CN109304139A - A kind of modified technique improving attapulgite absorption property - Google Patents
A kind of modified technique improving attapulgite absorption property Download PDFInfo
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- CN109304139A CN109304139A CN201710621484.5A CN201710621484A CN109304139A CN 109304139 A CN109304139 A CN 109304139A CN 201710621484 A CN201710621484 A CN 201710621484A CN 109304139 A CN109304139 A CN 109304139A
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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
- B01J20/12—Naturally occurring clays or bleaching earth
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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
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The present invention provides a kind of modified technique for improving attapulgite absorption property, be by 1) by attapulgite tcrude ore it is levigate after sieve with 100 mesh sieve, after the attapulgite after sieving be put into hydrochloric acid solution carry out acidification purification processes；2) attapulgite after acidification purification is rinsed, be centrifuged, dried, ground；3) and by attapulgite after grinding thermal activation treatment is carried out；Modified attapulgite is rinsed, is centrifuged, is dried, be ground up, sieved after obtain finished product, the method that this technique is combined using attapulgite acidification purification, thermal activation, the absorption property of attapulgite can be significantly improved, heavy metal pollution of soil problem is effectively administered, improves Soil Utilization efficiency.
Description
Technical field
The invention belongs to the development and utilization of high added value attapulgite new product, specifically a kind of raising attapulgite
The modified technique of absorption property.
Background technique
Attapulgite (attapulgite) also known as palygorskite are a kind of nonmetallic ores of aqueous rich magnesium silicate clay
Object, natural attapulgite are a kind of layer of chain structures, are the nonmetallic clay mineral of sepiolite group.Attapulgite is special because of having
Fibre structure, different usual colloids and absorption property are often known as thousand soil so it has a wide range of applications field
King, general-purpose soil.1862, this mineral of Russia scholar Long Keqinkefu first discovery, and it is native to slope thread is named as
(Palygorskite), this mine soil, until nineteen thirty-five, drawing hundred are had also discovered in the area Georgia, USA Ao Tebao later
Even Attapulgite is named as specially for it.It is 1976 that China, which finds that the time of this mine soil is, and the six directions in Jiangsu is small by winding
Once have found attapulgite mineral, Chinese scholar Mr. Xu Jiquan translates according to transliteration and the feature of the mineral crystal structure
At " attapulgite ", used at home always from this this name.
At present, domestic and international heavy metal pollution of soil, which is administered, combines place with active carbon adsorption with biochemical method or flocculent precipitation
Based on reason, because active carbon is expensive, regenerative process is complicated and limits its use scope.Therefore, seek efficient low-consume, operation
Convenient, with low investment heavy metal-polluted soil improvement new material becomes research hotspot.The strong adsorption of attapulgite, can be used for soil
Heavy Metal Pollution Control, and effect is preferable.Attapulgite after activation has adsorption cleaning effect to heavy metal ion, can part
Replace active carbon, improve degree of purification and recycling rate of waterused, reduces adsorbent cost.And attapulgite dosage is less than troilite and changes
Property bentonite, be a kind of cheap heavy metal pollution of soil conditioner.The ion-exchange capacity that attapulgite itself has,
It can be used for administering containing Cd2+、Pb2+Etc. heavy metal ion soil, achieve the purpose that administer soil pollution.Since attapulgite stores up
Amount is abundant, and development cost is low, and operation processing is simple, and absorption property is excellent, make its as heavy metal pollution of soil conditioner
It is widely used, and has obtained considerable economic and social benefit.
With becoming increasingly conspicuous for China's heavy metal pollution of soil problem, seeks efficient low-consume, runs convenient, soil with low investment
Earth heavy metal improvement new material has become research hotspot.Attapulgite cation exchange outstanding and adsorption capacity are in soil weight
It has a extensive future in terms of metallic pollution reparation.This technique using attapulgite acidification purification, thermal activation, inorganic modified combine
Method, the absorption property of attapulgite can be significantly improved, this administers heavy metal pollution of soil problem to effective, improves soil
Utilization efficiency is significant.
