CN102974320A - Method for preparing organic modified attapulgite adsorbent - Google Patents
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Abstract
The invention discloses a method for preparing an organic modified attapulgite adsorbent. An attapulgite or carbon nano composite material is prepared from cheap natural attapulgite clay and a biomass cellulose carbon source by a heterogeneous hydro-thermal synthesis method, so that organophilic amorphous carbon with a -CH functional group is loaded on the surfaces of attapulgite crystals. Compared with the natural non-modified attapulgite clay, the organic modified attapulgite adsorbent has the advantages that the removal rate to organic pollutants can be improved by more than 3 to 5 times, and the removal rate to methylene blue in water is 97 to 99 percent; and the adsorption balance time for the methylene blue is greatly shortened. The organic modification condition of attapulgite is mild; raw materials are readily available and are low in cost; the technical process is simple; the organic functional group is grafted to the surface of the modified attapulgite, so that the capacity of adsorbing the organic pollutants in water is obviously improved; and the organic modified attapulgite adsorbent can be used for deep treatment of the organic pollutants in water.
Description
One, technical field
The present invention relates to a kind of organically-modified method of attapulgite adsorbent, to improve attapulgite as the adsorption capacity of adsorbent to organic pollution, be applied to that micro quantity organic pollutant removes in the water body.
Two, background technology
Attapulgite is a kind of cheapness and the abundant zeopan clay mineral with chain layer structure of reserves, its monocrystal diameter is 30-50nm, having huge specific area, show nano effect, adsorption activity and chemism, is a kind of natural nano-mineral material of excellent performance.There is 3 types water in the attapulgite: constitution water, the crystallization water and zeolite water.The crystallization water in the attapulgite structure is positioned at its surface, duct, and it easily forms hydrogen bond with the adsorbate that is connected the duct and connects.Thereby when using as adsorbent, attapulgite to organic absorption a little less than.The traditional close Organic method of modifying of attapulgite is to utilize the in addition modification such as surfactant (such as cetyl ammonium bromide, bromohexadecane yl pyridines etc.), coupling agent (such as silane coupler and titanate coupling agent), high-temperature calcination organic matter and acid treatment.Yet surfactant, coupling agent and high temperature method modification exist that method of modifying is loaded down with trivial details, cost is high and consume energy the shortcoming such as large.
Three, summary of the invention
The present invention aims to provide a kind of preparation method of organically-modified attapulgite adsorbent, and technical problem to be solved is to improve it to the adsorption capacity of organic pollution by the close Organic that improves attapulgite.
Cellulose is a kind of polysaccharide that the occurring in nature distribution is the widest, content is maximum, accounts for more than 50% of plant kingdom's carbon content.According to the literature, in temperature is lower than 250 ℃ hydro-thermal reaction, cellulose can be hydrolyzed first and become oligosaccharide and monosaccharide, these materials compounds such as generating HMF and organic acid that ruptures again, the particulate carbon ball of these little molecule aggregation carbonization product nucleus shell structures afterwards, be rich in-OH ,-C=O ,-organic groups such as COOH.The advantages such as because Hydrothermal Synthesis possesses reaction condition gentleness (below 300 ℃), energy consumption is low, and reaction time is short and experimental facilities is simple, and growth characteristics is controlled are described as " green reaction " usually.Owing to be that low temperature is synthetic, the carbon material surface of acquisition generally all contains and enriches organo-functional group.Therefore this cheapness of cellulose widely living beings can prepare as hydro-thermal reaction the carbon source of composite.
Attapulgite has natural nanostructured, about tens nanometers of the diameter of single fiber crystalline substance, and length can reach 1 μ m.Utilize the natural hard template effect of attapulgite, adopt simple green one step hydro thermal method to induce cheap living beings carbon source cellulose in attapulgite surface carbonization, thereby obtain organically-modified attapulgite adsorbent, the grafting organo-functional group, improve the close Organic of attapulgite, improve it to the adsorption capacity of organic pollution.
The present invention is take Concave-convex clay rod and living beings carbon source cellulose as raw material, prepare organically-modified attapulgite adsorbent by heterogeneous hydrothermal synthesis method, the organically-modified attapulgite adsorbent of the present invention by attapulgite and plane of crystal load thereof contain-amorphous carbon of CH functional group forms, and therefore claims again attapulgite/carbon nanometer composite material.
The preparation method of the organically-modified attapulgite adsorbent of the present invention adopts the method for heterogeneous Hydrothermal Synthesis, it is characterized in that:
200 mesh sieves (d=74 μ m) are pulverized and crossed to the Concave-convex clay rod raw ore of attapulgite content 〉=98wt% get the attapulgite powder; With cellulose and the in mass ratio ratio mixing of 2-4:1 of described attapulgite powder, add catalyst, it is ultrasonic or dispersed with stirring is even to add water again, is warming up to 210-250 ℃ of reaction 12-48 hour, again through cooling, washing, dry and pulverize after obtain organically-modified concave and convex rod stone powder; Reactor volume filling rate remains on 70-80% during hydro-thermal reaction.
