CN105289506A - Multielement modified bentonite adsorption material and preparation method thereof - Google Patents
Multielement modified bentonite adsorption material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a multielement modified bentonite adsorption material and belongs to the technical field of composite materials and water treatment. Sodium bentonite as a main material is modified by a multielement composite modifier containing an organic long carbon chain cationic surfactant, inorganic polyhydroxyl-based metal cations and a functional short carbon chain organic complexing agent by a copolymerization method to form the organic-inorganic multielement composite bentonite adsorption material. The organic-inorganic multielement composite bentonite adsorption material has porous and large specific surface area characteristics of inorganic pillared bentonite and high carbon content and strong hydrophobicity characteristics of organic bentonite and has strong metal ion complexation and adsorption functions of bentonite and thus organic matters can be adsorbed by surface adsorption and distribution and heavy metal ions in water can be removed by complexation. The organic-inorganic multielement composite bentonite adsorption material can be popularized and used in the waste water treatment field.
Description
Technical field
The present invention relates to a kind of modified alta-mud sorbing material, particularly relate to a kind of with organic Long carbon chain cationic surfactant, the short carbon chain organic complexing agent of inorganic polymeric hydroxy metal cation and functionalization is the preparation that multicomponent composite modifier carries out poly modified sorbing material, belongs to field of compound material and water treatment field.
Background technology
Bentonite has a good application prospect in water treatment as Low Cost Sorbents.Bentonite not only rich reserves, cheap and easy to get, by carrying out suitable modification to bentonite, its absorption property can significantly improve, and has potential application prospect in the treatment of waste water.During modification, modifier used is different, then the interlayer structure of modified alta-mud and surface nature just have very big-difference, also has higher selective to the absorption of water pollutant.But the modifier kind of research institute is still more single at present, is poly-hydroxy metal cation and cationic surfactant mostly.Organobentonite can demonstrate excellent performance to the process of organic pollutants, but due to its surface hydrophobic, is then difficult to remove to the heavy metal ion in water; Although inorganic bentonite effectively can remove the heavy metal ion in water, can not organic pollution effectively in Adsorption water, reason is that metal hydroxy polycation has very strong hydrophily.
China's shortage of water resources, water pollutions is on the rise; And often focus on after various industrial wastewater mixing, cause in waste water simultaneously containing a large amount of heavy metals and various organic pollution.Therefore, the bentonite base new material of common contaminant in waste water and corresponding new technology can effectively be removed in the urgent need to exploitation.But up to the present relevant research is also rare.
Summary of the invention
The object of this invention is to provide the preparation method of the poly modified bentonite clay material of a kind of organic and inorganic;
One, the preparation of poly modified bentonite clay material
The preparation of the poly modified bentonite clay material of the present invention it be using sodium bentonite as material of main part, with the short carbon chain organic complexing agent multicomponent composite modifier of organic Long carbon chain cationic surfactant, inorganic polymeric hydroxy metal cation and functionalization, utilize copolymerization method to carry out poly modified to bentonite, obtain the bentonite material for water treatment that organic and inorganic is poly modified.Concrete preparation technology is: first sodium bentonite distilled water is made into the suspension of 2 ~ 4%, stirs, leaves standstill swelling 12 ~ 24h; Again 50 ~ 80 DEG C, the polynary column-supporting agent that the short carbon chain organic complexing agent by organic Long carbon chain cationic surfactant, inorganic polymeric Hydroxy-Al cations, functionalization forms is added in bentonite suspension under strong agitation, continue stirring 12 ~ 36h, aging 24 ~ 48h subsequently, suction filtration, the solid fraction material distilled water cyclic washing obtained, until without Cl
-and Br
-till; Then dry to constant weight in 50 ~ 80 DEG C, grinding, cross 200 mesh sieves, the product obtained is white powder multiple elements design bentonite material for water treatment.