Summary of the invention
Technical problem to be solved by the present invention lies in provide a kind of modification work for improving attapulgite absorption property
Skill, be by 1) by attapulgite tcrude ore it is levigate after sieve with 100 mesh sieve after it is stand-by；2) the concave convex rod original ore soil after handling well is set
In HCL solution in centrifugation, drying, grinding after heating stirring；3) attapulgite after acidification purification is subjected to thermal activation treatment
After obtain finished product, the method that this technique is combined using attapulgite acidification purification, thermal activation can significantly improve attapulgite
Absorption property, effectively administer heavy metal pollution of soil problem, improve Soil Utilization efficiency, processing step is simple.
A kind of modified technique improving attapulgite absorption property, the specific steps are as follows:
The acidification of first step attapulgite purifies:
Concave convex rod original ore soil after levigate sieve with 100 mesh sieve is put into the dilute hydrochloric acid solution that concentration is 0.2mol/l and is stirred
It mixes, 60 DEG C of souring temperature, acidificatoin time is 10 minutes；
The thermal activation of second step attapulgite
Attapulgite after will be acidified is rinsed with distilled water, and drying, grinding is put into Muffle furnace after sieving with 100 mesh sieve
It is calcined, temperature is 600 DEG C, and the reaction time is 3 hours；
The product handling system of third step attapulgite
The attapulgite of first two steps processing is rinsed, reagent residue extra in attapulgite is removed；Make when flushing
With distilled water, washing time 3 times, rinse 15 minutes every time；Attapulgite is put into supercentrifuge after flushing to be centrifuged, is turned
Speed is 4000rmin-1, centrifugation time is 10 minutes；The moisture separated after centrifugation is poured out, and by remaining concave convex rod
Soil is put into baking oven and is dried, and 105 DEG C of temperature, the time is 8-12 hours；Finally the attapulgite after drying is ground, and
It sieves with 100 mesh sieve, finally obtains finished product.
Specific steps are described as follows:
The acidification of first step attapulgite purifies: this operation can tentatively improve attapulgite tcrude ore purity, improve concave-convex
Stick soil tcrude ore absorption property is the depolymerization for showing themselves in that 1) fiber interfascicular in the process because of hydrochloric acid activation, predominantly non-adsorbent
The decomposition of impurity (such as carbonate mineral) grain-to-grain cementation object；2) increase of crystal specific surface area is brilliant so that adsorption capacity greatly improves
The specific surface area of body increases.It 3) is H+To octahedral cations Mg2+, Al3+, Fe3+By the successively metathesis at edge to center.
Due to H+With Mg2+, Al3+, Fe3+Ionic radius difference is too big and crystal chemistry behavior not etc. does not increase its surface-active.
The thermal activation of second step attapulgite: calcining can significantly improve the adsorptivity of attapulgite under the conditions of 600 DEG C
Energy；Its mechanism is that attapulgite adsorbs zeolite water in water and structure pore after firing, between mineral internal fiber and is removed, in turn
Increase attapulgite specific surface area.
Beneficial effects of the present invention:
1) non-adsorbent impurity (such as carbonate mineral) grain-to-grain cementation object impurity is divided in concave convex rod raw ore after modified
Solution, attapulgite purity is higher, and absorption property is obviously improved；
2) it adsorbs zeolite water in water and structure pore between modified concave convex rod tcrude ore internal fiber to be removed, attapulgite
Crystal specific surface area dramatically increases.
