutrophic water
Body and part heavy metal-polluted water, unknown to the absorbability in anion state molybdate.
In molybdate absorption investigative technique, there is also the patent of related fields.As, Chinese Patent Application No.
201310291466.7, on 01 14th, 2015 Shen Qing Publication day, disclosed portion is entitled " molybdic in a kind of removing water
Method " patent document；Chinese Patent Application No.: 201210212913.0, on October 03 2012 Shen Qing Publication day, discloses
The patent application document of a entitled " processing method of the molybdenum-containing acid wastewater that a kind of ammonium molybdate produces during generating ", with
And China Patent No.: 200710179661.5, authorized announcement date on 09 21st, 2011, disclosed entitled " a kind of containing molybdic acid
The processing method of property waste water ".But the process of above-mentioned technology and operating cost are higher, operating process is complicated.
Summary of the invention
Present in technology for existing removal water body molybdate, operating cost is high, operating difficulties, easily causes secondary dirty
The deficiency of dye, the invention provides the preparation method of a kind of water body molybdate adsorbent based on solid waste slag, to
Both realized the purpose that preparation process is easy, operating cost is low, improve the absorbability to molybdate, be also salvage property simultaneously
Source utilization provides effective way.
For solving the problems referred to above, the present invention adopts the following technical scheme that.
The preparation method of a kind of water body molybdate adsorbent based on solid waste slag of the present invention, specifically includes as follows
Step:
(1) being put into by slag and wash away 2d in clear water, carry out afterwards grinding, rinsing, natural drying, screening obtains particle diameter
The slag of below 0.15mm.
(2) by the H of 1.0-3.0mol/L2SO4Solution joins above-mentioned slag, and vibrate 8-10h, and vibration velocity is 200r/min, it
After be washed with water to not contain SO4 2-, air-dry standby.
(3) solid that step (2) obtains is put in conical flask, and add the LaCl of 0.01-0.03mol/L3·6H2O
Solution, seals conical flask and is placed in 30-35 DEG C of constant temperature oscillator, with the velocity fluctuation 2-4h of 150-200r/min, filters
And collection obtains solid material.
(4) solid material that step (3) obtains is joined in the CTMAB solution of 0.02-0.04mol/L, at 25-45 DEG C
Vibrate in water-bath 12-15h, is washed with deionized to neutrality, and this solid material is placed in the baking oven of 80-100 DEG C after filtration
Middle drying, obtains La-CTMAB modified steel scoria adsorbing material, is: water body molybdate adsorbent.
As one optimization, described slag is desulfurization slag.In all slags, the absorption of molybdate is imitated by desulfurization slag
Fruit is optimal.
Adsorbing material based on solid waste of the present invention is that slag is acidified, carried metal lanthanum and grafting
Functional group and obtain.The present invention utilizes described slag originally as porous solid, and specific surface area is relatively big, after being modified it
Adsorbing water body molybdate, concrete principle is presumed as follows:
As pH value 2.0-7.0, in La-CTMAB modified steel scoria, the group on lanthanum hydroxide surface is mainly with La-OH2 +And La-
OH form exists, and lanthanum hydroxide surface is positively charged generally；And as pH value 7.0-11.0, hydrogen in La-CTMAB modified steel scoria
The group on lanthana surface is mainly with La-OH and La-O-Form exists, and lanthanum hydroxide surface is electronegative generally.Meanwhile, warp
CTMAB is modified, the ammonium termination that CTMAB itself is carried and the Ca of slag itself2+、Mg2+Deng generation ion exchange, thus draw
Entering the carbon long-chain molecule of cationic surfactant, there is more hydrophobic active site in this long-chain, it is possible to preferably by lanthanum
Grain is adsorbed in surface.