The preparation of inorganic polymeric Hydroxy-Al cations column-supporting agent described above: under 50 ~ 80 DEG C, constantly stirring, the alkaline solution of 0.2 ~ 1.8mol/L is slowly added 0.5 ~ 1.5mol/LAlCl of 3 ~ 6 times of volumes
3in solution, make OH in mixed solution
-with Al
3+mol ratio be 2:1 ~ 3:1; In 50 ~ 80 DEG C of aging 12 ~ 36h after stirring 3 ~ 4h, obtain inorganic polymeric Hydroxy-Al cations column-supporting agent.This inorganic polymeric Hydroxy-Al cations column-supporting agent addition be: 6 ~ 10mmol/g bentonite.
The mol ratio of the short carbon chain organic complexing agent of described organic Long carbon chain cationic surfactant and functionalization is 1:0.5 ~ 1:1.5, and the total addition of the two is 0.82 ~ 1.23mmol/g bentonite.Wherein, described organic Long carbon chain cationic surfactant is softex kw (CTAB), cetalkonium chloride (HDBAC); The short carbon chain organic complexing agent of functionalization is diethylene triamine pentacetic acid (DTPA) (DTPA), ethylenediamine tetra-acetic acid (EDTA) or citric acid (CA).
Two, poly modified bentonite clay material characterizes
By X-ray powder diffraction (XRD), FFIR (FT-IR), with characterization methods such as JSM-6701F type SEM (SEM), the multiple elements design bentonite material for water treatment prepare the present invention and the surface functional group type of raw material thereof, structure and morphology carry out analytic explanation.
1, X-ray powder diffraction (XRD) is analyzed
The bentonitic XRD of Fig. 1 sodium bentonite original soil (Bent) and single modification and team member's modification.As seen from Figure 1, bentonite is after composite modified, and its surface nature and interlayer structure all there occurs change.The interlamellar spacing d of original soil Bent
001for 1.252nm, be equivalent to the thickness (0.96nm) of smectite structure layer (two silicon-oxy tetrahedrons press from both sides an alumina octahedral) and one deck adsorbed water molecule thickness (0.29nm) sum, show that testing original soil Bent used is na-montmorillonite really.Due to bentonitic expansiveness, in its structure modified, change is exactly basal spacing d the most significantly
001size change.After the interlayer of the introducing bentonite original soil of organic complexing agent DTPA and CTAB, basal spacing d
001increase to 1.597nm by original 1.252nm, the hydrophily on its surface weakens, and hydrophobicity strengthens; Due to the macromolecular introducing of interlayer, interlamellar spacing increases, and structure becomes comparatively fluffy.And after Long carbon chain Surfactant CTAB and complexing agent DTPA and hydroxy aluminum column-supporting agent introduce the interlayer of bentonite original soil simultaneously, the interlamellar spacing d of poly modified bentonite CTAB-DTPA-Al-Bent
001increase to 1.995nm.As can be seen here, copolymerization method is utilized successfully to prepare poly modified bentonite material for water treatment.
2, FT-IR analyzes
Fig. 2 is infrared spectrum (FT-IR) figure of sodium bentonite original soil (Bent) and various modified alta-mud.The internal structure change of FT-IR spectrum analysis alternatively bright bentonite modified front and back.The major absorbance peak of original soil Bent has six places (referring to table 1), compares discovery, be positioned at 467cm with the FT-IR spectrum of original soil Bent
-1, 521cm
-1, 793cm
-1, 845cm
-1, 916cm
-1and 1036cm
-1locate bentonitic characteristic absorption peak and afterwards obvious change does not occur before modification, illustrate that bentonite basic framework of silicate after organically-modified does not become; And in the FT-IR spectrum of CTAB-DTPA-Bent and CTAB-DTPA-Al-Bent, there are three new absworption peaks, i.e. 1474cm
-1-the CH at place
2scissoring vibration absworption peak, and 2851cm
-1and 2920cm
-1-the CH at place
2the symmetric and anti-symmetric stretching vibration absworption peak of H-C-H in group.Can infer that CTAB and DTPA enters between bentonite bed effectively thus.And compared with Bent original soil, multiple elements design bentonite CTAB-DTPA-Al-Bent is at 912cm
-1the flexural vibrations absworption peak generating portion displacement of neighbouring Al-OH, from 912cm
-1be displaced to 920cm
-1, this is because Al
3+with Na
+enter after exchange between bentonite bed, Al
3+have unoccupied orbital, easily coordinate with the O atom in bentonite structure OH, cause OH group vibrational frequency to strengthen, spectrum peak, to high wave number displacement, makes OH translational vibration peak change.This illustrates that hydroxy aluminum cation also successfully enters between bentonite bed.
