CN102974320B - A kind of preparation method of organically-modified attapulgite adsorbent - Google Patents
A kind of preparation method of organically-modified attapulgite adsorbent Download PDFInfo
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- CN102974320B CN102974320B CN201210550251.8A CN201210550251A CN102974320B CN 102974320 B CN102974320 B CN 102974320B CN 201210550251 A CN201210550251 A CN 201210550251A CN 102974320 B CN102974320 B CN 102974320B
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Abstract
The invention discloses a kind of preparation method of organically-modified attapulgite adsorbent, for raw material with the natural attapulgite clay of cheapness and biomass cellulose carbon source, prepare attapulgite/carbon nanometer composite material by heterogeneous hydrothermal synthesis method, make the load of attapulgite plane of crystal have close organic trait containing-CH functional group amorphous carbon.Compared with natural, unmodified Concave-convex clay rod, modified attapulgite adsorbent can improve more than 3-5 times to the removal efficiency of organic pollutants phenol, is 97-99%, greatly shortens methylene blue adsorption number equilibration time water Methylene Blue removal efficiency.The organically-modified mild condition of the attapulgite that the present invention relates to, raw material sources are extensively cheap, and technical process is simple, gained modified attapulgite surface graft organo-functional group, the adsorption capacity of organic pollutants is significantly improved, can be used for the advanced treating of organic pollutants.
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 micro quantity organic pollutant in water body and remove.
Two, background technology
Attapulgite is a kind of cheapness and the zeopan clay mineral with chain layer structure of rich 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.The water of 3 types is there is: constitution water, the crystallization water and zeolite water in attapulgite.The crystallization water in attapulgite structure is positioned at its channel surfaces, and it easily forms hydrogen bond with the adsorbate entering duct and is connected.Thus, when using as adsorbent, attapulgite is more weak to organic absorption.The traditional close Organic method of modifying of attapulgite utilizes the modification in addition such as surfactant (as cetyl ammonium bromide, bromide sixteen alkyls pyridine etc.), coupling agent (as silane coupler and titanate coupling agent), high-temperature calcination organic matter and acid treatment.But surfactant, coupling agent and high temperature method modification also exist that method of modifying is loaded down with trivial details, cost is high and the shortcoming such as large that consumes energy.
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 that the close Organic by improving attapulgite improves its adsorption capacity to organic pollution.
Cellulose is a kind of polysaccharide that 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 the hydro-thermal reaction of temperature lower than 250 DEG C, cellulose first can be hydrolyzed and become oligosaccharide and monosaccharide, these materials rupture and generate the compound such as HMF and organic acid, the carbonization of these Small molecular polymerization afterwards generates the particulate carbon ball of nucleocapsid structure, is rich in the organic groups such as-OH ,-C=O ,-COOH.Because Hydrothermal Synthesis possesses reaction condition gentleness (less than 300 DEG C), energy consumption is low, and reaction time is short and experimental facilities simple, and the advantages such as growth characteristics is controlled, are described as " green reaction " usually.Owing to being low temperature synthesis, the carbon material surface of acquisition is generally all containing enriching organo-functional group.Therefore this cheapness of cellulose widely living beings can be used as hydro-thermal reaction and prepare the carbon source of composite.
Attapulgite has natural nanostructured, and about tens nanometers of diameter of single fiber crystalline substance, length can reach 1 μm.Utilize the natural hard template effect of attapulgite, the living beings carbon source cellulose adopting simple green one step hydro thermal method induction cheap is at attapulgite surface carbonation, thus obtain organically-modified attapulgite adsorbent, grafting organo-functional group, improve the close Organic of attapulgite, improve its adsorption capacity to organic pollution.
The present invention with Concave-convex clay rod and living beings carbon source cellulose for raw material, organically-modified attapulgite adsorbent is prepared by heterogeneous hydrothermal synthesis method, the amorphous carbon that the organically-modified attapulgite adsorbent of the present invention contains-CH functional group by attapulgite and plane of crystal load thereof forms, therefore also known as 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:
The Concave-convex clay rod raw ore of attapulgite content >=98wt% is pulverized and crosses 200 mesh sieves (d=74 μm) and obtain attapulgite powder; By the ratio mixing of cellulose and described attapulgite powder 2-4:1 in mass ratio, add catalyst, ultrasonic or the dispersed with stirring of adding water again is even, is warming up to 210-250 DEG C of reaction 12-48 hour, then through cooling, washing, dry and obtain organically-modified concave and convex rod stone powder after pulverizing; During hydro-thermal reaction, reactor volumetric filling ratio remains on 70-80%.
