CN102580690B - Nano-aperture granular adsorbent and preparation and application thereof - Google Patents
Nano-aperture granular adsorbent and preparation and application thereof Download PDFInfo
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- CN102580690B CN102580690B CN201210056312.5A CN201210056312A CN102580690B CN 102580690 B CN102580690 B CN 102580690B CN 201210056312 A CN201210056312 A CN 201210056312A CN 102580690 B CN102580690 B CN 102580690B
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- 239000003463 adsorbent Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000000440 bentonite Substances 0.000 claims abstract description 20
- 229910000278 bentonite Inorganic materials 0.000 claims abstract description 20
- SVPXDRXYRYOSEX-UHFFFAOYSA-N bentoquatam Chemical compound O.O=[Si]=O.O=[Al]O[Al]=O SVPXDRXYRYOSEX-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 16
- 230000007935 neutral effect Effects 0.000 claims abstract description 10
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 9
- 239000011324 bead Substances 0.000 claims description 8
- 239000002245 particle Substances 0.000 claims description 7
- 239000002994 raw material Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 4
- 238000001179 sorption measurement Methods 0.000 abstract description 19
- 239000000463 material Substances 0.000 abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 14
- 230000000694 effects Effects 0.000 abstract description 10
- 239000003651 drinking water Substances 0.000 abstract description 9
- 235000020188 drinking water Nutrition 0.000 abstract description 8
- 239000000203 mixture Substances 0.000 abstract description 8
- 229910001385 heavy metal Inorganic materials 0.000 abstract description 7
- 229920001661 Chitosan Polymers 0.000 abstract description 5
- 239000012153 distilled water Substances 0.000 abstract description 5
- 239000004927 clay Substances 0.000 abstract description 2
- 239000003344 environmental pollutant Substances 0.000 abstract description 2
- 231100000719 pollutant Toxicity 0.000 abstract description 2
- 230000002378 acidificating effect Effects 0.000 abstract 1
- 230000007547 defect Effects 0.000 abstract 1
- 238000001035 drying Methods 0.000 abstract 1
- 239000000834 fixative Substances 0.000 abstract 1
- 239000008187 granular material Substances 0.000 abstract 1
- 229920000620 organic polymer Polymers 0.000 abstract 1
- 239000007788 liquid Substances 0.000 description 17
- 238000010521 absorption reaction Methods 0.000 description 11
- 150000001875 compounds Chemical class 0.000 description 6
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 4
- 239000002253 acid Substances 0.000 description 4
- 238000007596 consolidation process Methods 0.000 description 4
- 238000004090 dissolution Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 238000000465 moulding Methods 0.000 description 4
- 238000003795 desorption Methods 0.000 description 3
- 238000009826 distribution Methods 0.000 description 3
- 238000005189 flocculation Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000000746 purification Methods 0.000 description 3
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 2
- 229910021502 aluminium hydroxide Inorganic materials 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
- 230000007812 deficiency Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 230000016615 flocculation Effects 0.000 description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 239000011707 mineral Substances 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004913 activation Effects 0.000 description 1
- 238000001994 activation Methods 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 235000012206 bottled water Nutrition 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000005341 cation exchange Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000011162 core material Substances 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 229910052745 lead Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000007420 reactivation Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
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Abstract
The invention provides a nano-aperture granular adsorbent and a preparation method and application thereof. The method comprises the following steps: (1) weighting bentonite and a chitosan mixture in certain proportion, and uniformly mixing the two; (2) adding the obtained mixture into an acidic dissolved solution, then obtaining a thick object for standby after the mixture is dissolved uniformly; (3) slowly dripping the thick object into a fixative to form according to an actual demand; and (4) rinsing a formed adsorbent to a neutral adsorbent by using distilled water, and drying the neutral adsorbent so as to obtain a finished adsorbent. The nano-aperture granular adsorbent prepared by using the method disclosed by the invention overcomes the defects that powdered bentonite is poor in adsorption effect, and clay granules are uneasy to flocculate and remove and easy to cause second pollution and the like, a preparation process is simple and stable, a granular formed body is good in strength, selected materials are low in cost, and the nano-aperture granular adsorbent can efficiently adsorb pollutants such as trace heavy metals and organic polymers and the like in drinking water, thereby effectively guaranteeing the cleanness and security of the drinking water and realizing the virtuous cycle of environment-economy.