3, ESEM (SEM) is analyzed
Utilize ESEM just can observe bentonitic surface appearance feature more intuitively.Observe its surface appearance feature can find, original soil Bent and modified alta-mud are all assembled with aggregating state form.Bentonite original soil Bent(Fig. 3) likeness in form " cabbage ", particle is comparatively large, and surface is more smooth, and in more regular closelypacked lamellar structure, lamellar body is thicker, and hole is less; And CTAB-DTPA-Bent(Fig. 4) contours profiles is softer compared with Bent, in cloud sheet shape, surface ratio comparatively flat-satin, it is large to unfold degree, and continuity is better, and edge has perfectly round shape lace, and particle size distribution is more even; CTAB-DTPA-Al-Bent(Fig. 5) particle relatively little, more loose, present the lepidiod lamella of crimping, and with the unordered arrangement of different angles, there is that peel away, loose, curling lamella, these lamellas form many fine pores more.Can see from the side, certain distance is had between each lamella, simultaneously with some comparatively sharp-pointed edges, also to mix between block layer thinner granule, duct and gap are expanded further, surface area increases further, simultaneously for pollutant in bentonite adsorption water body provides favourable passage and gap structure.
In sum, the composite modifying method of the present invention by bentonitic surface modification is combined with functionalization, selecting a series of short carbon chain organic complexing agent with different structure feature carries out poly modified with polymerization hydroxy metal ion and Long carbon chain cationic surfactant to bentonite, and the multiple elements design bentonite obtained has the double effects simultaneously removing huge sum of money ion and organic pollutant.Compared with conventional surfactant organic modified bentonite, there is larger porosity and specific area, more high thermal stability relatively, and the combination of long and short modify carbon chains agent can improve bentonite to organic adsorptive selectivity, for the organic matter of all kinds of heterogeneity of Adsorption and concentration range.Utilize the special stability of complex compound simultaneously, heavy metal ion is fixed between bentonite bed by complexing, not only can effectively remove heavy metal ion in water, greatly can also reduce its residual concentration in water.Compared with inorganic pillared bentonite, both there is inorganic pillared bentonite specific area and the large advantage of pore volume, possessed again high hydrophobicity and high organic carbon content that inorganic pillared bentonite lacks, the organic matter in adsorbable water.Therefore, both simultaneously by adsorption and distribution two kinds of approach adsorb organic compounds, complexing can be utilized again to remove heavy metal ion in water, can promote the use of in field of waste water treatment.
Accompanying drawing explanation
The XRD spectra of Fig. 1 sodium bentonite and modified alta-mud.
Infrared spectrum (FT-IR) spectrogram of Fig. 2 sodium bentonite original soil and modified alta-mud.
SEM photo under Fig. 3 sodium bentonite original soil different amplification.
Fig. 4 is the SEM photo under CTAB-DTPA-Bent different amplification.
Fig. 5 is the SEM photo under CTAB-DTPA-Al-Bent different amplification.
Detailed description of the invention
Below by specific embodiment, the poly modified bentonitic preparation technology of the present invention is further elaborated.
