CN1593745A - Ferrum carried spherical cellulose adsorbent, preparation and application thereof - Google Patents
Ferrum carried spherical cellulose adsorbent, preparation and application thereof Download PDFInfo
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Abstract
The invention relates to a kind of globe-form cellulose absorbent with iron carrying and its manufacturing and application. The carrying agent of the invention is globe-form cellulose, and the active center is the hydroxide of iron in the specific form, which has the high absorption activity. The manufacturing feature is as follows: dropwise alkali solution tardily into the solution of cellulose bead and molysite; in stirring condition, iron can load the cellulose bead by dispersing and hydrolyzing; after loading repeatedly and frequently, use the alkali solution to stabilize the ferruginous form. The manufacturing method of the absorbent has the advantages of environmental protection, novelty, simplicity and low cost. Moreover, it can remove arsenic, fluorine and other heavy metal with high efficiency and high selectivity, and the absorbent has excellent usage-prospect in nowadays.
Description
Technical field
The present invention relates to a kind of year iron ball shape cellulose adsorbent and preparation and application.
Background technology
Arsenic is one of the most malicious element, occupies to pollute (WHO, 1999) first of the poisonous element blacklist.Drinking water source in recent years, the pollution of particularly drinking arsenic from underwater has caused global concern (AWWA, 2001; Bagla, 1996).Because drink high-arsenic underground water, whole 7,000,000 people's of Bangladesh health be on the hazard (Nickson, 1998; Bearak, 1998).The arsenic contamination problem of China is also very outstanding, Taiwan, Xinjiang and some areas, Inner Mongol underground water arsenic content severe overweight, and some regional content of Inner Mongol is up to 2000ppb (Smedley, 2002; Sun Tianzhi, 1994).The European Union and the U.S. have reformulated the sanitary standard of drinking water arsenic, drop to 10ppb (EPA, 1997 from 50ppb; EC, 1998).The formulation of new standard is had higher requirement to the removal technology and the technology of arsenic in the drinking water.
The common method of removing water body arsenic has oxidation/precipitation method (Stephan, 2001), precipitation-flocculence (Laurie S.Mcneill, 1997; Janet G Hering, 1997; S.Tokunaga, 1999; XiaoGuang Meng, 2000), ion-exchange and absorption method (Altundogan, 2000; Wasay, 1996; Diamadopoulos, 1993; Elizalde-Gonz á lez, 2001), membrane filter method, floatation (Matis, 1997; Zhao Y.C., 1996; Nenov, 1992) and counter-infiltration (Waypa, 1997) etc.
Arsenic is in the great majority with inorganic arsenic in the natural water, and wherein surface water is based on pentavalent arsenic, and trivalent arsenic accounts for suitable proportion in the underground water.Oxidation/precipitation method are to be pentavalent arsenic with illumination or chemical agent pre-oxidation trivalent arsenic, the precipitation flocculation takes place and remove arsenic by the iron ion in the water body, though this method is simple, cheapness is subjected to the restriction of water body iron-holder, only can remove water body part arsenic.Coagulation Method is to add certain molysite or aluminium salt, by its hydrolytic precipitation, arsenic in absorption or the co-precipitation water, the weakness of the method is to produce a large amount of moisture very high mud, dehydration difficulty, waste residue are difficult to handle, and Coagulation Method can only effectively be removed pentavalent arsenic, the trivalent arsenic removal effect is bad, generally needs a pre-oxidation treatment that is translated into pentavalent arsenic.Though membrane technology can efficiently be removed arsenic, cost and operating cost are too high, and produce a large amount of high strong brines.