Detailed description of the invention:
Fig. 1 heat activation temperature is to attapulgite Adsorption of Cu2+Influence diagram
Fig. 2 heat activation temperature adsorbs Cd to attapulgite2+Influence diagram
Fig. 3 heat activation temperature adsorbs Pb to attapulgite2+Influence diagram
Fig. 4 heat activation temperature adsorbs Zn to attapulgite2+Influence diagram
Specific embodiment:
A kind of modified technique improving attapulgite absorption property, specific implementation step are as follows:
The acidification of first step attapulgite purifies
Concave convex rod original ore soil after levigate sieve with 100 mesh sieve is put into the dilute hydrochloric acid solution that concentration is 0.2mol/l and is stirred
It mixes, 60 DEG C of souring temperature, acidificatoin time is 10 minutes.The operation can tentatively improve attapulgite tcrude ore purity, improve concave-convex
Stick soil tcrude ore absorption property is the depolymerization for showing themselves in that 1) fiber interfascicular in the process because of hydrochloric acid activation, predominantly non-adsorbent
The decomposition of impurity (such as carbonate mineral) grain-to-grain cementation object；2) increase of crystal specific surface area is brilliant so that adsorption capacity greatly improves
The specific surface area of body increases.It 3) is H+To octahedral cations Mg2+, Al3+, Fe3+By the successively metathesis at edge to center.
Due to H+With Mg2+, Al3+, Fe3+Ionic radius difference is too big and crystal chemistry behavior not etc. does not increase its surface-active.
The thermal activation of second step attapulgite
Attapulgite after will be acidified is rinsed with distilled water, and drying, grinding is put into Muffle furnace after sieving with 100 mesh sieve
It is calcined, temperature is 600 DEG C, and the reaction time is 3 hours.Calcining can significantly improve attapulgite under the conditions of 600 DEG C
Absorption property.Its mechanism be attapulgite after firing, zeolite water quilt in water and structure pore is adsorbed between mineral internal fiber
Removing, and then increase attapulgite specific surface area.
The product handling system of third step attapulgite
The attapulgite of first two steps processing is rinsed, reagent residue extra in attapulgite is removed.Make when flushing
With distilled water, washing time 3 times, rinse 15 minutes every time；Attapulgite is put into supercentrifuge after flushing to be centrifuged, is turned
Speed is 4000rmin-1, centrifugation time is 10 minutes；The moisture separated after centrifugation is poured out, and by remaining concave convex rod
Soil is put into baking oven and is dried, and 105 DEG C of temperature, the time is 8-12 hours；Finally the attapulgite after drying is ground, and
It sieves with 100 mesh sieve, finally obtains finished product.
Analysis of experiments:
It tests to show that this patent modified parameter (acidification concentration, heat activation temperature) changes attapulgite absorption property
Kind situation, concave convex rod original ore soil and modified attapulgite are respectively put into Cu, Cd, Pb, Zn heavy metal solution and adsorbed
Property test, purport is that the R&D and promotion of this patent is provided fundamental basis and reference frame.
Test 1
1.1 experimental raws and equipment
Primary raw material: attapulgite tcrude ore, hydrochloric acid (chemical analysis is pure).
Key instrument: electromagnetic mixer, reciprocating vibrating machine, supercentrifuge, baking oven, atomic absorption spectrophotometer.
The optimization of the acidification purifying technique of 1.2 attapulgites
1.2.1 the selection of technic index
Binding experiment experience, technic index are set as three processing, and three gradients, specific targets set as follows: hydrochloric acid is dense
It spends (0.2mol, 0.5mol, 1mol)；Mixing time (10min, 30min, 60min)；Treatment temperature (30 DEG C, 60 DEG C, 90 DEG C),
And be combined each processing, each gradient, specific combined situation is as follows:
Each horizontal, each gradient combination situation of the acidification purification of table 1
1.2.2 the acidification of attapulgite
Attapulgite, each numbering attapulgite are successively purified according to number and each processing, each gradient situation
50g.Untreated concave convex rod original soil is weighed, is placed in three-necked flask and the HCL solution of (0.2mol, 0.5mol, 1mol) is added
100ml is put into magnetic stirrer (10min, 30min, 60min), and temperature is set as (30 DEG C, 60 DEG C, 90 DEG C), be centrifuged, dry,
Grinding, number after be put into drier be sealed it is to be measured.
