CN103191696A - Method for improving adsorption property of attapulgite by using hydrothermal process - Google Patents
Method for improving adsorption property of attapulgite by using hydrothermal process Download PDFInfo
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Abstract
The invention discloses a method for improving the adsorption property of an attapulgite by using a hydrothermal process. The attapulgite is treated by using the hydrothermal process, and treatment parameters such as reaction temperature, reaction time and raw material concentration are optimized, so that the adsorption property of the attapulgite can be remarkably improved. Compared with a natural attapulgite, the attapulgite subjected to hydrothermal treatment has the advantages that the specific surface area of the attapulgite is remarkably increased, and the equilibrium adsorption capacity of the attapulgite to methylene blue in water is remarkably increased. The equilibrium adsorption capacity of the raw ore of the attapulgite to the methylene blue is 220mg/g, the adsorption capacity of the attapulgite which is subjected to hydrothermal treatment at the temperature of 110 DEG C for 12h to the methylene blue is highest, and the equilibrium adsorption capacity is up to 277.5mg/g which is increased by 26% as comparison with that of the raw ore.
Description
One, technical field
What the present invention relates to is that attapulgite is carried out hydro-thermal method modification cheaply, improves it to the absorption property of organic dyestuff in the water with modified attapulgite as adsorbent, can be applicable to removing of micro-difficult degradation dyestuff in the water body.
Two, background technology
Attapulgite is a kind of stratiform hydration zeopan mineral of natural nanoscale, has more rich pore passage structure and bigger specific area and stronger absorption property.Therefore, attapulgite has been widely used in various fields, comprises heavy metal ion and dye sorbent, catalyst carrier.Yet the attapulgite surface has stronger hydrophily, makes its adsorption capacity and applicability have much room for improvement, especially to the organic pollutant adsorption performance relatively a little less than.The traditional close organically-modified method of attapulgite mainly is surfactant-modified, for example utilizes surfactant (as cetyl ammonium bromide, OTAC etc.) and coupling agent (as silane coupler and titanate coupling agent) that attapulgite is carried out modification; Also have method of modifying such as high-temperature calcination and acid treatment in addition.Yet surfactant and coupling agent modified to exist method of modifying loaded down with trivial details, shortcomings such as cost height.High-temperature calcination modified attapulgite, reaction temperature reach more than 500 ℃ at least, and energy consumption is big, and the removal efficiency of methylene blue is had only 69%.
Three, summary of the invention
The present invention aims to provide the method that a kind of hydro-thermal method modification improves the attapulgite absorption property, and technical problem to be solved is to improve it to the adsorption capacity of difficult degradation organic dyestuff in the water by the specific area that improves attapulgite.
Hydro-thermal method modification of the present invention improves the method for attapulgite absorption property, and difference with the prior art is:
200 mesh sieves (d=74 μ m) are pulverized and crossed to the Concave-convex clay rod raw ore of attapulgite content 〉=95wt% get the attapulgite powder; The mass volume ratio of described attapulgite powder and distilled water being pressed 1g:8-32mL mixes, ultrasonic being uniformly dispersed is warming up to 100-120 ℃, reaction 6-24h, reaction is cooled to room temperature after finishing, and obtains the modified attapulgite stone powder through washing, drying with after pulverizing successively.
The mass volume ratio of described attapulgite powder and the preferred 1g:16mL of distilled water is mixed into optimal proportion.
Reaction temperature is preferably 110 ℃, and the reaction time is preferably 12h, is optimum hydrothermal condition.
Attapulgite is a kind of cheapness and the abundant zeopan clay mineral with chain layer structure of reserves, and its bigger specific area, Surface Physical chemical constitution and charge characteristic etc. make Concave-convex clay rod have the good adsorption characteristic.The present invention is raw material with the attapulgite, adopts hydro-thermal method that attapulgite has been carried out modification.After the hydrothermal treatment consists, the dispersiveness of attapulgite in the aqueous solution improves, and progressively removes the hydrone of different shape in the hydrothermal treatment consists process, and pore passage structure is corresponding to change, and improves thereby organic pollutant adsorption is removed ability.
The present invention is raw material with the Concave-convex clay rod, adopts heterogeneous hydro-thermal method to handle attapulgite, obtains the attapulgite adsorbent that specific area increases.
