CN106824062A - A kind of lanthanum aluminum composite metal pillared montmorillonite de-fluoridation adsorbent and preparation method thereof - Google Patents
A kind of lanthanum aluminum composite metal pillared montmorillonite de-fluoridation adsorbent and preparation method thereof Download PDFInfo
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- CN106824062A CN106824062A CN201710174429.6A CN201710174429A CN106824062A CN 106824062 A CN106824062 A CN 106824062A CN 201710174429 A CN201710174429 A CN 201710174429A CN 106824062 A CN106824062 A CN 106824062A
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/06—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising oxides or hydroxides of metals not provided for in group B01J20/04
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—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
- 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
- C02F2101/12—Halogens or halogen-containing compounds
- C02F2101/14—Fluorine or fluorine-containing compounds
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/06—Contaminated groundwater or leachate
Abstract
The invention discloses a kind of lanthanum aluminum composite metal pillared montmorillonite de-fluoridation adsorbent and preparation method thereof, the adsorbent includes carrier pillared montmorillonite, active component lanthanum and aluminium, and its preparation process includes montmorillonite sodium, the preparation of pillared liquid, pillared aging, centrifuge washing, the process such as calcines, pulverizes and sieves.The de-fluoridation adsorbent that the present invention is prepared is high to the adsorption capacity of fluorine, be easy to regeneration, do not result in secondary pollution；When using it for high-fluorine drinking water treatment, the Funing tablet after treatment in water reaches national drinking water standard.
Description
Technical field
It is more particularly to a kind of to can be used to the fluorine removal that efficient absorption processes high-fluorine water the invention belongs to water-treatment technology field
Adsorbent and preparation method thereof.
Background technology
Fluorine is one of the essential trace elements of the human body, and taking in appropriate fluorine can effectively pre- anti-caries；But fluorine high is drunk for a long time
Water can then influence the metabolism of in-vivo element, gently then cause fluorine spot tooth, heavy then can cause fluorosis of bone or even make one paralysis.China is existing
Fluoride concentration limit value is 1.0mg/L in standards for drinking water quality regulation water body, and China is that drinking water type is local in the world
Property fluorine poisoning harm most serious one of country.In the wide geographic areas such as China North China, northwest, especially rural area backward in economy,
Underground water fluoride content is generally exceeded, and these area major parts are with underground water as drinking water source, it is necessary to be carried out at fluorine removal to underground water
Reason.
Defluorination method is varied both at home and abroad at present, including chemical precipitation, absorption, ion exchange, counter-infiltration, electrodialysis
Deng wherein absorption method is easy to operate, and cost benefit is higher, is always the important method of Ca reservoir.Its principle is will be fluorine-containing
Water is filtered by special defluoridation filter material, and fluorine occurs the effect such as absorption, ion exchange when by filtrate with adsorbent, raw
Into indissoluble fluoride, with constantly absorption, the fluorine removal ability of filtrate can be reduced constantly, when fluorine removal ability drops to certain limit
Value, i.e. fluorine removal ability reach when being unable to reach setting, it is necessary to regenerative agent regeneration, recovery adsorbent fluorine removal ability, are circulated with this and reached
To the purpose for removing excessive fluoride.The restriction of the main sorbent suspension species of height of defluorination effect, therefore, select suitable adsorbent
It is very crucial.It is used for the active aluminum oxide of sorbing material, bone black and modified zeolite of fluorine removal etc. in the prior art, wherein with activity
Aluminum oxide is most widely used, but activated alumina is influenceed larger by pH value, is also easy to produce secondary pollution, and adsorption capacity is relatively low, right
Weakly alkaline Removal of Fluorine From Underground Water effect is typically presented poor.Adsorption capacity high, preparation process is simple and economical and practical are developed for this
Adsorption-defluorination material, with great environment and economic implications.