Description
(1) technical field
The present invention relates to nano-aperture granular adsorbent and the preparation and application thereof of micropollutants in a kind of energy efficient adsorption drinking water.
(2) background technology
At present, in the water purification field of drinking water, the absorption method especially research and development of sorbing material obtains the concern of Chinese scholars.And existing sorbing material, as active carbon, is difficult to meet efficient adsorption multiple pollutant, reach energy-saving and emission-reduction, the eucyclic requirement of economy and environment.In recent years, Chinese scholars is constantly found novel absorption material, and attempts material, the reagent of compound other functions in sorbing material, to improve adsorption.According to research (bentonite physical and chemical performance and exploitation thereof) report, New Type of Bentonite water purification agent is take bentonite, aluminium hydroxide as primary raw material, and adds the process low-temperature activations such as auxiliary agent, acid, water to form.Aluminium hydroxide and acid have improved bentonitic flocculation and absorption property to a certain extent, can effectively remove suspension, colourity and turbidity in water.Its deficiency is: (1) Powdered bentonite is easy residual solids particle in use, is difficult for filtering, and causes the secondary pollution of drinking water; (2) not good enough to the adsorption effect of organic matter, heavy metal etc. in water; (3) complicated process of preparation.
(3) summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of manufacture craft simple and stable is provided, immobilization degree is high, environmentally friendly, and low production cost and adsorption range be nano aperture type granular adsorbent and preparation method thereof and application widely.
The technical solution used in the present invention is:
A kind of nano-aperture granular adsorbent, the bentonite take mass ratio as 1: 1～10 and shitosan, as primary raw material, are prepared as follows and obtain:
(1) get bentonite and the shitosan of formula ratio, mix, dissolve with appropriate 0.8%～2.4% (w/w) acetum, obtain mixed liquor; Acetum consumption is suitable just raw material is dissolved as, and obtaining mixed liquor is thick liquid;
(2) step (1) mixed liquor is dropwise splashed in fixer under stirring, make single-size bead; Described fixer is the mixed liquor of 30%～40% (w/w) NaOH and absolute ethyl alcohol volume ratio 1: 5～20;
(3) particle bead rinsing step (2) being made is to neutral, dry, obtains described nano-aperture granular adsorbent.Adsorbent of the present invention is that particle is coccoid, can design according to actual requirement the shape and size size of particle.
The invention still further relates to the preparation method of described nano-aperture granular adsorbent, described method is as follows:
(1) getting mass ratio is 1: 1～10 bentonite and shitosan, mixes, and dissolves with 0.8%～2.4% acetum, obtains mixed liquor; Described acetum consumption is 30～110mL: 3g with the ratio of bentonite and the total consumption of shitosan;
(2) step (1) mixed liquor is dropwise splashed in fixer under stirring, make single-size bead; Described fixer is the mixed liquor of 30%～40% NaOH and absolute ethyl alcohol volume ratio 1: 5～20;
(3) particle bead rinsing step (2) being made is to neutral, dry, obtains described nano-aperture granular adsorbent.
Preferably, described fixer is 40% NaOH and the absolute ethyl alcohol volume ratio mixed liquor of 1: 10.
Concrete, described being dried is: air-dry 12～24 hours of room temperature, or 60 ℃, baking oven is dried 2～4 hours.
The invention still further relates to described nano-aperture granular adsorbent in the application of preparing in device for purifying potable water.Specifically can be used for micro heavy and the absorption of larger molecular organics and the core material of relevant purifier thereof in drinking water.
Nano-aperture granular adsorbent prepared by the inventive method is compared with existing adsorbent: in use procedure, easily remove, can not cause secondary pollution; Preparation technology's simple and stable; Granular adsorbent formed body intensity is good; Selected materials has good physico-chemical property, all has larger specific area.Bentonite have the title of " omnipotent " clay, has stronger cation exchange capacity (CEC) and adsorption capacity, and the hygroscopicity that it is powerful can be adsorbed and is equivalent to the water of 8～20 times of own vols and is expanded to 30 times.As natural mineral resources, it is widely distributed, cheap, though research is started late, has wide practical use in water purification field; Shitosan is as a kind of natural polymers, nontoxic, easily biological-degradable, can not cause secondary pollution and aboundresources, it contains a large amount of hydroxyls and amino, can it be removed from the aqueous solution by hydrogen bond, covalent bond or coordinate bond and organic molecule strong bonded, and have the double action of charge neutrality flocculation and adsorption-flocculation concurrently.The synergy of two kinds of sorbing materials can be removed wider organic compound.