embodiment 1
(1) preparation of inorganic polymeric Hydroxy-Al cations column-supporting agent: under 60 DEG C, constantly stirring, the NaOH solution of 0.4mol/L is slowly added the 1.0mol/LAlCl of 6 times of volumes in 3h
3in solution, make OH in mixed solution
-with Al
3+mol ratio be 1:2.4; After dropwising, continue stir 3h, then by gained solution at 60 DEG C of aging 24h, obtain inorganic polymeric Hydroxy-Al cations column-supporting agent;
(2) preparation of multiple elements design column-supporting agent: CTAB, DTPA are mixed with inorganic polymeric Hydroxy-Al cations column-supporting agent (wherein the mol ratio of DTPA and CTAB is total consumption of 1:1, DTPA and CTAB is 0.85mmol/g bentonite; The consumption of inorganic polymeric Hydroxy-Al cations column-supporting agent is: 6mmol/g bentonite), stir 2h, obtained multiple elements design column-supporting agent;
(3) preparation of poly modified bentonite adsorption material: take 3.0g sodium bentonite, adds the suspension 100mL that distilled water is made into mass percent 3%, stirring, static swelling 12h; 70 DEG C, under strong agitation, multiple elements design column-supporting agent is dropwise instilled bentonite suspension; After dropwising, continue to stir 12h, aging 24h at the same temperature subsequently; Suction filtration, the solid fraction material distilled water cyclic washing obtained, until without Cl
-and Br
-till, then dry to constant weight in 80 DEG C, grinding, cross 200 mesh sieves, the product obtained is the poly modified bentonite adsorption material of white powder.BET surface area is 107m
2/ g, pore volume is 0.065cm
3/ g, average pore size 2.45nm.
embodiment 2
(1) preparation of inorganic polymeric Hydroxy-Al cations column-supporting agent: under 80 DEG C, constantly stirring, first by the Na of 0.5mol/L
2cO
3solution slowly adds the 1.0mol/LAlCl of 3 times of volumes
3in solution, make OH in mixed solution
-with Al
3+mol ratio be 2.4:1, after dropwising; In 80 DEG C of aging 36h after continuation stirring 4h, obtain inorganic polymeric Hydroxy-Al cations column-supporting agent;
(2) preparation of multiple elements design column-supporting agent: CTAB, DTPA are mixed with inorganic polymeric Hydroxy-Al cations column-supporting agent (wherein the mol ratio of DTPA and CTAB is total consumption of 1:1.5, DTPA and CTAB is 0.85mmol/g bentonite; The consumption of inorganic polymeric Hydroxy-Al cations column-supporting agent is: 6mmol/g bentonite), stir 2h, obtained multiple elements design column-supporting agent;
3, the preparation of poly modified bentonite adsorption material: take 3.0g sodium bentonite, adds the suspension 100mL that distilled water is made into mass percent 3%, stirring, static swelling 12h; 80 DEG C, under strong agitation, multiple elements design column-supporting agent is dropwise instilled bentonite suspension; After dropwising, continue to stir 12h, aging 24h at the same temperature subsequently; Suction filtration, the solid fraction material distilled water cyclic washing obtained, until without Cl
-and Br
-till, then dry to constant weight in 80 DEG C, grinding, cross 200 mesh sieves, the product obtained is the poly modified bentonite adsorption material of white powder.BET surface area is 138m
2/ g, pore volume is 0.093cm
3/ g, average pore size 2.2nm.
embodiment 3
(1) preparation of inorganic polymeric Hydroxy-Al cations column-supporting agent: under 60 DEG C, constantly stirring, the NaOH solution of 0.4mol/L is slowly added the 1.0mol/LAlCl of 6 times of volumes in 3h
3in solution, make OH in mixed solution
-with Al
3+mol ratio be 1:2.4, after dropwising, continue stir 3h, then by gained solution 60 DEG C of aging 24h, inorganic polymeric hydroxy metal cation column-supporting agent can be obtained;
(2) preparation of multiple elements design column-supporting agent: CTAB, DTPA are mixed with inorganic polymeric Hydroxy-Al cations column-supporting agent (wherein the mol ratio of DTPA and CTAB is total consumption of 1:0.35, DTPA and CTAB is 1.03mmol/g bentonite; The consumption of inorganic polymeric Hydroxy-Al cations column-supporting agent is: 6mmol/g bentonite), stir 2h, obtained multiple elements design column-supporting agent;
(3) preparation of poly modified bentonite adsorption material: take 2.0g sodium bentonite, adds the suspension 100mL that distilled water is made into mass percent 2%, stirring, static swelling 12h; 80 DEG C, under strong agitation, multiple elements design column-supporting agent is dropwise instilled bentonite suspension; After dropwising, continue to stir 24h, aging 24h at the same temperature subsequently; Suction filtration, the solid fraction material distilled water cyclic washing obtained, until without Cl
-and Br
-till, then dry to constant weight in 80 DEG C, grinding, cross 200 mesh sieves, the product obtained is the poly modified bentonite adsorption material of white powder.BET surface area is 123m
2/ g, pore volume is 0.085cm
3/ g, average pore size 2.75nm.