The test of 1.3 absorption properties
1.3.1 the drafting of standard curve
Weigh 1.0156gCdCl2·2.5H2O after deionized water dissolving is added, is moved into 1000ml volumetric flask, and dilute
To graticule.Standard solution 2,4,6,8,10ml are pipetted respectively with pipette in 1000ml volumetric flask, is diluted to deionized water
It at 1000ml graduation mark, shakes up, using water as reference, measures Cd content with atomic absorption spectrophotometer, draw standard curve.
2.3.2 adsorptivity is tested
The attapulgite powder 500mg (each purification processes weigh 3 parts) purified is weighed, concentration is put into and contains for 4mg/L
In Cd solution 400ml, and with 1d is shaken on reciprocating vibration machine, Aspirate supernatant after centrifugation measures on atomic spectrophotometer
Cd ion concentration calculates attapulgite to the equilibrium adsorption capacity and adsorption rate of Cd ion, to evaluate each purification processes with formula 1
Improved effect.
Qe=(C0-Ce) * V/m ... (1)
In formula, Qe is the equilibrium adsorption capacity (mg/g) of adsorbent, and Ce is the equilibrium concentration (mg/L) of Cd ion in solution, C0
For the initial concentration (mg/L) of Cd ion, V is the volume (L) of solution, and m is the quality (g) of adsorbent.
1.4 results and analysis
Table 2 is the result of study of attapulgite acidification purification orthogonal experiment, and K is the sum of the data of all same levels, and k is
The average value of the attapulgite adsorbance of each same level, R2Indicate the variation of experimental index of the factor in its value range
Amplitude, according to very poor R2Size, can judge influence factor primary and secondary sequence.R2Value it is bigger, to change empirical factor heavier for expression
It wants.By being analyzed above as it can be seen that it is A > C > B that the factor in attapulgite acidification purification experiment, which influences primary and secondary sequence,.According to K, the value of k
The optimal set of deducibility attapulgite acidification purification is A1, B1, C3, i.e. acid concentration 0.2mol, mixing time 10min, temperature 90
It is DEG C best to the improvement of concave convex rod absorption property.
2 Orthogonal experiment results of table
Test 2
2 research methods
2.1 experimental raws and equipment
Primary raw material: attapulgite tcrude ore, hydrochloric acid, sodium hydroxide, potassium nitrate, ammonium chloride, trimethyl chlorine
Change ammonium, dodecyl benzyl dimethyl ammonium chloride, cetyl trimethylammonium bromide, octadecyltrimethylammonium chloride (more than
Reagent is that chemical analysis is pure).
Key instrument: Muffle furnace, electromagnetic mixer, reciprocating vibrating machine, supercentrifuge, baking oven, atomic absorption spectrophotometry
Photometer.
The thermal activation technique of 2.2 attapulgites
It is heat activation temperature that this test, which is respectively set 400 DEG C, 500 DEG C, 600 DEG C,.Specific experiment operation is as follows, and 50g is taken to pass through
The concave convex rod original ore soil for crossing acid system purification (0.2mol, 10min, 90 DEG C), is forged under conditions of 400 DEG C, 500 DEG C, 600 DEG C respectively
3h is burnt, is cooled to room temperature, smashing and grinding to 100 mesh.The attapulgite being disposed is respectively put into it is to be measured in container, and according to
Temperature number H1, H2, H3 respectively.
The test of 2.4 absorption properties
2.4.1 absorption and desorption experiment
To understand attapulgite modified confinement capabilities of the technique to heavy metal and the releasable property to institute's sticking heavy metal.This
Project will complete absorption and desorption experiment of the purification with the attapulgite after improvement to heavy metal (Cu, Cd, Pb and Zn), initial dense
Degree is respectively for 200,50,200,200mg/L.The specific operation method is as follows: weigh respectively (H1, H2, H3, CK, wherein CK be it is recessed
Convex stick soil raw ore) for attapulgite 0.50g in the solution of a certain heavy metal of 400mL, every soil sample weighs 3 parts.Continuous oscillation for 24 hours,
The heavy metal mass concentration in equilibrium liquid is measured after centrifugal filtration.It is calculated not according to the variation of heavy metal mass concentration before and after sticking
With the attapulgite modified equilibrium adsorption capacity to addition heavy metal.Attapulgite is calculated to the balance of each metal ion with formula 1
Adsorbance and adsorption rate, to evaluate the improved effect of each purification processes.