Molybdate existing forms in water body is sufficiently complex, is highly prone to the impact of pH.When pH is 2.0-4.6, molybdenum
The existing forms of acid ion mainly has Mo7O21(OH)3 3-、Mo7O22(OH)2 4-、Mo7O23(OH)5-、Mo7O24 6-.Reaction system warp
After dilute sulfuric acid acid adjustment, La-CTMAB modified steel scoria has stronger complexing (as shown in Equation 1) to molybdate, and molybdate is cloudy simultaneously
Ion and the La-OH with positive charge2 +Electrostatic attraction (as shown in Equation 2) can occur in the solution, promote La-CTMAB modified
The slag comprehensive absorbability to molybdenum acid ion, thus realize removing the purpose of water body molybdate.
S-La-OH+MoxOy z-→S-La-MoxOy z-+OH- (1)
S-La-OH2 ++MoxOy z-→S-La-OH2 +-MoxOy z- (2)
Wherein, S is adsorbing material surface, MoxOy z-For polymorphic molybdenum acid ion.
Compared to prior art, the invention have the benefit that
(1) the La-CTMAB modified steel scoria that prepared by the present invention has certain pore structure and surface chemistry, to water body
Molybdate adsorption rate is high (when Mo concentration is 5.0mg/L, clearance is up to more than 95%).Molybdate concentration is the earth's surface of 5mg/L
Sewage is after adsorbing material of the present invention processes, and water body molybdate content reaches groundwater quality standard (GB/T 14848-9) IV class
(≤0.5mg/L)。
(2) rejected material solid that the present invention uses is slag, and this absorption raw material is the conventional solid refuse in steel industry,
Wide material sources, cheap.Meanwhile, slag itself possesses certain mechanical strength, thus expands it as adsorbing material
Range of application.
(3) saturated material is adsorbed repeatable as molybdenum adsorbing material after backwash, and the recovered process of the molybdenum of eluting
After can be further with.The present invention not only achieves the recycling of garbage, also brings good social benefit simultaneously
And economic benefit.
Accompanying drawing explanation
Fig. 1 is the preparation flow schematic diagram of the present invention.
Fig. 2 is the scanning electron microscope (SEM) photograph in the embodiment of the present invention 1 before La-CTMAB modified steel scoria absorption molybdenum acid ion；
It may be seen that modified slag adsorbing material surface texture more disperses, mainly due to lanthanoid metal ion
Insert adsorbing material interlayer with CTMAB to cause.
Fig. 3 is the scanning electron microscope (SEM) photograph in the embodiment of the present invention 1 after La-CTMAB modified steel scoria absorption molybdenum acid ion；
It may be seen that material surface structure is comparatively dense after absorption molybdenum acid ion, ectonexine space is relatively reduced.
Fig. 4 is the affecting laws curve that the adsorbing material that the embodiment of the present invention 1 is prepared by pH value of solution removes molybdenum acid ion
Figure (experiment condition by: being tried Mo concentration is 5mg/L；Adsorption temp is 25 DEG C；Adsorbing material is 0.1g, molybdenum solution 50mL)；
It may be seen that adsorption process is affected relatively big by environment acid-base condition, adsorption efficiency is higher in acid condition.
Fig. 5 is the La-CTMAB modified steel scoria adsorption isotherm (experiment condition to molybdenum acid ion in the embodiment of the present invention 1
For: adsorption temp is 25 DEG C；Solution system pH is 4.5；Adsorbing material is 0.1g, molybdenum solution 50mL)；
It can be seen that along with the increase of molybdenum equilibrium concentration, adsorption capacities of materials is gradually increased and tends to constant；Adsorption process
Meet Langmuir isotherm adsorption model, show that adsorption process mainly top layer is adsorbed as main.
Detailed description of the invention
In conjunction with accompanying drawing, the present invention is described in more detail, but not as a limitation of the invention.