Absorption method is one of effective ways that arsenic is removed in the drinking water, and the adsorbent of having reported has activated alumina, active carbon, functional resin, metal oxide such as iron oxide, and various natural minerals such as fluorite.During the ion exchange resin treatment arsenic-containing water, follow anion such as sulfate ion to have a strong impact on removal effect.Activated alumina has strict requirement to former water pH, can only could effectively remove arsenic in narrower pH scope, and regeneration back adsorption capacity descends obviously.Remove the arsenic low price with natural minerals, wide material sources, but adsorption capacity is generally very low, and it is not high to remove efficient, and because of it contains other trace elements, may have other health risks (Zouboulis, 1993; Chakravarty, 2002).With the oxide of various metal oxides such as lanthanum, cerium, zirconium, the technology that the oxide of iron such as goethite, magnetic iron ore, amorphous ferric hydroxide etc. are removed arsenic all has report (Tokunaga, 1997; Suzuki, 2000; Appelo, 2002; Jain, 1999), but these oxides are affected and be applied to packed bed as adsorbent mostly owing to the situation of structure and distribution of pores.Arsenic from underwater acid group and arsenous anion ion all have a certain proportion of existence, above-mentioned adsorbent mostly can not effectively be removed the arsenous anion ion, therefore when removing arsenic with them, an essential preoxidation process has increased operation sequence and expense as with chlorine, potassium permanganate, ozone oxidation etc.A patent of Germany is that the granulation of β type FeOOH is obtained granular arsenic-removing adsorption agent, but it is not wear-resisting, and lump easily in the column operation process (Driehaus, 1994).Being written into adsorption sites such as iron, zirconium, cerium at various absorption carriers, improving the selectivity and the capacity of arsenic-adsorbing, is main points (Bonnin, 2000 of absorption arsenic removal technology now; Min, 1998; Muzoz, 2002; Lenoble, 2002).By active carbon, zeolite, ion exchange resin, high polymer and molecular sieve etc. are carried the iron modification, can further improve the arsenic adsorption capacity and remove efficient (Bonnin, 2000; Manning, 2002; Farquhar, 2002; Fendorf, 1997).
Summary of the invention
The purpose of this invention is to provide a kind of environmental protection, porosity is big, hydrophily is strong, the iron content height, and possess excellent mechanical intensity and anti-wear performance carry iron ball shape cellulose adsorbent and preparation and application.
The present invention solves this technical problem the technical scheme that is adopted: the carrier of adsorbent of the present invention is a ball shaped cellulose, and the adsorbent activity center is the hydroxide of iron, and the particle diameter of described adsorbent is at the 20-60 order.
The carrier of described adsorbent is a ball shaped cellulose, and described adsorbent activity center is the hydroxide of iron.
The preparation method of carrying iron ball shape cellulose adsorbent be a slow dropping aqueous slkali in cellulose ball and iron salt solutions, and under stirring condition, molysite is written into the cellulose ball through dispersion, hydrolysis;
Concrete steps comprise:
1) aqueous solution of adding trivalent iron salt in the cellulose ball;
2) under the stirring condition, slowly splash into aqueous slkali, trivalent iron salt is through dispersion, hydrolysis and be written into cellulose balls;
3) after the molysite complete hydrolysis, inclining suspension and residual ferric hydroxide precipitate;
4) repeat above-mentioned year iron process repeatedly, the content of iron increases and increases along with carrying the iron number of times in the cellulose ball;
5) add appropriate bases solution, the iron that is written in the ball is existed with stable iron form.
The preparation method of described year iron ball shape cellulose adsorbent, it is characterized by trivalent iron salt is iron chloride or ferric sulfate or ferric nitrate.
The preparation method of described year iron ball shape cellulose adsorbent, it is characterized by and carrying the iron temperature is 0-100 ℃.
The preparation method of described year iron ball shape cellulose adsorbent, the aqueous slkali that it is characterized by dropping is NaOH or potassium hydroxide or ammoniacal liquor.
The preparation method of described year iron ball shape cellulose adsorbent is characterized by in year iron process and slowly drips aqueous slkali while stirring, and it is 1h-48h that the speed of dripping alkali liquid is controlled at each year iron time.
The preparation method of described year iron ball shape cellulose adsorbent, it is characterized by and carrying the iron process is that continuous several times is carried iron, number of times is 3-50 time.
The preparation method of described year iron ball shape cellulose adsorbent, it is characterized by carry iron after, adding aqueous slkali is NaOH or potassium hydroxide or ammoniacal liquor.
The application process that carries iron ball shape cellulose adsorbent is for carrying arsenic, fluorine and other heavy metal ion in the plain adsorbent removal of the iron fiber water.