Mineral material montmorillonite is widely distributed and cheap in China, is a kind of preferable natural adsorbent.Montmorillonite
It is a kind of layer silicate mineral, the aluminum oxide octahedral sheet structure that its structure is sandwiched in therebetween by two-layer tetrahedral si-o film and a layer
Into.It has structure charge higher, heat endurance, specific surface area and interlayer controllability.Use unmodified natural smectite
It is undesirable to fluorine removal effect, it is necessary to improve its adsorption capacity by modified.Method of modifying mainly has inorganic modified, organically-modified
Etc. technique, it is inorganic modified in metal ion oxide, especially the research of hydroxy Al polymerizing cationically and application are most.But aluminium
Pillared compound montmorillonite adsorbent remains unchanged and there are problems that the sensitive to pH, the consumption to acid, is brought to popularization
Certain difficulty.Rare earth ion and fluorine have good compatibility, but only use rare earth element fluorine removal high cost, and by its
Adsorbent is prepared with the composite modified pillared montmorillonite of aluminium, you can with reduces cost, rare earth element can be made full use of again to the height of fluorine
Selectivity.At present, it is compound less to the research of Adsorbent modification using rare-earth elements of lanthanum and common metal aluminium phase, do not have lanthanum also
The composite modified montmorillonite material of aluminium is used for report and related application technology from removing fluor in water.
The content of the invention
The present invention is intended to provide a kind of lanthanum aluminum composite metal pillared montmorillonite that can efficiently remove fluorine ion in high-fluorine water
De-fluoridation adsorbent and preparation method thereof, to overcome that existing adsorbent adsorption capacity is not high, preparation technology is complicated, preparation cost is high,
Only with rare earth element fluorine removal high cost with the natural smectite of the non-pillared modification shortcoming undesirable to fluorine removal effect.
The present invention solves technical problem, adopts the following technical scheme that：
A kind of lanthanum aluminum composite metal pillared montmorillonite de-fluoridation adsorbent, including carrier and be carried on carrier activity into
Point, the carrier is pillared montmorillonite, and the active component is lanthanum and aluminium.
The preparation method of above-mentioned lanthanum aluminum composite metal pillared montmorillonite de-fluoridation adsorbent, including montmorillonite sodium, pillared liquid
Preparation, pillared aging, centrifuge washing, the process such as calcine, pulverize and sieve, specifically including following steps：
(1) after montmorillonite is mixed with the sodium carbonate for accounting for montmorillonite quality 2-5%, then by montmorillonite and the matter of deionized water
Amount is added in deionized water than being 5%, and stirring 2h, aging 24h obtain montmorillonite suspension；
(2) salt of lanthanum is dissolved in deionized water, is made the salting liquid of the lanthanum of 0.1mol/L；Aluminium chlorohydrate is dissolved in
In ionized water, the liquor alumini chloridi of 0.2mol/L is made；
It is 1 by the mol ratio of lanthanum and aluminium:1-1:50, the salting liquid of the lanthanum and the liquor alumini chloridi are sufficiently mixed,
Stirring obtains lanthanum aluminium mixing salt solution；
(3) NaOH is added in the lanthanum aluminium mixing salt solution so that aluminium and OH-Mol ratio be 2.4：1, acutely stir
2h, aging 24h are mixed, pillared liquid is obtained；
(4) it is 1 by the volume ratio of pillared liquid and montmorillonite suspension:1, the pillared liquid is slowly added into montmorillonite and is hanged
In turbid liquid, stirring 2h, aging 24h are then proceeded to, the 3-5 dissolving salt to wash away residual of centrifuge washing finally will centrifugation gained
Solid is placed in baking oven and is dried to constant weight under the conditions of 105 DEG C, obtains pillared montmorillonite solid；
(5) the pillared montmorillonite solid is placed in Muffle furnace, in 2h is calcined at 100-600 DEG C, is then produced gained
Thing pulverizes and sieves, and obtains the granular materials of particle diameter 0.1-1.0mm, as lanthanum aluminum composite metal pillared montmorillonite de-fluoridation adsorbent.
The salt of the lanthanum is lanthanum nitrate or lanthanum sulfate.