Embodiment 1
Being put into by desulfurization slag and wash away 2d in clear water, carry out afterwards grinding, rinsing, natural drying, screening obtains particle diameter
The slag 20g of below 0.15mm.By the H of 1.0mol/L2SO4Solution 50mL joins in above-mentioned slag, and vibrate 10h, and vibration velocity is
200r/min, is washed with water to not contain SO afterwards4 2-, air-dry standby；Take above-mentioned solid 10g and put into the conical flask of 500mL,
And join the LaCl of 0.01mol/L3·6H2In O solution 200mL, conical flask is sealed and is placed in 35 DEG C of constant temperature oscillators,
With the velocity fluctuation 2h of 200r/min, filter and collect and obtain solid material；This solid material is joined 0.02mol/L's
In CTMAB solution 200mL, vibrate in 25 DEG C of water-baths 13h, is washed with deionized to neutrality after filtration, and by this solid material
Material is placed in the baking oven of 100 DEG C and dries, and is La-CTMAB modified steel scoria 1.
Embodiment 2
Being put into by desulfurization slag and wash away 2d in clear water, carry out afterwards grinding, rinsing, natural drying, screening obtains particle diameter
The slag 20g of below 0.15mm.By the H of 3.0mol/L2SO4Solution 50mL joins in above-mentioned slag, and vibrate 8h, and vibration velocity is
200r/min, is washed with water to not contain SO afterwards4 2-, air-dry standby；Take above-mentioned solid 10g and put into the conical flask of 500mL,
And add the LaCl of 0.01mol/L3·6H2O solution 200mL, seals conical flask and is placed in 35 DEG C of constant temperature oscillators, with
The velocity fluctuation 2h of 200r/min, filters and collects and obtain solid material；This solid material is joined 0.03mol/L's
In CTMAB solution 200mL, vibrate in 30 DEG C of water-baths 12h, is washed with deionized to neutrality after filtration, and by this solid material
Material is placed in the baking oven of 100 DEG C and dries, and is La-CTMAB modified steel scoria 2.
Embodiment 3
Being put into by desulfurization slag and wash away 2d in clear water, carry out afterwards grinding, rinsing, natural drying, screening obtains particle diameter
The slag 20g of below 0.15mm.By the H of 3.0mol/L2SO4Solution 50mL joins in above-mentioned slag, and vibrate 8h, and vibration velocity is
200r/min, is washed with water to not contain SO afterwards4 2-, air-dry standby；Take above-mentioned solid 10g and put into the conical flask of 500mL,
And add the LaCl of 0.03mol/L3·6H2O solution 200mL, seals conical flask and is placed in 35 DEG C of constant temperature oscillators, with
The velocity fluctuation 2h of 200r/min, filters and collects and obtain solid material；This solid material is joined 0.04mol/L's
In CTMAB solution 200mL, vibrate in 45 DEG C of water-baths 15h, is washed with deionized to neutrality after filtration, and by this solid material
Material is placed in the baking oven of 100 DEG C and dries, and is La-CTMAB modified steel scoria 3.
Embodiment 4
With embodiment 3, except that test slag is converter slag.
Embodiment 5
With embodiment 3, except that the H of 1.0mol/L2SO4Solution joins above-mentioned slag, and vibrate 10h.
Embodiment 6
With embodiment 3, it is placed in 30 DEG C of constant temperature oscillators except that conical flask seals, with the speed of 200r/min
Vibration 4h.
Comparative example
Being put into by slag in clear water and wash away 2d, carry out afterwards grinding, rinsing, natural drying, screening obtains particle diameter 0.15mm
Following slag, by it directly as molybdenum adsorbing material.
The slag adsorbing material prepared in above-described embodiment 1-6 and comparative example is carried out respectively except molybdenum absorption test,
Experimental water uses sodium molybdate (Na2MoO4) autogamy molybdenum sewage, its Mo (VI) concentration is 5.0mg/L.Adsorbing material 0.1g, molybdenum
Acid salt solution 50mL, adsorption time is 10h, and dilute sulfuric acid regulation pH value of solution is 4.5, and water temperature is 25 DEG C, and hunting speed is 150r/
min。
Test data show, the molybdate in sewage is had very by the adsorbing material obtained in embodiment of the present invention 1-6
Significantly removal efficiency (as shown in table 1).When molybdate concentration is 5.0mg/L, adsorbing material 1-6 is obvious to the clearance of molybdenum
Clearance higher than contrast adsorbing material.