Qe=(C0-Ce) * V/m ... (1)
In formula, Qe is the equilibrium adsorption capacity (mg/g) of adsorbent, and Ce is the equilibrium concentration (mg/ of heavy metal ion in solution
L), C0 is the initial concentration (mg/L) of heavy metal ion, and V is the volume (L) of solution, and m is the quality (g) of adsorbent.
The solution stripping of the heavy metal free of remaining attapulgite same volume, oscillation are centrifuged afterwards for 24 hours after the above centrifugation,
The heavy metal mass concentration in equilibrium liquid is measured, calculates heavy metal release amount, desorption experiment is carried out continuously 2 times, so that it is determined that recessed
Degree of stability of the convex stick soil to heavy metal adsorption.After the completion of experiment, after going out attapulgite acidification according to analysis of experimental data
Thermal activation Optimal Temperature.
3 results and analysis
Influence of the 3.1 thermal activation techniques to attapulgite absorption property is as shown in Figure of description:
Fig. 1 heat activation temperature is to attapulgite Adsorption of Cu2+Influence
Fig. 2 heat activation temperature adsorbs Cd to attapulgite2+Influence
Fig. 3 heat activation temperature adsorbs Pb to attapulgite2+Influence
Fig. 4 heat activation temperature adsorbs Zn to attapulgite2+Influence
From FIG. 1 to FIG. 4 it can be seen that thermal activation can improve concave convex rod original ore soil to the adsorption capacity of heavy metal ion, and
With the increase of heat activation temperature, attapulgite becomes apparent heavy metal ion adsorbed performance capability promotion.Work as thermal activation
When temperature is 400 DEG C, attapulgite original ore soil Cd is compared2+Absorption property promotes 11.46%, to Pb2+Absorption property is promoted
0.54%, to Zn2+Absorption property promotes 2.48%, to Cu2+Absorption property is declined slightly；When heat activation temperature is 500 DEG C, phase
Than attapulgite original ore soil to Cu2+Absorption property rises 26.88%, Cd2+Absorption property promotes 74.18%, to Pb2+Adsorptivity
11.18% can be promoted, to Zn2+Absorption property promotes 60.47%；When heat activation temperature is 600 DEG C, attapulgite original ore soil is compared
To Cu2+Absorption property rises 36.86%, Cd2+Absorption property promotes 177.52%, to Pb2+Absorption property promotion 18.57%, it is right
Zn2+Absorption property promotes 67.97%.In summary it can be found that carrying out thermal activation treatment to attapulgite, it can be improved bumps
Performance boost is the most significant to the absorption property of heavy metal ion, and when heat activation temperature is 600 DEG C for stick soil, this is to attapulgite
The processing technology research and development of heavy metal conditioner have important directive significance.
All above-mentioned this intellectual properties of primarily implementation, there is no this new products of implementation of setting limitation other forms
And/or new method.Those skilled in the art will utilize this important information, above content modification, to realize similar execution feelings
Condition.But all modifications or transformation belong to the right of reservation based on new product of the present invention.
The above described is only a preferred embodiment of the present invention, being not that the invention has other forms of limitations, appoint
What those skilled in the art changed or be modified as possibly also with the technology contents of the disclosure above equivalent variations etc.
Imitate embodiment.But without departing from the technical solutions of the present invention, according to the technical essence of the invention to above embodiments institute
Any simple modification, equivalent variations and the remodeling made, still fall within the protection scope of technical solution of the present invention.