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, more preferably 5-7%, effectively can improve the carbonization degree of carbon source, promote the growth on attapulgite surface of charcoal particle and dispersion.
Organically-modified for the present invention attapulgite adsorbent is used for the adsorption treatment of Organic Pollutants In Water:
Carry out adsorption treatment using 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 at 25 DEG C, constant temperature oscillation absorption 12h, measures adsorbing and removing rate;
Adsorption treatment is carried out using 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 at 25 DEG C, constant temperature oscillation absorption 4-12h, measures 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 remains original pattern and crystal structure, and its plane of crystal has inductive effect, and after biomass cellulose hydro-thermal is carbonized, charcoal is in its superficial growth, obtains attapulgite/carbon nanometer composite material.Compared with preparing modified attapulgite method with 500 DEG C of-1000 DEG C of high-temperature calcinations of routine, the inventive method hydrothermal condition temperature is lower than 250 DEG C, and without the need to atmosphere protection, without the need to adding any surfactant, be a kind of organically-modified method of attapulgite of environmental protection; Compared with preparing modified attapulgite with the surfactant method of routine, the inventive method is raw materials used to be easy to get, cheap, modification route is simple, and energy consumption is little.
2, after the present invention carries Organic carbon by hydro-thermal method, the close Organic of attapulgite is improved, and the absorption property for Typical Organic Pollutants increases substantially.
Four, accompanying drawing explanation
Fig. 1 is cellulose and Concave-convex clay rod mass ratio is 2:1, and the addition of catalyst is with Fe
2+count 5wt%, reaction temperature 240 DEG C, the SEM photo of the organically-modified attapulgite that the reaction time obtains for 12h.As can be seen from Figure 1, nano carbon particle (50nm) is carried on attapulgite cluster surface.
Fig. 2 is cellulose and Concave-convex clay rod mass ratio is 4:1, and the addition of catalyst is with Fe
2+count 3.4wt%, reaction temperature 250 DEG C, the IR figure of the organically-modified attapulgite that the reaction time obtains for 48h.As can be seen from Figure 2,2930cm
-1and 2851cm
-1having there is the C-H vibration absorption peak of saturated hydrocarbons in place, illustrates that cellulosic molecule is surperficial containing creating abundant organo-functional group at attapulgite after hydro-thermal reaction, thus make prepared attapulgite/carbon composite material possess an engagement Organic.
Fig. 3 be under different temperatures (220-250 DEG C) obtain organically-modified attapulgite and unmodified attapulgite Pyrogentisinic Acid absorption property contrast (hydro-thermal time: 12h).As can be seen from Figure 3, after Organic carbon modification is carried on attapulgite surface, the adsorbing and removing ability of Pyrogentisinic Acid improves greatly.Compared to unmodified attapulgite raw ore, the removal efficiency of modified attapulgite Pyrogentisinic Acid 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%, reaction temperature 220 DEG C, the reaction time obtains by 48h 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 carrying Organic carbon modification is 2 hours to the time of equilibrium adsorption of methylenum careuleum.Carry charcoal parent organically-modified after, the time of equilibrium adsorption of attapulgite to methylene blue shortens 3 times.
Five, specific implementation method
Embodiment 1:
The Concave-convex clay rod raw ore of attapulgite content >=98wt% is pulverized and crossed 200 mesh sieves and obtains attapulgite powder, get 2.5g attapulgite powder and 5g cellulose, mix in 72ml distilled water, add iron ammonium sulfate 2.8g again, ultrasonic disperse is even obtains mixed liquor, and now the pH value of mixed liquor is 5;
Be transferred in polytetrafluoroethylene (PTFE) water heating kettle by described mixed liquor, filling rate remains on 75%, reaction temperature 250 DEG C, carbonizes 12 hours; Naturally cool to room temperature after reaction terminates, centrifugation obtains black product 60 DEG C of oven dry after also alternately washing with water and ethanol and is organically-modified attapulgite.
SEM and infrared spectrum analysis known, attapulgite area load contains the nano-sized carbon of the organo-functional groups such as C-H.
To get initial concentration be 5mg/L phenol solution is organic pollution, organically-modified attapulgite adsorbent is added in phenol solution, solid-to-liquid ratio is 1g:50mL, and with 200r/min rotating speed constant temperature oscillation absorption 12h at 25 DEG C, Adsorption of Phenol removal efficiency is that 70%(is shown in Fig. 3).