Methylene blue is a kind of waste water from dyestuff pollutant of common very difficult degraded, and the surface of solids is shown good affinity, and commonly used at dye industry.It mainly is to be parent with aromatic hydrocarbons and heterocyclic compound, and has colour developing group and polar group, complex structure, and stable performance, this has brought very big difficulty for processing of dyeing waste water.The processing method that is used for the improvement waste water from dyestuff at present mainly comprises biological oxidation process, oxidizing process, photocatalytic method, absorption method, Coagulation Method and electrochemical process etc.Wherein absorption method is easy and simple to handle with it, cost is low and receive much concern.In the absorption method processing procedure, adsorbent is core.
The adsorption treatment that modified attapulgite of the present invention is used for the water body organic dyestuff:
The present invention carries out adsorption treatment with methylene blue as the representative of waste water dyestuff, the initial concentration of methylene blue is 500mg/L, the addition of modified attapulgite of the present invention and the solid-to-liquid ratio of methylene blue solution are 1g:2500mL, 200r/min, constant temperature vibration absorption 12-24h under 30 ° of C.
The solid-to-liquid ratio of hydro-thermal method modified attapulgite sample addition of the present invention and methylene blue solution (500mg/L) is 1g:2500mL, 200r/min, and constant temperature vibration 12-24h measures the methylene blue equilibrium adsorption capacity under 30 ° of C.
Compared with the prior art, the technology of the present invention advantage is embodied in:
1, the present invention adopts hydro-thermal method that attapulgite is carried out modification, and simple, process is energy-conservation, the non-secondary pollution discharging.Traditional acid treatment, heat treatment, shortcoming such as methods such as high-temperature calcination and surfactant are carried out modification to attapulgite, and it is expensive to exist raw material (acid), and calcining heat height (〉=500 ℃) or method of modifying are loaded down with trivial details.Compare with these methods, the hydro-thermal method raw material only relates to cleaning, attapulgite and water pollution-free and cheap and easy to get, and reaction condition gentleness (≤150 ℃) is simple to operate, no any pollution in the course of reaction, environmental protection.
2, the present invention is by the hydro-thermal method modified attapulgite, and under the optimal conditions, the specific area of attapulgite enlarges markedly after the hydrothermal treatment consists, obviously improves for the absorption property of the waste water dyestuff (methylene blue) of typical difficult degradation.
Four, description of drawings
Fig. 1 is the IR collection of illustrative plates of modified attapulgite among attapulgite former state and the embodiment 1.As can be seen from Figure 1, after the hydrothermal treatment consists, at 1656cm
-1The intensity at peak, place has weakened.This is that attapulgite removes the hydrone of different shape because during hydro-thermal reaction, thereby the intensity at peak has weakened.
Fig. 2 is attapulgite former state and embodiment 1, comparative example 1, and comparative example 2, the attapulgite sample in the comparative example 3 is to the adsorption equilibrium curve of methylene blue.As can be seen from Figure 2, in the absorption incipient stage, different attapulgites to the adsorbance of methylene blue along with time lengthening improves rapidly.When adsorption time was 12h, absorption reached balance substantially.And the attapulgite of 110 ° of C hydrothermal treatment consists illustrates that to the absorption of methylene blue obviously more effective than the raw ore (embodiment 1) the hydrothermal treatment consists attapulgite can significantly improve it to the adsorption capacity of methylene blue.
Fig. 3 is attapulgite former state and embodiment 1, and embodiment 2, and embodiment 3, and embodiment 4, and the modified attapulgite sample among the embodiment 5 is to the absorption of methylene blue (500mg/L), and absorption reaches balance.As can be seen from Figure 3, the attapulgite former state is 220mg/g to the equilibrium adsorption capacity of methylene blue.The sample of 110 ° of C hydrothermal treatment consists is better than the attapulgite former state to the adsorption effect of methylene blue, illustrates that the hydrothermal treatment consists attapulgite can improve its absorption property.
Five, specific implementation method
Embodiment 1:
200 mesh sieves are pulverized and crossed to the Concave-convex clay rod raw ore of attapulgite content 95wt% get the attapulgite powder, get 1g attapulgite powder, add 16mL distilled water, use magnetic stirrer 2h, make solution mix mixed liquor, record pH of mixed value 7 this moment;
Described mixed liquor is transferred in the polytetrafluoroethylene (PTFE) water heating kettle, and reaction temperature is 110 ℃, and the reaction time is 12h; Naturally cool to room temperature after reaction finishes, centrifugation also washes the back with water and obtains modified attapulgite 60 ℃ of oven dry.