embodiment 4
(1) preparation of inorganic polymeric Hydroxy-Al cations column-supporting agent: under 60 DEG C, constantly stirring, the NaOH solution of 0.4mol/L is slowly added the 1.0mol/LAlCl of 6 times of volumes in 3h
3in solution, make OH in mixed solution
-with Al
3+mol ratio be 1:2.4, after dropwising, continue stir 3h, then by gained solution 60 DEG C of aging 24h, inorganic polymeric hydroxy metal cation column-supporting agent can be obtained;
(2) preparation of multiple elements design column-supporting agent: CTAB, DTPA are mixed with inorganic polymeric Hydroxy-Al cations column-supporting agent (wherein the mol ratio of DTPA and CTAB is total consumption of 1:0.5, DTPA and CTAB is 1.23mmol/g bentonite; The consumption of inorganic polymeric Hydroxy-Al cations column-supporting agent is: 10mmol/g bentonite), stir 2h, obtained multiple elements design column-supporting agent;
(3) preparation of poly modified bentonite adsorption material: take 3.0g sodium bentonite, adds the suspension 100mL that distilled water is made into mass percent 3%, stirring, static swelling 12h; 80 DEG C, under strong agitation, multiple elements design column-supporting agent is dropwise instilled bentonite suspension; After dropwising, continue to stir 24h, aging 36h at the same temperature subsequently; Suction filtration, the solid fraction material distilled water cyclic washing obtained, until without Cl
-and Br
-till, then dry to constant weight in 80 DEG C, grinding, cross 200 mesh sieves, the product obtained is the poly modified bentonite adsorption material of white powder.BET surface area is 139m
2/ g, pore volume is 0.13cm
3/ g, average pore size 2.98nm.
embodiment 5
(1) preparation of inorganic polymeric Hydroxy-Al cations column-supporting agent: under 80 DEG C, constantly stirring, by the Na of 0.5mol/L in 3h
2cO
3solution slowly adds the 1.0mol/LAlCl of 3 times of volumes
3in solution, make OH in mixed solution
-with Al
3+mol ratio be 1:2.4, after dropwising, continue stir 4h, then by gained solution 80 DEG C of aging 24h, inorganic polymeric hydroxy metal cation column-supporting agent can be obtained;
(2) preparation of multiple elements design column-supporting agent: CTAB, DTPA are mixed with inorganic polymeric Hydroxy-Al cations column-supporting agent (wherein the mol ratio of DTPA and CTAB is total consumption of 1:1, DTPA and CTAB is 0.82mmol/g bentonite; The consumption of inorganic polymeric Hydroxy-Al cations column-supporting agent is: 10mmol/g bentonite), stir 2h, obtained multiple elements design column-supporting agent;
(3) preparation of poly modified bentonite adsorption material: take 3.0g sodium bentonite, adds the suspension 100mL that distilled water is made into mass percent 3%, stirring, static swelling 18h; 80 DEG C, under strong agitation, multiple elements design column-supporting agent is dropwise instilled bentonite suspension; After dropwising, continue to stir 24h, aging 36h at the same temperature subsequently; Suction filtration, the solid fraction material distilled water cyclic washing obtained, until without Cl
-and Br
-till, then dry to constant weight in 80 DEG C, grinding, cross 200 mesh sieves, the product obtained is the poly modified bentonite adsorption material of white powder.BET surface area is 132m
2/ g, pore volume is 0.11cm
3/ g, average pore size 2.58nm.