Claims (1)
1. a kind of modified technique for improving attapulgite absorption property, it is characterised in that: its specific implementation step is as follows:
The acidification of first step attapulgite purifies
Concave convex rod original ore soil after levigate sieve with 100 mesh sieve is put into the dilute hydrochloric acid solution that concentration is 0.2mol/l and is stirred,
90 DEG C of souring temperature, acidificatoin time is 10 minutes；
The thermal activation of second step attapulgite
Attapulgite after will be acidified is rinsed with distilled water, drying, and grinding is put into Muffle furnace progress after sieving with 100 mesh sieve
Calcining, temperature are 600 DEG C, and the reaction time is 3 hours；Calcining can significantly improve the suction of attapulgite under the conditions of 600 DEG C
Attached performance；Its mechanism is that attapulgite adsorbs zeolite water in water and structure pore after firing, between mineral internal fiber and is removed,
And then increase attapulgite specific surface area；
The product handling system of third step attapulgite
The attapulgite of first two steps processing is rinsed, reagent residue extra in attapulgite is removed；Steaming is used when flushing
Distilled water washing time 3 times, is rinsed 15 minutes every time；Attapulgite is put into supercentrifuge after flushing to be centrifuged, revolving speed is
4000r·min-1, centrifugation time is 10 minutes；The moisture separated after centrifugation is poured out, and remaining attapulgite is put
Enter baking oven to be dried, 105 DEG C of temperature, the time is 8-12 hours；Finally the attapulgite after drying is ground, and mistake
100 meshes, finally obtain finished product.
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| CN110369484A (en) * | 2019-07-08 | 2019-10-25 | 王帘里 | A kind of microwave repairing method in situ of contaminated soil |
| CN110396393A (en) * | 2019-07-08 | 2019-11-01 | 南京迪天高新产业技术研究院有限公司 | A kind of heavy metal deactivator and preparation method thereof using matrix production |
| CN110402632A (en) * | 2019-07-08 | 2019-11-05 | 王帘里 | A kind of comprehensive processing method of beach saline land |
| CN110484264A (en) * | 2019-07-08 | 2019-11-22 | 南京迪天高新产业技术研究院有限公司 | A kind of passivator and preparation method thereof for repairing farming land Heavy Metals in Soil Contaminated chromium |
| CN110721656A (en) * | 2019-10-29 | 2020-01-24 | 江苏开放大学（江苏城市职业学院） | Method for optimizing Pb (II) adsorption condition of modified attapulgite by BP-PSO (Back propagation-PSO) and application |
| CN113070047A (en) * | 2021-03-30 | 2021-07-06 | 江西理工大学 | Functionalized mineral material and preparation method and application thereof |
| CN114452933A (en) * | 2022-01-28 | 2022-05-10 | 天津科技大学 | Preparation method and application of modified attapulgite for adsorbing organic arsenic compounds |
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| CN110396393A (en) * | 2019-07-08 | 2019-11-01 | 南京迪天高新产业技术研究院有限公司 | A kind of heavy metal deactivator and preparation method thereof using matrix production |
| CN110402632A (en) * | 2019-07-08 | 2019-11-05 | 王帘里 | A kind of comprehensive processing method of beach saline land |
| CN110484264A (en) * | 2019-07-08 | 2019-11-22 | 南京迪天高新产业技术研究院有限公司 | A kind of passivator and preparation method thereof for repairing farming land Heavy Metals in Soil Contaminated chromium |
| CN110402632B (en) * | 2019-07-08 | 2022-04-29 | 王帘里 | Comprehensive treatment method for coastal saline-alkali soil |
| CN110721656A (en) * | 2019-10-29 | 2020-01-24 | 江苏开放大学（江苏城市职业学院） | Method for optimizing Pb (II) adsorption condition of modified attapulgite by BP-PSO (Back propagation-PSO) and application |
| CN113070047A (en) * | 2021-03-30 | 2021-07-06 | 江西理工大学 | Functionalized mineral material and preparation method and application thereof |
| CN113070047B (en) * | 2021-03-30 | 2022-11-25 | 江西理工大学 | Functionalized mineral material and preparation method and application thereof |
| CN114452933A (en) * | 2022-01-28 | 2022-05-10 | 天津科技大学 | Preparation method and application of modified attapulgite for adsorbing organic arsenic compounds |
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Application publication date: 20190205 |