Embodiment 2:
The Concave-convex clay rod raw ore of attapulgite content >=98wt% is pulverized and crossed 200 mesh sieves and obtains attapulgite powder, get 2.5g attapulgite powder and 5g cellulose, mix in 72ml distilled water, add iron ammonium sulfate 2.8g again, ultrasonic disperse is even obtains mixed liquor, and now the pH value of mixed liquor is 5;
Be transferred in polytetrafluoroethylene (PTFE) water heating kettle by described mixed liquor, filling rate remains on 80%, reaction temperature 240 DEG C, carbonizes 12 hours; Naturally cool to room temperature after reaction terminates, centrifugation obtains black product 60 DEG C of oven dry after also alternately washing with water and ethanol and is organically-modified attapulgite.
Infrared analysis is known, and organically-modified attapulgite contains the organo-functional groups such as C-H; Sem analysis to show on attapulgite load amorphous carbon (see figure 1).
To get initial concentration be 5mg/L phenol solution is organic pollution, organically-modified attapulgite adsorbent is added in phenol solution, solid-to-liquid ratio is 1g:50mL, and with 200r/min rotating speed constant temperature oscillation absorption 12h at 25 DEG C, Adsorption of Phenol removal efficiency is that 66%(is shown in Fig. 3).
Embodiment 3:
The Concave-convex clay rod raw ore of attapulgite content >=98wt% is pulverized and crossed 200 mesh sieves and obtains attapulgite powder, get 2.5g attapulgite powder and 10g cellulose, mix in 72ml distilled water, add iron ammonium sulfate 3.0g again, ultrasonic disperse is even obtains mixed liquor, and now the pH value of mixed liquor is 5;
Be transferred in polytetrafluoroethylene (PTFE) water heating kettle by described mixed liquor, filling rate remains on 80%, reaction temperature 250 DEG C, carbonizes 48 hours; Naturally cool to room temperature after reaction terminates, centrifugation obtains black product 60 DEG C of oven dry after also alternately washing with water and ethanol and is organically-modified attapulgite.
Infrared analysis is known, and organically-modified attapulgite contains the organo-functional groups such as C-H.SEM characterizes and finds load amorphous carbon on attapulgite.
To get initial concentration be 5mg/L phenol solution is organic pollution, and 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 at 25 DEG C, Adsorption of Phenol removal efficiency is 92%.
Embodiment 4:
The Concave-convex clay rod raw ore of attapulgite content >=98wt% is pulverized and crossed 200 mesh sieves and obtains attapulgite powder, get 2.5g attapulgite powder and 8g cellulose, mix in 72ml distilled water, add iron ammonium sulfate 5.8g again, ultrasonic disperse is even obtains mixed liquor, and now the pH value of mixed liquor is 5;
Be transferred in polytetrafluoroethylene (PTFE) water heating kettle by described mixed liquor, filling rate remains on 70%, reaction temperature 210 DEG C, carbonizes 24 hours; Naturally cool to room temperature after reaction terminates, centrifugation obtains black product 60 DEG C of oven dry after also alternately washing with water and ethanol and is organically-modified attapulgite.
SEM and infrared spectrum analysis known, attapulgite area load contains the nano-sized carbon of the organo-functional groups such as C-H.
To get initial concentration be 5mg/L phenol solution is organic pollution, and 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 at 25 DEG C, Adsorption of Phenol removal efficiency is 60%.
Embodiment 5:
The Concave-convex clay rod raw ore of attapulgite content >=98wt% is pulverized and crossed 200 mesh sieves and obtains attapulgite powder, get 2.5g attapulgite powder and 5g cellulose, mix in 72ml distilled water, add iron ammonium sulfate 2.8g again, ultrasonic disperse is even obtains mixed liquor, and now the pH value of mixed liquor is 5;
Be transferred in polytetrafluoroethylene (PTFE) water heating kettle by described mixed liquor, filling rate remains on 80%, reaction temperature 220 DEG C, carbonizes 24 hours; Naturally cool to room temperature after reaction terminates, centrifugation obtains black product 60 DEG C of oven dry after also alternately washing with water and ethanol and is organically-modified attapulgite.
To get initial concentration be 5mg/L methylene blue solution is organic pollution, organically-modified attapulgite adsorbent is added in methylene blue solution, solid-to-liquid ratio is 1g:2500mL, and with 200r/min rotating speed constant temperature oscillation absorption 6h at 25 DEG C, methylene blue adsorption number removal efficiency is that 97%(is shown in Fig. 4).