By infrared spectrum analysis as can be known, after the hydrothermal treatment consists, at 1656cm
-1The intensity at peak, place has weakened.This is that attapulgite has removed the hydrone of different shape because during hydro-thermal reaction, thereby the intensity at peak has weakened (see figure 1).
Analyzed as can be known by the BET value, gained modified attapulgite BET value is 238, is maximum (the seeing Table 1) of BET value in all modified attapulgites.
The methylene blue solution of getting initial concentration and be 500mg/L is organic pollution, the solid-to-liquid ratio of modified attapulgite and methylene blue is 1g:2500mL, with the rotating speed constant temperature vibration absorption 12h of 200r/min, be that 277.5mg/g(sees Fig. 3 to the equilibrium adsorption capacity of methylene blue under 30 ° of C).
Embodiment 2:
200 mesh sieves are pulverized and crossed to the Concave-convex clay rod raw ore of attapulgite content 95wt% get the attapulgite powder, get 1g attapulgite powder, add 8mL distilled water, use magnetic stirrer 2h, make solution mix mixed liquor, record pH of mixed value 7 this moment;
Described mixed liquor is transferred in the polytetrafluoroethylene (PTFE) water heating kettle, and reaction temperature is 110 ℃, and the reaction time is 12h; Naturally cool to room temperature after reaction finishes, centrifugation also washes the back with water and obtains modified attapulgite 60 ℃ of oven dry.
Analyzed as can be known by the BET value, gained modified attapulgite BET value is 225, is higher than the BET value (seeing Table 1) of attapulgite former state.
The methylene blue solution of getting initial concentration and be 500mg/L is organic pollution, the solid-to-liquid ratio of modified attapulgite and methylene blue is 1g:2500mL, rotating speed constant temperature vibration absorption 12h with 200r/min under 30 ° of C reaches balance, is that 265mg/g(sees Fig. 3 to the equilibrium adsorption capacity of methylene blue).
Embodiment 3:
200 mesh sieves are pulverized and crossed to the Concave-convex clay rod raw ore of attapulgite content 95wt% get the attapulgite powder, get 1g attapulgite powder, add 32mL distilled water, use magnetic stirrer 2h, make solution mix mixed liquor, record pH of mixed value 7 this moment;
Described mixed liquor is transferred in the polytetrafluoroethylene (PTFE) water heating kettle, and reaction temperature is 110 ° of C, and the reaction time is 12h; Naturally cool to room temperature after reaction finishes, centrifugation also washes the back with water and obtains modified attapulgite 60 ° of C oven dry.
Analyzed as can be known by the BET value, gained modified attapulgite BET value is 216, is higher than the BET value (seeing Table 1) of attapulgite former state.
The methylene blue solution of getting initial concentration and be 500mg/L is organic pollution, the solid-to-liquid ratio of modified attapulgite and methylene blue is 1g:2500mL, rotating speed constant temperature vibration absorption 12h with 200r/min under 30 ° of C reaches balance, is that 248mg/g(sees Fig. 2 to the equilibrium adsorption capacity of methylene blue).
Embodiment 4:
200 mesh sieves are pulverized and crossed to the Concave-convex clay rod raw ore of attapulgite content 95wt% get the attapulgite powder, get 1g attapulgite powder, add 16mL distilled water, use magnetic stirrer 2h, make solution mix mixed liquor, record pH of mixed value 7 this moment;
Described mixed liquor is transferred in the polytetrafluoroethylene (PTFE) water heating kettle, and reaction temperature is 110 ° of C, and the reaction time is respectively 6h; Naturally cool to room temperature after reaction finishes, centrifugation also washes the back with water and obtains modified attapulgite 60 ° of C oven dry.
Analyzed as can be known by the BET value, gained modified attapulgite BET value is 217, is higher than attapulgite former state BET value (seeing Table 1).
The methylene blue solution of getting initial concentration and be 500mg/L is organic pollution, the solid-to-liquid ratio of modified attapulgite and methylene blue is 1g:2500mL, rotating speed constant temperature vibration absorption 12h with 200r/min under 30 ° of C reaches balance, is that 235mg/g(sees Fig. 2 to the equilibrium adsorption capacity of methylene blue).