Nano-aperture granular adsorbent prepared by the inventive method is compared with external adsorbent: (1) host material is natural, nontoxic, easily biological-degradable and have stronger absorption property; (2) material therefor has stronger adsorption capacity, is conducive to improve adsorption, and as natural mineral resources, it is very extensive at distribution in China, and financial cost is low; (3) clean, the safety of this adsorbent, can not cause secondary pollution; (4) adsorbent of the present invention does not in use need reactivation, can save a set of Sealing Arrangement and electric energy.
Beneficial effect of the present invention is mainly reflected in: the present invention has overcome existing compound adsorbent complicated process of preparation,, the shortcoming that easily cause secondary pollution not good enough to the adsorption effect of micropollutants in drinking water, a kind of nano-aperture granular adsorbent is provided, its manufacture craft simple and stable, selected sorbing material is widely distributed, heavy metal in its synergy energy efficient adsorption water, phenolic compound, macromolecule organic etc., can realize the benign cycle of environment-economy.
(4) accompanying drawing explanation
Fig. 1 is the outside drawing that embodiment 1 prepares adsorbent.
Fig. 2 is the electron scanning micrograph that embodiment 1 prepares adsorbent.
Fig. 3 is the N that embodiment 1 prepares adsorbent
2absorption/desorption isotherm.
Fig. 4 is the graph of pore diameter distribution of the adsorbent prepared of embodiment 1.
Fig. 5 is the adsorption effect of the ABSORBENTS ABSORPTION metal of different materials ratio.
(5) specific embodiment
Below in conjunction with specific embodiment, the present invention is described further, but protection scope of the present invention is not limited in this:
Embodiment 1:
(1) taking 3g ratio is bentonite and the chitosan compound of 1: 1, mixes; (2) said mixture is added in the acetate dissolution liquid of 1.2% (w/w) and be dissolved into thick liquid; (3) above-mentioned thick liquid is slowly splashed into spheroiding graininess in the alkaline consolidation liquid that 50mL is made up of 40% (w/w) NaOH and absolute ethyl alcohol for 1: 5 by volume; (4) adsorbent of this moulding is extremely neutral with distilled water rinsing, after being dried, obtain nano-aperture granular adsorbent finished product.
Fig. 1 is the finished product effect of the nano-aperture granular adsorbent prepared of embodiment 1.
Fig. 2 is the electron scanning micrograph that embodiment 1 prepares adsorbent, this adsorbent surface degree of roughness high (multiplication factor is 3000 times), and pore volume is larger, is conducive to heavy metal and organic absorption.
Fig. 3 is the N that embodiment 1 prepares adsorbent
2absorption/desorption isotherm, can find out N in figure
2start with polymolecular layer absorption with the absorption of adsorbent surface, in the time that pressure approaches saturated vapor pressure, curve presents the asymptote that is parallel to the longitudinal axis, and adsorption and desorption line slope is larger, by N
2known with adsorption isotherm line computation, adsorbent specific area prepared by the inventive method is 298m
2/ g.The pore-size distribution of this adsorbent as described in Figure 4, has the aperture of known this adsorbent of figure to be distributed between 1～20nm, belongs to typical nano material.
Embodiment 2:
(1) taking 3g ratio is bentonite and the chitosan compound of 1: 3, mixes; (2) said mixture is added in 1.2% acetate dissolution liquid and be dissolved into thick liquid; (3) above-mentioned thick liquid is slowly splashed into spheroiding graininess in the alkaline consolidation liquid that 80mL is made up of 40% NaOH and absolute ethyl alcohol for 1: 10 by volume; (4) adsorbent of this moulding is extremely neutral with distilled water rinsing, after being dried, obtain nano-aperture granular adsorbent finished product.
Embodiment 3:
(1) taking 3g ratio is bentonite and the chitosan compound of 1: 8, mixes; (2) said mixture is added in 1.2% acetate dissolution liquid and be dissolved into thick liquid; (3) above-mentioned thick liquid is slowly splashed into spheroiding graininess in the alkaline consolidation liquid that 100mL is made up of 40% NaOH and absolute ethyl alcohol for 1: 15 by volume; (4) adsorbent of this moulding is extremely neutral with distilled water rinsing, after being dried, obtain nano-aperture granular adsorbent finished product.