Embodiment 6:
The Concave-convex clay rod raw ore of attapulgite content >=98wt% is pulverized and crossed 200 mesh sieves and obtains attapulgite powder, get 2.5g attapulgite powder and 5g cellulose, mix in 72ml distilled water, add iron ammonium sulfate 2.8g again, ultrasonic disperse is even obtains mixed liquor, and now the pH value of mixed liquor is 5;
Be transferred in polytetrafluoroethylene (PTFE) water heating kettle by described mixed liquor, filling rate remains on 80%, reaction temperature 220 DEG C, carbonizes 48 hours; Naturally cool to room temperature after reaction terminates, centrifugation obtains black product 60 DEG C of oven dry after also alternately washing with water and ethanol and is organically-modified attapulgite.
To get initial concentration be 5mg/L methylene blue solution is organic pollution, organically-modified attapulgite adsorbent is added in methylene blue solution, solid-to-liquid ratio is 1g:1600mL, and with 200r/min rotating speed constant temperature oscillation absorption 4h at 25 DEG C, methylene blue adsorption number removal efficiency is 99%.
Embodiment 7: contrast test
To get initial concentration be 5mg/L phenol solution is target contaminant, and attapulgite raw ore and phenol solution solid-to-liquid ratio are 1g:50mL, with 200r/min rotating speed constant temperature oscillation absorption 12h at 25 DEG C.Adsorption of Phenol removal efficiency is 18%.
Embodiment 8: contrast test
To get initial concentration be 5mg/L methylene blue solution is target contaminant, and attapulgite raw ore and methylene blue solution solid-to-liquid ratio are 1g:2500mL, with 200r/min rotating speed constant temperature oscillation absorption 6h at 25 DEG C.Methylene blue adsorption number removal efficiency is 94%.(see Fig. 4).
Claims (2)
1. a preparation method for organically-modified attapulgite adsorbent, adopts the method for heterogeneous Hydrothermal Synthesis, it is characterized in that:
The Concave-convex clay rod raw ore of attapulgite content 98wt% is pulverized and crossed 200 mesh sieves and obtains attapulgite powder, get 2.5g attapulgite powder and 10g cellulose, mix in 72ml distilled water, add iron ammonium sulfate 3.0g again, ultrasonic disperse is even obtains mixed liquor, and now the pH value of mixed liquor is 5;
Be transferred in polytetrafluoroethylene (PTFE) water heating kettle by described mixed liquor, filling rate remains on 80%, reaction temperature 250 DEG C, carbonizes 48 hours; Naturally cool to room temperature after reaction terminates, centrifugation obtains black product 60 DEG C of oven dry after also alternately washing with water and ethanol and is organically-modified attapulgite.
2. a preparation method for organically-modified attapulgite adsorbent, adopts the method for heterogeneous Hydrothermal Synthesis, it is characterized in that:
The Concave-convex clay rod raw ore of attapulgite content 98wt% is pulverized and crossed 200 mesh sieves and obtains attapulgite powder, get 2.5g attapulgite powder and 5g cellulose, mix in 72ml distilled water, add iron ammonium sulfate 2.8g again, ultrasonic disperse is even obtains mixed liquor, and now the pH value of mixed liquor is 5;
Be transferred in polytetrafluoroethylene (PTFE) water heating kettle by described mixed liquor, filling rate remains on 80%, reaction temperature 220 DEG C, carbonizes 48 hours; Naturally cool to room temperature after reaction terminates, centrifugation obtains black product 60 DEG C of oven dry after also alternately washing with water and ethanol and is organically-modified attapulgite.
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| CN104289179B (en) * | 2014-09-24 | 2017-01-18 | 合肥工业大学 | Method for preparing attapulgite/carbon composite adsorbent by one-step carbonization-activation |
| CN104289178B (en) * | 2014-09-24 | 2016-08-31 | 合肥工业大学 | The method preparing attapulgite/carbon adsorbent based on hydro-thermal-activation coupling technology |
| CN105396552B (en) * | 2015-12-18 | 2018-08-03 | 中国科学技术大学 | A kind of molding biological carbon and preparation method thereof |
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| CN109078611A (en) * | 2018-09-16 | 2018-12-25 | 安徽乐农环保科技有限公司 | Target heavy-metal adsorption material and preparation method thereof |
| CN113023851A (en) * | 2021-03-24 | 2021-06-25 | 湖南久正环保科技有限公司 | Medicament capable of removing activated carbon powder in wastewater |
| CN116459790B (en) * | 2023-04-24 | 2024-03-29 | 西华师范大学 | Preparation method of flying wadding fiber loaded zero-valent nano silver high-efficiency fixed gaseous iodine material |
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