Described catalyst is six ferrous sulfate hydrate ammoniums, and the addition of catalyst is with Fe
2+Count the 3-10% of cellulose and attapulgite powder gross mass, 5-7% more preferably, carbonization degree that can the Effective Raise carbon source promotes the charcoal particle in growth and the dispersion on attapulgite surface.
The adsorption treatment that the organically-modified attapulgite adsorbent of the present invention is used for Organic Pollutants In Water:
Carry out adsorption treatment with phenol as organic pollution, the concentration of phenol solution is 5mg/L, and the addition of the organically-modified attapulgite adsorbent of the present invention and the solid-to-liquid ratio of phenol solution are 1g:50mL, and 25 ℃ of lower constant temperature oscillation absorption 12h measure the adsorbing and removing rate;
Carry out adsorption treatment with methylene blue as organic pollution, the concentration of methylene blue solution is 5mg/L, the addition of the organically-modified attapulgite adsorbent of the present invention and the solid-to-liquid ratio of methylene blue solution are 1g:1600-2500mL, and 25 ℃ of lower constant temperature oscillation absorption 4-12h measure the adsorbing and removing rate.
Compared with the prior art, beneficial effect of the present invention is embodied in:
1, the present invention adopts the method for Hydrothermal Synthesis, and attapulgite has kept original pattern and crystal structure, and its plane of crystal has inductive effect, so that charcoal obtains attapulgite/carbon nanometer composite material in its superficial growth after the charing of biomass cellulose hydro-thermal.Preparing the modified attapulgite method with 500 ℃ of-1000 ℃ of high-temperature calcinations of routine compares, the inventive method hydrothermal condition temperature is lower than 250 ℃, and need not atmosphere protection, need not to add any surfactant, is a kind of organically-modified method of attapulgite of environmental protection; Prepare modified attapulgite with the surfactant method of routine and compare, the inventive method is raw materials used to be easy to get, cheap, and the modification route is simple, and energy consumption is little.
2, the present invention is loaded with after the machine charcoal by hydro-thermal method, so that the close Organic of attapulgite improves, increases substantially for the absorption property of Typical Organic Pollutants.
Four, description of drawings
Fig. 1 is that cellulose and Concave-convex clay rod mass ratio are 2:1, and the addition of catalyst is with Fe
2+Count 5wt%, 240 ℃ of reaction temperatures, the reaction time is the SEM photo of the organically-modified attapulgite that obtains of 12h.As can be seen from Figure 1, nano carbon particle (50nm) is carried on attapulgite cluster surface.
Fig. 2 is that cellulose and Concave-convex clay rod mass ratio are 4:1, and the addition of catalyst is with Fe
2+Count 3.4wt%, 250 ℃ of reaction temperatures, the reaction time is the IR figure of the organically-modified attapulgite that obtains of 48h.As can be seen from Figure 2,2930cm
-1And 2851cm
-1The C-H vibration absorption peak of saturated hydrocarbons has appearred in the place, illustrate that cellulosic molecule contains on the attapulgite surface to have produced abundant organo-functional group after hydro-thermal reaction, thereby makes prepared attapulgite/carbon composite material possess the Organic of becoming engaged.
Fig. 3 be under the different temperatures (220-250 ℃) absorption property contrast (hydro-thermal time: 12h) of the organically-modified attapulgite that obtains and unmodified attapulgite Pyrogentisinic Acid.As can be seen from Figure 3, the attapulgite surface is loaded with after the modification of machine charcoal, and Pyrogentisinic Acid's adsorbing and removing ability improves greatly.Than unmodified attapulgite raw ore, modified attapulgite Pyrogentisinic Acid's removal efficiency can improve 3-5 times more than.
Fig. 4 cellulose and Concave-convex clay rod mass ratio are 2:1, and the addition of catalyst is with Fe
2+Count 5wt%, 220 ℃ of reaction temperatures, the reaction time is that 48h obtains organically-modified attapulgite and unmodified attapulgite to the adsorption equilibrium curve comparison (solid-to-liquid ratio 1:2500, adsorption time 4h, hunting speed 200r/min) of methylene blue.As can be seen from Figure 4, unmodified attapulgite raw ore is 6 hours to the time of equilibrium adsorption of methylene blue, and the attapulgite that is loaded with the modification of machine charcoal is 2 hours to the time of equilibrium adsorption of methylenum careuleum.Carry the charcoal parent organically-modified after, attapulgite has shortened 3 times to the time of equilibrium adsorption of methylene blue.