Embodiment 4:
(1) taking 3g ratio is bentonite and the chitosan compound of 1: 10, mixes; (2) said mixture is added in 1.2% acetate dissolution liquid and be dissolved into thick liquid; (3) above-mentioned thick liquid is slowly splashed into spheroiding graininess in the alkaline consolidation liquid that 110mL is made up of 40% NaOH and absolute ethyl alcohol for 1: 20 by volume; (4) adsorbent of this moulding is extremely neutral with distilled water rinsing, after being dried, obtain nano-aperture granular adsorbent finished product.
Embodiment 5: different materials ratio adsorbent is to representative heavy metal and organic adsorption effect comparison
Separately get respectively mass ratio and be bentonite and the shitosan raw material of 2: 1,1: 2,1: 4,1: 5,1: 6,1: 7,1: 9, make adsorbent product according to embodiment 1 method, and the adsorbent finished product that embodiment 1～4 is made with the said goods together, carry out respectively representative heavy metal and organic adsorption effect and detect, the results are shown in Figure 5 and table 1.
Table 1: the adsorbent Pyrogentisinic Acid's of different materials ratio adsorption effect
This adsorbent exceedes 90% substantially to the clearance of Pb, Cr, Cu tri-heavy metal species in the aqueous solution as seen from Figure 5, the especially prepared adsorbent of embodiment 1, and its clearance all exceedes 99%.As can be seen from Table 1, the prepared adsorbent of the inventive method is also very obvious to the removal effect of phenol in water, and the prepared adsorbent Pyrogentisinic Acid's of 4 kinds of embodiment removal efficiency is all greater than 50%.
In sum, utilize its performance parameter of the prepared nano-aperture granular adsorbent of the inventive method to be obviously better than adsorbent of the same type, there is cost of manufacture low, advantages of good adsorption effect, adsorption range is wide, the plurality of advantages such as environmental friendliness, can be widely used in micro heavy and organic macromolecule removal in drinking water.
Claims (3)
1. a nano-aperture granular adsorbent, the bentonite take mass ratio as 1:1～10 and shitosan are primary raw material, are prepared as follows and obtain:
(1) get bentonite and the shitosan of formula ratio, mix, dissolve with appropriate 0.8%～2.4% acetum, obtain mixed liquor;
(2) step (1) mixed liquor is dropwise splashed in fixer under stirring, make single-size bead; Described fixer is the mixed liquor of 40% NaOH and absolute ethyl alcohol volume ratio 1:10;
(3) particle bead rinsing step (2) being made is to neutral, dry, obtains described nano-aperture granular adsorbent.
2. a preparation method for nano-aperture granular adsorbent, described method is as follows:
(1) get bentonite and the shitosan that mass ratio is 1:1～10, mix, dissolve with 0.8%～2.4% acetum, obtain mixed liquor; Described acetum consumption is 30～110mL:3g with the ratio of bentonite and the total consumption of shitosan;
(2) step (1) mixed liquor is dropwise splashed in fixer under stirring, make single-size bead; Described fixer is the mixed liquor of 40% NaOH and absolute ethyl alcohol volume ratio 1:10;
(3) particle bead rinsing step (2) being made is to neutral, dry, obtains described nano-aperture granular adsorbent.
3. method as claimed in claim 2, is characterized in that described being dried is: air-dry 12～24 hours of room temperature, or 60 ℃, baking oven is dried 2～4 hours.
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| CN104014312B (en) * | 2014-05-30 | 2016-09-21 | 扬州天辰精细化工有限公司 | A kind of preparation method of chitosan-silicon dioxide composite molding adsorbent |
| CN108246260A (en) * | 2016-12-28 | 2018-07-06 | 海门市源美美术图案设计有限公司 | A kind of bentonite of surface modification and its preparation method and application |
| CN108355621B (en) * | 2018-03-21 | 2022-04-01 | 成都理工大学 | Magnetic porous bentonite chitosan composite microsphere and preparation method thereof |
| CN108745299A (en) * | 2018-05-17 | 2018-11-06 | 菏泽学院 | A kind of preparation method of special appearance adsorbent |
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| CN1204055C (en) * | 2002-10-28 | 2005-06-01 | 张建英 | Water purifying agent and its prepn process |
| CN101298038B (en) * | 2008-03-13 | 2011-03-23 | 西南石油大学 | Gel adsorbing agent for wastewater treatment |
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