Embodiment 5:
200 mesh sieves are pulverized and crossed to the Concave-convex clay rod raw ore of attapulgite content 95wt% get the attapulgite powder, get 1g attapulgite powder, add 16mL distilled water, use magnetic stirrer 2h, make solution mix mixed liquor, record pH of mixed value 7 this moment;
Described mixed liquor is transferred in the polytetrafluoroethylene (PTFE) water heating kettle, and reaction temperature is 110 ° of C, and the reaction time is respectively 24h; Naturally cool to room temperature after reaction finishes, centrifugation also washes the back with water and obtains modified attapulgite 60 ° of C oven dry.
Analyzed as can be known by the BET value, gained modified attapulgite BET value is 218, is higher than attapulgite former state BET value (seeing Table 1).
The methylene blue solution of getting initial concentration and be 500mg/L is organic pollution, the solid-to-liquid ratio of modified attapulgite and methylene blue is 1g:2500mL, rotating speed constant temperature vibration absorption 12h with 200r/min under 30 ° of C reaches balance, is that 225mg/g(sees Fig. 2 to the equilibrium adsorption capacity of methylene blue).
Comparative example 1:
200 mesh sieves are pulverized and crossed to the Concave-convex clay rod raw ore of attapulgite content 95wt% get the attapulgite powder, get 1g attapulgite powder, add 16mL distilled water, use magnetic stirrer 2h, make solution mix mixed liquor, record pH of mixed value 7 this moment;
Described mixed liquor is transferred in the polytetrafluoroethylene (PTFE) water heating kettle, and reaction temperature is 200 ° of C, and the reaction time is 12h; Naturally cool to room temperature after reaction finishes, centrifugation also washes the back with water and obtains modified attapulgite 60 ° of C oven dry.
Analyzed as can be known by the BET value, gained modified attapulgite BET value is 206, is lower than the BET value (seeing Table 1) of attapulgite former state.
The methylene blue solution of getting initial concentration and be 500mg/L is organic pollution, the solid-to-liquid ratio of modified attapulgite and methylene blue is 1g:2500mL, with the rotating speed constant temperature vibration absorption 24h of 200r/min, be that 180mg/g(sees Fig. 2 to the equilibrium adsorption capacity of methylene blue under 30 ° of C).
Comparative example 2:
200 mesh sieves are pulverized and crossed to the Concave-convex clay rod raw ore of attapulgite content 95wt% get the attapulgite powder, get 1g attapulgite powder, add 16mL distilled water, use magnetic stirrer 2h, make solution mix mixed liquor, record pH of mixed value 7 this moment;
Described mixed liquor is transferred in the polytetrafluoroethylene (PTFE) water heating kettle, and reaction temperature is 220 ° of C, and the reaction time is 12h; Naturally cool to room temperature after reaction finishes, centrifugation also washes the back with water and obtains modified attapulgite 60 ° of C oven dry.
Analyzed as can be known by the BET value, gained modified attapulgite BET value is 207, is lower than the BET value (seeing Table 1) of attapulgite former state.
The methylene blue solution of getting initial concentration and be 500mg/L is organic pollution, the solid-to-liquid ratio of modified attapulgite and methylene blue is 1g:2500mL, with the rotating speed constant temperature vibration absorption 24h of 200r/min, be that 142mg/g(sees Fig. 2 to the equilibrium adsorption capacity of methylene blue under 30 ° of C).
Comparative example 3:
200 mesh sieves are pulverized and crossed to the Concave-convex clay rod raw ore of attapulgite content 95wt% get the attapulgite powder, get 1g attapulgite powder, add 16mL distilled water, use magnetic stirrer 2h, make solution mix mixed liquor, record pH of mixed value 7 this moment;
Described mixed liquor is transferred in the polytetrafluoroethylene (PTFE) water heating kettle, and reaction temperature is 250 ° of C, and the reaction time is 12h; Naturally cool to room temperature after reaction finishes, centrifugation also washes the back with water and obtains modified attapulgite 60 ° of C oven dry.
Analyzed as can be known by the BET value, gained modified attapulgite BET value is 199, is minimum (the seeing Table 1) of BET value in all attapulgites.
The methylene blue solution of getting initial concentration and be 500mg/L is organic pollution, the solid-to-liquid ratio of modified attapulgite and methylene blue is 1g:2500mL, with the rotating speed constant temperature vibration absorption 24h of 200r/min, be that 147mg/g(sees Fig. 2 to the equilibrium adsorption capacity of methylene blue under 30 ° of C).