Used as a kind of preferred scheme, in step (2) the lanthanum aluminium mixing salt solution, the mol ratio of lanthanum and aluminium is 1:20；
Used as a kind of preferred scheme, the temperature of step (5) described calcining is 200 DEG C；
As a kind of preferred scheme, supportted with pillared fluid column again after the montmorillonite suspension ultrasonic disperse 20min.
Fluorine ion of the lanthanum aluminum composite metal pillared montmorillonite de-fluoridation adsorbent of the invention suitable for removal underground water.
Compared with the prior art, beneficial effects of the present invention are embodied in：
1st, the present invention utilizes absorption of the adsorbent that the composite compaction technique pillared montmorillonite of lanthanum and aluminium is prepared to fluorine ion
Amount is very high, is significantly higher than single aluminium pillared montmorillonite or other materials, and adsorption rate is fast；And with merely with rare earth as raw material system
The adsorbent for obtaining is compared, and material preparation cost is substantially reduced.
2nd, de-fluoridation adsorbent preparation process is simple of the invention, with short production cycle, it is easy to operate during for fluorine removal, need not
Heating, reaction temperature are low.
3rd, activated alumina is to use most de-fluoridation adsorbents both at home and abroad, and to play its optimal adsorption ability will adjust water
Sample pH value is 5, and processing procedure is big to the consumption of acid, and processing cost is higher, and adsorption capacity is relatively low, is easily caused aluminium element
Dissolution and cause secondary pollution, influence aluminum oxide absorption property.And de-fluoridation adsorbent of the invention be applied to various concentrations,
The water quality of different hardness, with adsorption capacity higher, can use, it is not necessary to adjust the pH value of water, enter one in pH=6-8 scopes
Step has saved fluorine removal cost of water treatment, in neutrality, lanthanum, aluminium are not detected water outlet pH value in the water sample after treatment, it is to avoid secondary dirt
Dye.
Brief description of the drawings
Fig. 1 is adsorption effect of the lanthanum aluminum composite metal pillared montmorillonite de-fluoridation adsorbent in different pH water samples.
Specific embodiment
For a better understanding of the present invention, it is with reference to the example content that the present invention is furture elucidated but of the invention interior
Appearance is not limited solely to following example.
The measuring method of adsorbance of the present invention is as follows：0.1g de-fluoridation adsorbents are added to 100mL containing F-Ion concentration is
In the pending water sample of 5mg/L, 2h (adsorption equilibrium) is vibrated with the condition of 25 DEG C, rotating speed 160r/min in constant temperature oscillation case
Afterwards, the fluorinion concentration in solution is detected with chromatography of ions, adsorption capacity is calculated according to the following formula：
In formula：Q- adsorption capacities (mg/g)；
C0Fluorinion concentration (mg/L) before-absorption；
CeFluorinion concentration (mg/L) after-absorption；
W- adsorbent weights (g)；
V- volume of water sample (mL)；
The computing formula of clearance η (%) is as follows：
The measure of lanthanum ion uses arsenazo Ⅲ AAS in water, and aluminum ions measure uses inductive coupling plasma
Body emission spectroanalysis (ICP) method, high-fluorine water is prepared with chemical pure NaF.
Embodiment 1
The present embodiment prepares lanthanum aluminum composite metal pillared montmorillonite de-fluoridation adsorbent as follows：
(1) 10g montmorillonites and 0.4gNa are weighed2CO3It is put into beaker, it is 5wt%'s to add 200mL water to be made into mass ratio
Suspension, after high-speed stirred 2h, aging 24h, obtains montmorillonite suspension；
(2) a certain amount of La (NO are weighed3)3, it is made the La (NO of 0.1mol/L3)3Solution；Weigh a certain amount of hydration chlorine
Change aluminium, be made the liquor alumini chloridi of 0.2mol/L；
Take the La (NO of 10mL 0.1mol/L3)3Liquor alumini chloridi with 100mL 0.2mol/L mixes so that lanthanum and aluminium
Mol ratio is 1:20, obtain lanthanum aluminium mixing salt solution；
(3) NaOH solution of 20.8mL 0.4mol/L is added in above-mentioned lanthanum aluminium mixing salt solution so that aluminium and OH-
Mol ratio be 2.4, be stirred vigorously 2h, aging 24h, be made pillared liquid；
(4) under high velocity agitation, it is 1 by the volume ratio of pillared liquid and montmorillonite suspension:1, pillared liquid is slowly added dropwise
To in montmorillonite suspension, after completion of dropwise addition, after persistently stirring 2h, at room temperature aging 24h, mixed liquor centrifuge washing 3 times, precipitation
Thing is placed directly within crucible, in 16h is dried at 105 DEG C, obtains pillared montmorillonite solid；
(5) by the solid in the Muffle furnace after 2h is calcined at 200 DEG C, pulverize and sieve, obtain particle diameter 0.1-1.0mm
Grain material, as lanthanum aluminum composite metal pillared montmorillonite de-fluoridation adsorbent.