embodiment 6
(1) preparation of inorganic polymeric Hydroxy-Al cations column-supporting agent: under 80 DEG C, constantly stirring, first by the Na of 0.5mol/L
2cO
3solution slowly adds the 1.0mol/LAlCl of 3 times of volumes
3in solution, make OH in mixed solution
-with Al
3+mol ratio be 2.4:1, after dropwising; In 80 DEG C of aging 24h after continuation stirring 4h, obtain inorganic polymeric Hydroxy-Al cations column-supporting agent;
(2) preparation of multiple elements design column-supporting agent: CTAB, DTPA are mixed with inorganic polymeric Hydroxy-Al cations column-supporting agent (wherein the mol ratio of DTPA and CTAB is total consumption of 1:1, DTPA and CTAB is 1.23mmol/g bentonite; The consumption of inorganic polymeric Hydroxy-Al cations column-supporting agent is: 6mmol/g bentonite), stir 2h, obtained multiple elements design column-supporting agent;
(3) preparation of poly modified bentonite adsorption material: take 3.0g sodium bentonite, adds the suspension 100mL that distilled water is made into mass percent 3%, stirring, static swelling 12h; 80 DEG C, under strong agitation, multiple elements design column-supporting agent is dropwise instilled bentonite suspension; After dropwising, continue to stir 12h, aging 24h at the same temperature subsequently; Suction filtration, the solid fraction material distilled water cyclic washing obtained, until without Cl
-and Br
-till, then dry to constant weight in 80 DEG C, grinding, cross 200 mesh sieves, the product obtained is the poly modified bentonite adsorption material of white powder.BET surface area is 142m
2/ g, pore volume is 0.16cm
3/ g, average pore size 2.78nm.
Claims (7)
1. the preparation method of a poly modified bentonite adsorption material, using sodium bentonite as material of main part, with the short carbon chain organic complexing agent of organic Long carbon chain cationic surfactant, inorganic polymeric Hydroxy-Al cations and functionalization for multicomponent composite modifier, utilize copolymerization method to carry out poly modified to bentonite, obtain poly modified bentonite adsorption material.
2. the preparation method of bentonite adsorption material poly modified as claimed in claim 1, is characterized in that: first sodium bentonite distilled water is made into the suspension of 2 ~ 4%, stirs, leaves standstill swelling 12 ~ 24h; Again 50 ~ 80 DEG C, the polynary column-supporting agent that the short carbon chain organic complexing agent by organic Long carbon chain cationic surfactant, inorganic polymeric Hydroxy-Al cations, functionalization forms is added in bentonite suspension under strong agitation, continue stirring 12 ~ 36h, aging 24 ~ 48h subsequently, suction filtration, the solid fraction material distilled water cyclic washing obtained, until without Cl
-and Br
-till; Then dry to constant weight in 50 ~ 80 DEG C, grinding, cross 200 mesh sieves, the product obtained is white powder multiple elements design bentonite material for water treatment.
3. the preparation method of bentonite adsorption material poly modified as claimed in claim 1 or 2, it is characterized in that: the preparation of described inorganic polymeric Hydroxy-Al cations column-supporting agent: under 50 ~ 80 DEG C, constantly stirring, the alkaline solution of 0.2 ~ 1.8mol/L is slowly added 0.5 ~ 1.5mol/LAlCl of 3 ~ 6 times of volumes
3in solution, make OH in mixed solution
-with Al
3+mol ratio be 2:1 ~ 3:1; In 50 ~ 80 DEG C of aging 12 ~ 36h after stirring 3 ~ 4h, obtain inorganic polymeric Hydroxy-Al cations column-supporting agent.
4. the preparation method of bentonite adsorption material poly modified as claimed in claim 3, is characterized in that: described inorganic polymeric Hydroxy-Al cations column-supporting agent addition be: 6 ~ 10mmol/g bentonite.
5. the preparation method of bentonite adsorption material poly modified as claimed in claim 1 or 2, it is characterized in that: the mol ratio of the short carbon chain organic complexing agent of described organic Long carbon chain cationic surfactant and functionalization is 1:0.5 ~ 1:1.5, the total addition of the two is 0.82 ~ 1.23mmol/g bentonite.
6. the preparation method of bentonite adsorption material poly modified as claimed in claim 1 or 2, is characterized in that: described organic Long carbon chain cationic surfactant is softex kw or cetalkonium chloride.
7. the preparation method of bentonite adsorption material poly modified as claimed in claim 1 or 2, is characterized in that: the short carbon chain organic complexing agent of described functionalization is diethylene triamine pentacetic acid (DTPA), ethylenediamine tetra-acetic acid or citric acid.
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