Comparative example 4:
200 mesh sieves are pulverized and crossed to the Concave-convex clay rod raw ore of attapulgite content 95wt% get the attapulgite powder, get 1g attapulgite powder, add 16mL distilled water, use magnetic stirrer 2h, make solution mix mixed liquor, record pH of mixed value 7 this moment;
Described mixed liquor is transferred in the polytetrafluoroethylene (PTFE) water heating kettle, and reaction temperature is 100 ℃, and the reaction time is 12h; Naturally cool to room temperature after reaction finishes, centrifugation also washes the back with water and obtains modified attapulgite 60 ° of C oven dry.
Analyzed as can be known by the BET value, the size of BET value is subjected to the influence of reaction temperature, and gained modified attapulgite BET value is 214, is lower than the BET value (seeing Table 1) of attapulgite raw ore.
Comparative analysis: attapulgite mainly contains four kinds of water, surperficial adsorbed water, duct zeolite water, the crystallization water and constitution water.In the hydrothermal treatment consists process, attapulgite progressively removes the hydrone of various different shapes, thereby causes the variation of specific area.Specific area is more big, and the absorption property of attapulgite is more good.At 110 ° of C hydrothermal treatment consists 6-24h, surperficial adsorbed water removes, and the duct zeolite water progressively removes, and abdicating of duct makes specific area increase.200 ° of C-250 ° of C hydrothermal treatment consists, attapulgite begins progressively to remove the crystallization water, and the duct is folding to be dwindled, and causes reducing gradually of inner ratio surface area.In a word, the absorption property of attapulgite and different structure form water removed inner link, be reflected at the variation of BET value, and final decision attapulgite to methylene Blue Adsorbing.
Table 1
Table 1 is the BET value of attapulgite in attapulgite former state and embodiment, the comparative example.Attapulgite concentration as can be seen from Table 1, reaction temperature and reaction time influence the size of BET value; Optimal reaction temperature is 110 ° of C; The best reaction time is 12h.On the whole, ratio is 1:16, and reaction temperature is 110 ° of C, and the reaction time is that the product B ET value of 12h is maximum.
Claims (3)
1. a hydro-thermal method modification improves the method for attapulgite absorption property, it is characterized in that:
200 mesh sieves are pulverized and crossed to the Concave-convex clay rod raw ore of attapulgite content 〉=95wt% get the attapulgite powder; The mass volume ratio of described attapulgite powder and distilled water being pressed 1g:8-32mL mixes, ultrasonic being uniformly dispersed is warming up to 100-120 ° of C, reaction 6-24h, reaction is cooled to room temperature after finishing, and obtains the modified attapulgite stone powder through washing, drying with after pulverizing successively.
2. method according to claim 1 is characterized in that:
The mass volume ratio that described attapulgite powder and distilled water are pressed 1g:16mL mixes.
3. method according to claim 1 and 2 is characterized in that:
Reaction temperature is 110 ° of C, and the reaction time is 12h.
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| CN103736444A (en) * | 2013-12-31 | 2014-04-23 | 常州大学 | Preparation method and application of hydrothermally solidified attapulgite clay filtering material |
| CN103752263A (en) * | 2014-01-15 | 2014-04-30 | 中国科学院兰州化学物理研究所盱眙凹土应用技术研发中心 | Preparation method of nano attapulgite adsorbent |
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| CN103736444A (en) * | 2013-12-31 | 2014-04-23 | 常州大学 | Preparation method and application of hydrothermally solidified attapulgite clay filtering material |
| CN103752263A (en) * | 2014-01-15 | 2014-04-30 | 中国科学院兰州化学物理研究所盱眙凹土应用技术研发中心 | Preparation method of nano attapulgite adsorbent |
| CN104261421B (en) * | 2014-09-23 | 2016-08-17 | 中国科学院兰州化学物理研究所 | Hydro-thermal method prepares the method for rice white attapulgite |
| CN104261421A (en) * | 2014-09-23 | 2015-01-07 | 中国科学院兰州化学物理研究所 | Hydrothermal method for preparing creamy white attapulgite |
| 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 |
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| CN104383873B (en) * | 2014-11-13 | 2016-08-24 | 中国科学院兰州化学物理研究所盱眙凹土应用技术研发中心 | Utilize the method that low-grade attapulgite clay prepares compound adsorbent |
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| CN107694554A (en) * | 2017-09-27 | 2018-02-16 | 绍兴文理学院 | A kind of preparation method of nano-zinc oxide composite photocatalyst |
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