Weigh lanthanum aluminum composite metal pillared montmorillonite de-fluoridation adsorbent 0.1g to be put into the conical flask of 250mL, add 100mL
Containing F-During ion concentration is for the aqueous solution of 5mg/L, 3 Duplicate Samples are done, vibrate 2h, rotating speed in 25 DEG C of constant temperature oscillators respectively
160r/min.Supernatant liquid filtering (0.45 μm of miillpore filter) is taken, F is surveyed-Content and lanthanum content.
After measured, the lanthanum aluminum composite metal pillared montmorillonite de-fluoridation adsorbent of the present embodiment reaches to removal efficiency of flouride
85.34%, Funing tablet is 0.733mg/L in supernatant, reaches national drinking water standard, and La, Al ion are not detected.
Embodiment 2
The preparation of the present embodiment de-fluoridation adsorbent is with embodiment 1.
The lanthanum aluminum composite metal pillared montmorillonite de-fluoridation adsorbent 0.1g for weighing the present embodiment is put into the conical flask of 250mL
In, add 100mL to contain F-Ion concentration is the aqueous solution of 5mg/L, with HCl or NaOH adjust fluorine solution ph be respectively 2,4,6,
8th, 10,3 Duplicate Samples are done to each pH, 2h, rotating speed 160r/min are vibrated in 25 DEG C of constant temperature oscillators respectively.Take supernatant mistake
Filter (0.45 μm of miillpore filter), surveys F-Content, as a result see Fig. 1.
From figure 1 it appears that when pH is in the range of 6-8, the lanthanum aluminum composite metal pillared montmorillonite of the present embodiment is removed
The adsorption effect of fluorine adsorbent preferably, goes out water fluoridation and has reached domestic drinking water standard.Have in the range of pH wider
Preferable adsorption effect so that lanthanum aluminum composite metal pillared montmorillonite de-fluoridation adsorbent is conducive to the fluorine removal in real process.
Exemplary embodiment of the invention is the foregoing is only, is not intended to limit the invention, it is all of the invention
Any modification, equivalent and improvement made within spirit and principle etc., should be included within the scope of the present invention.
Claims (3)
1. a kind of lanthanum aluminum composite metal pillared montmorillonite de-fluoridation adsorbent, including carrier and the active component being carried on carrier,
It is characterized in that：The carrier is pillared montmorillonite, and the active component is lanthanum and aluminium.