The renovation process that carries iron ball shape cellulose adsorbent is with the NaOH regenerated from washing for the renovation process that carries the plain adsorbent of iron fiber, and concentration is 1-4mmol/L.
The invention has the beneficial effects as follows:
Cellulose carrier is different with other carriers, is a kind of natural reproducible material, the carrier good hydrophilic property, and porosity is big, has been widely used as bioactive materials, is used for (Heinze, 2001) such as absorption and amino acid separation, protein and nucleic acid.We utilize gossypin to do carrier, by modification cleverly, are prepared into and carry iron ball shape cellulose adsorbent, can be successfully used to the removal of arsenic in the drinking water.The preparation thinking of carrying iron ball shape cellulose adsorbent is to drip aqueous slkali under cellulose ball and molysite aqueous solution stirring condition, and molysite is written into the cellulose ball through dispersion, hydrolysis, and stablizes through alkali.
Iron ball shape cellulose adsorbent particle diameter was moderate in of the present invention year, and porosity is big, and hydrophily is strong, possesses excellent mechanical intensity and anti-wear performance.With existing relevant document both at home and abroad relatively, the iron-holder of adsorbent is the highest, can be up to 50% (dry weight), and the active height of iron, big to the adsorption capacity of arsenic.Carry iron gossypin adsorbent and in wide pH scope, all showed effect of removing arsenic efficiently, pentavalent arsenic and trivalent arsenic are all had high selectivity, and pH is also higher than pentavalent arsenic to arsenious adsorbance near neutrality, need not pre-oxidation treatment.Anion such as common carbonate, bicarbonate radical, sulfate radical and silicate and cation all do not influence the removal effect of arsenic in the water.Adsorbent has the regeneration effect that the satisfied rate of adsorption is become reconciled.From technology of preparing, preparation of adsorbent method novelty, simple, environmental protection, with low cost have a good application prospect to arsenic, fluorine and other heavy metals of removing in the water etc.
The specific embodiment
Embodiment 1:
Absorbent cotton 16.0g (Henan Jiaozuo City Sanitary Materials Factory) is dipped in the NaOH aqueous solution 2h of 400ml 20% (m/v), and to 75 grams (press ratio is 4: 1) extracted in squeezing, obtains alkali cellulose, and alkali cellulose was sealed under the room temperature aging 2-3 days, adds 8ml CS
2(CS
2Milliliter number=gossypin dry weight (gram)/2), sealing, the 150rpm vibration is 4-8 hour under the room temperature, obtains orange red viscose glue, adds the 100ml 6%NaOH aqueous solution, stirs and can get the uniform viscose of esterification in 3-5 hour.Viscose can not be placed for a long time.In the 500ml there-necked flask, add 200ml pump oil-chlorobenzene decentralized medium (pump oil: chlorobenzene=2: 1), 0.4g potassium oleate, the above-mentioned viscose of 50ml, 200-250rpm stirred 30 minutes, slowly be warming up to 90 ℃ again in 30-60 minute, insulation 2h stops to stir, remove decentralized medium (decentralized medium can be repeatedly used), the cellulose balls ball that hot water wash makes is to white.Collect 20-60 order cellulose ball (this particle size range accounts for more than 90%) with standard screen, the wet preservation in the deionized water.
Embodiment 2:
Get 50ml cellulose ball, add 100ml 5% (m/v) FeCl
36H
2O solution, under the 180rpm stirring condition, the sample rate that divides with 12ml/ slowly splashes into the 100-110ml 0.5mol/LNaOH aqueous solution under the room temperature.When pH rose to 3.5-4.0, the part iron precipitation that is not written into was separated out, and inclining suspension and residual iron hydroxide flocculent deposit, washes ball with water 5 times.Repeat above-mentioned year iron process 12 times, what obtain every milliliter of iron content and be 200 ± 20mg carries iron ball shape cellulose adsorbent, and mass content is 42% (dry weight).