Five, specific implementation method
Embodiment 1:
200 mesh sieves are pulverized and crossed to the Concave-convex clay rod raw ore of attapulgite content 〉=98wt% get the attapulgite powder, get 2.5g attapulgite powder and 5g cellulose, in 72ml distilled water, mix, add again iron ammonium sulfate 2.8g, the ultrasonic mixed liquor that is uniformly dispersed to get, this moment, the pH value of mixed liquor was 5;
Described mixed liquor is transferred in the polytetrafluoroethylene (PTFE) water heating kettle, and filling rate remains on 75%, 250 ℃ of reaction temperatures, charing 12 hours; Reaction naturally cools to room temperature after finishing, and obtains the black product 60 ℃ of oven dry after centrifugation and water and ethanol alternately wash and is organically-modified attapulgite.
SEM and infrared spectrum analysis as can be known, the attapulgite area load contains the nano-sized carbon of the organo-functional groups such as C-H.
Getting initial concentration is that the 5mg/L phenol solution is organic pollution, in phenol solution, add organically-modified attapulgite adsorbent, solid-to-liquid ratio is 1g:50mL, and with 200r/min rotating speed constant temperature oscillation absorption 12h, the Adsorption of Phenol removal efficiency is that 70%(sees Fig. 3 under 25 ℃).
Embodiment 2:
200 mesh sieves are pulverized and crossed to the Concave-convex clay rod raw ore of attapulgite content 〉=98wt% get the attapulgite powder, get 2.5g attapulgite powder and 5g cellulose, in 72ml distilled water, mix, add again iron ammonium sulfate 2.8g, the ultrasonic mixed liquor that is uniformly dispersed to get, this moment, the pH value of mixed liquor was 5;
Described mixed liquor is transferred in the polytetrafluoroethylene (PTFE) water heating kettle, and filling rate remains on 80%, 240 ℃ of reaction temperatures, charing 12 hours; Reaction naturally cools to room temperature after finishing, and obtains the black product 60 ℃ of oven dry after centrifugation and water and ethanol alternately wash and is organically-modified attapulgite.
Infrared analysis as can be known, organically-modified attapulgite contains the organo-functional groups such as C-H; Amorphous carbon (see figure 1) that sem analysis has shown on attapulgite load.
Getting initial concentration is that the 5mg/L phenol solution is organic pollution, in phenol solution, add organically-modified attapulgite adsorbent, solid-to-liquid ratio is 1g:50mL, and with 200r/min rotating speed constant temperature oscillation absorption 12h, the Adsorption of Phenol removal efficiency is that 66%(sees Fig. 3 under 25 ℃).
Embodiment 3:
200 mesh sieves are pulverized and crossed to the Concave-convex clay rod raw ore of attapulgite content 98wt% get the attapulgite powder, get 2.5g attapulgite powder and 10g cellulose, in 72ml distilled water, mix, add again iron ammonium sulfate 3.0g, the ultrasonic mixed liquor that is uniformly dispersed to get, this moment, the pH value of mixed liquor was 5;
Described mixed liquor is transferred in the polytetrafluoroethylene (PTFE) water heating kettle, and filling rate remains on 80%, 250 ℃ of reaction temperatures, charing 48 hours; Reaction naturally cools to room temperature after finishing, and obtains the black product 60 ℃ of oven dry after centrifugation and water and ethanol alternately wash and is organically-modified attapulgite.
Infrared analysis as can be known, organically-modified attapulgite contains the organo-functional groups such as C-H.SEM characterize to have found on attapulgite load amorphous carbon.
Getting initial concentration is that the 5mg/L phenol solution is organic pollution, adds organically-modified attapulgite adsorbent in the phenol solution, and solid-to-liquid ratio is 1g:50mL, and with 200r/min rotating speed constant temperature oscillation absorption 12h, the Adsorption of Phenol removal efficiency is 92% under 25 ℃.
Embodiment 4:
200 mesh sieves are pulverized and crossed to the Concave-convex clay rod raw ore of attapulgite content 〉=98wt% get the attapulgite powder, get 2.5g attapulgite powder and 8g cellulose, in 72ml distilled water, mix, add again iron ammonium sulfate 5.8g, the ultrasonic mixed liquor that is uniformly dispersed to get, this moment, the pH value of mixed liquor was 5;
Described mixed liquor is transferred in the polytetrafluoroethylene (PTFE) water heating kettle, and filling rate remains on 70%, 210 ℃ of reaction temperatures, charing 24 hours; Reaction naturally cools to room temperature after finishing, and obtains the black product 60 ℃ of oven dry after centrifugation and water and ethanol alternately wash and is organically-modified attapulgite.
SEM and infrared spectrum analysis as can be known, the attapulgite area load contains the nano-sized carbon of the organo-functional groups such as C-H.