2. the preparation method of lanthanum aluminum composite metal pillared montmorillonite de-fluoridation adsorbent according to claim 1, its feature exists
In comprising the following steps：
(1) after montmorillonite is mixed with the sodium carbonate for accounting for montmorillonite quality 2-5%, then by montmorillonite and the mass ratio of deionized water
It is 5%, adds in deionized water, stirring 2h, aging 24h obtains montmorillonite suspension；
(2) salt of lanthanum is dissolved in deionized water, is made the salting liquid of the lanthanum of 0.1mol/L；Aluminium chlorohydrate is dissolved in deionization
In water, the liquor alumini chloridi of 0.2mol/L is made；
It is 1 by the mol ratio of lanthanum and aluminium:1-1:50, the salting liquid of the lanthanum and the liquor alumini chloridi are sufficiently mixed, stir
Obtain lanthanum aluminium mixing salt solution；
(3) NaOH is added in the lanthanum aluminium mixing salt solution so that aluminium and OH-Mol ratio be 2.4：1, be stirred vigorously 2h,
Aging 24h, obtains pillared liquid；
(4) it is 1 by the volume ratio of pillared liquid and montmorillonite suspension:1, the pillared liquid is slowly added into montmorillonite suspension
In, stirring 2h, aging 24h are then proceeded to, the 3-5 dissolving salt to wash away residual of centrifuge washing finally will centrifugation gained solid
Dried to constant weight under the conditions of being placed in 105 DEG C, obtain pillared montmorillonite solid；
(5) the pillared montmorillonite solid is placed in Muffle furnace, in 2h is calcined at 100-600 DEG C, then by products therefrom powder
Broken sieving, obtains the granular materials of particle diameter 0.1-1.0mm, as lanthanum aluminum composite metal pillared montmorillonite de-fluoridation adsorbent.
3. preparation method according to claim 2, it is characterised in that：The salt of the lanthanum is lanthanum nitrate or lanthanum sulfate.
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Cited By (7)
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| CN108273470A (en) * | 2018-02-24 | 2018-07-13 | 高姌 | Transition metal modified montmorillonite dephosphorization adsorbent based on deposition method preparation of reporting to the leadship after accomplishing a task |
| CN109173991A (en) * | 2018-09-17 | 2019-01-11 | 榆林学院 | A kind of load lanthanum-aluminium apricot shell method for preparation of active carbon handling fluoride waste |
| CN113952920A (en) * | 2020-07-21 | 2022-01-21 | 天津大学 | Preparation method and application of millimeter-grade aluminum-lanthanum composite hydroxide gel ball adsorbent |
| CN114100585A (en) * | 2020-08-26 | 2022-03-01 | 兰州石化职业技术学院 | Defluorinating agent for drinking water |
| CN115518620A (en) * | 2022-09-15 | 2022-12-27 | 西南交通大学 | Starch and lanthanum modified montmorillonite material and preparation and application methods thereof |
| CN115745115A (en) * | 2022-10-31 | 2023-03-07 | 深圳信息职业技术学院 | Polymeric lanthanum silicate flocculant, and preparation method and application thereof |
| CN116854180A (en) * | 2023-09-04 | 2023-10-10 | 杭州尚善若水环保科技有限公司 | Fluorine removing agent mixture and application thereof |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108273470A (en) * | 2018-02-24 | 2018-07-13 | 高姌 | Transition metal modified montmorillonite dephosphorization adsorbent based on deposition method preparation of reporting to the leadship after accomplishing a task |
| CN109173991A (en) * | 2018-09-17 | 2019-01-11 | 榆林学院 | A kind of load lanthanum-aluminium apricot shell method for preparation of active carbon handling fluoride waste |
| CN113952920A (en) * | 2020-07-21 | 2022-01-21 | 天津大学 | Preparation method and application of millimeter-grade aluminum-lanthanum composite hydroxide gel ball adsorbent |
| CN114100585A (en) * | 2020-08-26 | 2022-03-01 | 兰州石化职业技术学院 | Defluorinating agent for drinking water |
| CN115518620A (en) * | 2022-09-15 | 2022-12-27 | 西南交通大学 | Starch and lanthanum modified montmorillonite material and preparation and application methods thereof |
| CN115745115A (en) * | 2022-10-31 | 2023-03-07 | 深圳信息职业技术学院 | Polymeric lanthanum silicate flocculant, and preparation method and application thereof |
| CN116854180A (en) * | 2023-09-04 | 2023-10-10 | 杭州尚善若水环保科技有限公司 | Fluorine removing agent mixture and application thereof |
| CN116854180B (en) * | 2023-09-04 | 2023-12-15 | 杭州尚善若水环保科技有限公司 | Fluorine removing agent mixture and application thereof |
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Application publication date: 20170613 |