Embodiment 3:
Get 50ml cellulose ball, add 100ml 10% (m/v) FeCl
36H
2O solution under the 180rpm stirring condition, slowly splashes into the 100-110ml 1.0mol/LNaOH aqueous solution with the 10ml/ branch under the room temperature.When pH rose to 3.5-4.0, inclining suspension and residual ferric hydroxide precipitate, washes ball with water 5 times.Repeat above-mentioned year iron process 7 times, what obtain every milliliter of iron content and be 200 ± 20mg carries iron ball shape cellulose adsorbent, and mass content is 42%.
Embodiment 4:
Get the plain adsorbent bead of year iron fiber 1ml that iron-holder is respectively 34mg/ml (No.1), 84mg/ml (No.2), 134mg/ml (No.3), 176mg/ml (No.4), 216mg/ml (No.5), the arsenic solution 50ml (pH 7.0) that adds variable concentrations respectively, 120rpm vibration absorption under the room temperature, regulate pH every a few hours with several rare HCl or NaOH, make equilibrium liquid pH stabilize to 7.0 ± 0.1, hypsokinesis in 15 hours goes out supernatant, washing, bead is through digestion, gradient dilution is measured the amount of carrying the plain adsorbent ball of iron fiber arsenic-adsorbing with atomic fluorescence method.Adsorption isotherm Langmuir equation simulation, coefficient R
2All more than 0.9.Table 1 is the saturated extent of adsorption of year iron ball shape cellulose adsorbent of different iron contents to As (III) and As (V).
Year iron ball shape cellulose adsorbent of the different iron contents of table 1 is to the saturated extent of adsorption of As (III) and As (V)
Density Fe content As (V) saturated extent of adsorption As (III) saturated extent of adsorption
mg/mL mg/mL mg/g mg/mL mg/g mg/mL mg/g
No.1 0.129 33.5 260 1.56 12.1 9.43 73.1
No.2 0.226 83.6 370 5.82 25.8 16.8 74.3
No.3 0.300 134 447 7.43 24.8 20.3 67.7
No.4 0.400 176 440 10.5 26.3 27.3 68.3
No.5 0.471 220 468 15.6 33.2 46.8 99.6
Embodiment 5:
Getting the 12ml iron content and be the plain ball of iron fiber that carries of 220mg/ml, to be filled in internal diameter be that 10mm, post are high for (filling the 1cm mineral wool at the bottom of the post) in the glass column of 400mm.Adopting Ji County, Tianjin underground water is former water background, adds standard trivalent arsenic solution, and making trivalent arsenic concentration is 500 μ g/L.Water inlet pH8.2, flow velocity 2.1m/hr, empty bench grafting touches time 4.2min.Carry iron ball shape cellulose adsorbent the post of As (III) is tested elution curve as shown in Figure 1, press the drinking water arsenic sanitary standard 10 μ g/L that WHO recommends, it is 2000 times of empty bed volumes that adsorbent is removed arsenious penetration volume, and the capacity of penetrating is 2.1mg/g; As pressing existing Chinese drinking water arsenic sanitary standard 50 μ g/L, adsorbent is removed arsenious penetration volume then up to 4000 times of empty bed volumes, and the capacity of penetrating is 4.0mg/g.The saturated adsorption capacity of adsorbent removal As (III) is 12.9mg/g under this operating parameter.By measuring the concentration of Inlet and outlet water zwitterion, the result shows that adsorbent does not change common anion and cationic concentration in the former water, the iron form stable that adsorbent is written into, and not stripping of iron in the post experiment, water outlet pH is 8.2, all meets water standard.
Embodiment 6:
The plain ball of iron fiber that carries of getting the 12ml iron content and be 220mg/ml is filled in internal diameter 10mm, (fills the 1cm mineral wool at the bottom of the post) in the glass column of the high 400mm of post.Adopting Ji County, Tianjin underground water is former water background, adds standard pentavalent arsenic solution, and making pentavalent arsenic concentration is 500 μ g/L.Water inlet pH7.0, flow velocity 1.5m/hr, empty bench grafting touches time 5.9min.Carry iron ball shape cellulose adsorbent the post of As (V) is tested elution curve as shown in Figure 2.According to the drinking water arsenic sanitary standard 10 μ g/L that WHO recommends, the penetration volume that adsorbent is removed pentavalent arsenic is 5000 times of empty bed volumes, and the capacity of penetrating is 5.2mg/g; As pressing existing Chinese drinking water arsenic sanitary standard 50 μ g/L, adsorbent is removed the penetration volume of pentavalent arsenic then up to 8500 times of empty bed volumes, and the capacity of penetrating is 8.6mg/g.By measuring the concentration of Inlet and outlet water zwitterion, the result shows that adsorbent does not change common anion and cationic concentration in the former water, the iron form stable that adsorbent is written into, and not stripping of iron in the post experiment, water outlet pH is about 7.5, all meets water standard.