Getting initial concentration is that the 5mg/L phenol solution is organic pollution, adds organically-modified attapulgite adsorbent in the phenol solution, and solid-to-liquid ratio is 1g:50mL, and with 200r/min rotating speed constant temperature oscillation absorption 12h, the Adsorption of Phenol removal efficiency is 60% under 25 ℃.
Embodiment 5:
200 mesh sieves are pulverized and crossed to the Concave-convex clay rod raw ore of attapulgite content 98wt% get the attapulgite powder, get 2.5g attapulgite powder and 5g cellulose, in 72ml distilled water, mix, add again iron ammonium sulfate 2.8g, the ultrasonic mixed liquor that is uniformly dispersed to get, this moment, the pH value of mixed liquor was 5;
Described mixed liquor is transferred in the polytetrafluoroethylene (PTFE) water heating kettle, and filling rate remains on 80%, 220 ℃ of reaction temperatures, charing 24 hours; Reaction naturally cools to room temperature after finishing, and obtains the black product 60 ℃ of oven dry after centrifugation and water and ethanol alternately wash and is organically-modified attapulgite.
Getting initial concentration is that the 5mg/L methylene blue solution is organic pollution, in methylene blue solution, add organically-modified attapulgite adsorbent, solid-to-liquid ratio is 1g:2500mL, and with 200r/min rotating speed constant temperature oscillation absorption 6h, the methylene blue adsorption number removal efficiency is that 97%(sees Fig. 4 under 25 ℃).
Embodiment 6:
200 mesh sieves are pulverized and crossed to the Concave-convex clay rod raw ore of attapulgite content 98wt% get the attapulgite powder, get 2.5g attapulgite powder and 5g cellulose, in 72ml distilled water, mix, add again iron ammonium sulfate 2.8g, the ultrasonic mixed liquor that is uniformly dispersed to get, this moment, the pH value of mixed liquor was 5;
Described mixed liquor is transferred in the polytetrafluoroethylene (PTFE) water heating kettle, and filling rate remains on 80%, 220 ℃ of reaction temperatures, charing 48 hours; Reaction naturally cools to room temperature after finishing, and obtains the black product 60 ℃ of oven dry after centrifugation and water and ethanol alternately wash and is organically-modified attapulgite.
Getting initial concentration is that the 5mg/L methylene blue solution is organic pollution, in methylene blue solution, add organically-modified attapulgite adsorbent, solid-to-liquid ratio is 1g:1600mL, and with 200r/min rotating speed constant temperature oscillation absorption 4h, the methylene blue adsorption number removal efficiency is 99% under 25 ℃.
Embodiment 7: contrast test
Getting initial concentration is that the 5mg/L phenol solution is target contaminant, and attapulgite raw ore and phenol solution solid-to-liquid ratio are 1g:50mL, under 25 ℃ with 200r/min rotating speed constant temperature oscillation absorption 12h.The Adsorption of Phenol removal efficiency is 18%.
Embodiment 8: contrast test
Getting initial concentration is that the 5mg/L methylene blue solution is target contaminant, and attapulgite raw ore and methylene blue solution solid-to-liquid ratio are 1g:2500mL, under 25 ℃ with 200r/min rotating speed constant temperature oscillation absorption 6h.The methylene blue adsorption number removal efficiency is 94%.(seeing Fig. 4).
Claims (3)
1. the preparation method of an organically-modified attapulgite adsorbent adopts the method for heterogeneous Hydrothermal Synthesis, it is characterized in that:
200 mesh sieves are pulverized and crossed to the Concave-convex clay rod raw ore of attapulgite content 98wt% get the attapulgite powder; With cellulose and the in mass ratio ratio mixing of 2-4:1 of described attapulgite powder, add catalyst, it is ultrasonic or dispersed with stirring is even to add water again, is warming up to 210-250 ℃ of reaction 12-48 hour, again through cooling, washing, dry and pulverize after obtain organically-modified concave and convex rod stone powder.
2. preparation method according to claim 1 is characterized in that:
Described catalyst is six ferrous sulfate hydrate ammoniums, and the addition of described catalyst is with Fe
2+Count the 3-10% of cellulose and attapulgite powder gross mass.
3. preparation method according to claim 2 is characterized in that:
The addition of described catalyst is with Fe
2+Count the 5-7% of cellulose and attapulgite powder gross mass.
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| CN103723824A (en) * | 2013-12-26 | 2014-04-16 | 南京大学 | Carbon-iron microbattery slow-release carbon source filler and preparation method thereof |
| CN104289179A (en) * | 2014-09-24 | 2015-01-21 | 合肥工业大学 | Method for preparing attapulgite/carbon composite adsorbent by one-step carbonization-activation |
| CN104289178A (en) * | 2014-09-24 | 2015-01-21 | 合肥工业大学 | Method for preparing attapulgite/carbon adsorbent based on hydrothermal-activation coupling technology |
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