The different embodiment of table 1 is except molybdenum experimental result
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Comparative example | |
| Mo equilibrium concentration (mg/L) | 0.21 | 0.16 | 0.08 | 0.17 | 0.14 | 0.10 | 1.88 |
| Clearance (%) | 95.80 | 96.80 | 98.40 | 96.60 | 97.20 | 98.00 | 62.40 |
Claims (2)
1. the preparation method of a water body molybdate adsorbent based on solid waste slag, it is characterised in that include walking as follows
Rapid:
(1) slag is put into clear water washes away 2d, carry out afterwards grinding, rinsing, natural drying, screening obtain particle diameter 0.15mm with
Under slag；
(2) by the H of 1.0-3.0mol/L2SO4Solution joins above-mentioned slag, and vibrate 8-10h, and vibration velocity is 200r/min, uses afterwards
Water washs to no longer containing SO4 2-, air-dry standby；
(3) solid that step (2) obtains is put in conical flask, and add the LaCl of 0.01-0.03mol/L3·6H2O is molten
Liquid, seals conical flask and is placed in 30-35 DEG C of constant temperature oscillator, with the velocity fluctuation 2-4h of 150-200r/min, filters also
Collection obtains solid material；
(4) solid material that step (3) obtains is joined in the CTMAB solution of 0.02-0.04mol/L, 25-45 DEG C of water-bath
Middle vibration 12-15h, is washed with deionized after filtration to neutrality, and this solid material is placed in the baking oven of 80-100 DEG C baking
Dry, obtain La-CTMAB modified steel scoria adsorbing material.
A kind of preparation method of water body molybdate adsorbent based on solid waste slag, its
Being characterised by, described slag is desulfurization slag.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107899555A (en) * | 2017-11-30 | 2018-04-13 | 安徽工业大学 | One kind removes the preparation and application of the composite adsorbing material of heavy metal in water Mo (VI) |
| CN108295806A (en) * | 2017-12-06 | 2018-07-20 | 柳州市柳晶科技股份有限公司 | A kind of method and application preparing desulfuration adsorbent using Industrial Solid Waste |
| CN113578914A (en) * | 2021-06-02 | 2021-11-02 | 长安大学 | Steel slag strengthening treatment method integrating physicochemical reaction |
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| CN101264441A (en) * | 2008-05-09 | 2008-09-17 | 成都信息工程学院 | Modified steel scoria adsorbent and preparation thereof |
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| CN101264441A (en) * | 2008-05-09 | 2008-09-17 | 成都信息工程学院 | Modified steel scoria adsorbent and preparation thereof |
| JP2011006616A (en) * | 2009-06-26 | 2011-01-13 | Bridgestone Corp | Tire |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107899555A (en) * | 2017-11-30 | 2018-04-13 | 安徽工业大学 | One kind removes the preparation and application of the composite adsorbing material of heavy metal in water Mo (VI) |
| CN107899555B (en) * | 2017-11-30 | 2020-05-01 | 安徽工业大学 | Preparation and application of composite adsorbing material for removing heavy metals Mo (VI) in water body |
| CN108295806A (en) * | 2017-12-06 | 2018-07-20 | 柳州市柳晶科技股份有限公司 | A kind of method and application preparing desulfuration adsorbent using Industrial Solid Waste |
| CN108295806B (en) * | 2017-12-06 | 2019-11-15 | 柳晶（长春）环保科技有限公司 | A kind of method and application preparing desulfuration adsorbent using Industrial Solid Waste |
| CN113578914A (en) * | 2021-06-02 | 2021-11-02 | 长安大学 | Steel slag strengthening treatment method integrating physicochemical reaction |
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Application publication date: 20170111 |