Embodiment 7:
Measure 1ml and carry the plain ball of iron fiber (iron content is a 180mg Fe/ml ball) in the 250ml conical flask, adding 50ml concentration is respectively pentavalent arsenic and the trivalent arsenic solution of 0.5mmol/L and 1mmol/L, 120rpm vibration absorption is 24 hours under the room temperature, equilibrium system pH7.The supernatant that inclines adds the NaOH solution of 50ml 1.5mol/L, 120rpm vibration desorb 24 hours down under the room temperature.The NaOH eluent that inclines, it is closely neutral to pH to wash ball with deionized water.Repeat twice of above-mentioned absorption-desorption process.Measure the clearance of each time of adsorbent arsenic-adsorbing.The result is as shown in table 2:
Table 2: carry iron ball shape cellulose adsorbent the static regeneration of arsenic is removed
The trivalent arsenic pentavalent arsenic
The clearance first time (%) 99.6 99.1
The clearance second time (%) 99.1 98.4
Clearance (%) 99.4 99.8 for the third time
Claims (10)
1. one kind carries iron ball shape cellulose adsorbent, and it is characterized in that: the carrier of described adsorbent is a ball shaped cellulose, and described adsorbent activity center is the hydroxide of iron.
2. preparation method of carrying iron ball shape cellulose adsorbent is characterized in that: slow dropping aqueous slkali in cellulose ball and iron salt solutions, and under stirring condition, molysite is written into the cellulose ball through dispersion, hydrolysis;
Concrete steps comprise:
1) aqueous solution of adding trivalent iron salt in the cellulose ball;
2) under the stirring condition, slowly splash into aqueous slkali, trivalent iron salt is through dispersion, hydrolysis and be written into cellulose balls;
3) after the molysite complete hydrolysis, inclining suspension and residual ferric hydroxide precipitate;
4) repeat above-mentioned year iron process repeatedly, the content of iron increases and increases along with carrying the iron number of times in the cellulose ball;
5) add appropriate bases solution, the iron that is written in the ball is existed with stable iron form.
3. the preparation method of according to claim 2 year iron ball shape cellulose adsorbent is characterized in that: trivalent iron salt is iron chloride or ferric sulfate or ferric nitrate.
4. the preparation method of according to claim 2 year iron ball shape cellulose adsorbent is characterized in that: carrying the iron temperature is 0-100 ℃.
5. the preparation method of according to claim 2 year iron ball shape cellulose adsorbent is characterized in that: the aqueous slkali of dropping is NaOH or potassium hydroxide or ammoniacal liquor.
6. the preparation method of according to claim 2 year iron ball shape cellulose adsorbent is characterized in that: carry in the iron process and slowly drip aqueous slkali while stirring, it is 1h-48h that the speed of dripping alkali liquid is controlled at each year iron time.
7. the preparation method of according to claim 2 year iron ball shape cellulose adsorbent is characterized in that: carrying the iron process is that continuous several times is carried iron, and number of times is 3-50 time.
8. the preparation method of according to claim 2 year iron ball shape cellulose adsorbent is characterized in that: after carrying iron, adding aqueous slkali is NaOH or potassium hydroxide or ammoniacal liquor.
9. an application process that carries iron ball shape cellulose adsorbent is characterized in that: carry arsenic, fluorine and other heavy metal ion in the plain adsorbent removal of the iron fiber water.
10. renovation process that carries iron ball shape cellulose adsorbent, it is characterized in that: the renovation process that carries the plain adsorbent of iron fiber is with the NaOH regenerated from washing, and concentration is 1-4mmol/L.
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