CN103331146B - Modified bean pulp adsorbent as well as preparation method and application thereof - Google Patents
Modified bean pulp adsorbent as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a modified bean pulp adsorbent as well as a preparation method and the application thereof, belonging to the technical field of adsorbents. The adsorbent is bean pulp adsorbent modified by sodium hydroxide; the preparation method of the modified bean pulp adsorbent comprises the following steps of: immersing bean pulp powder with particle size of 300-1,200 microns into a sodium hydroxide solution, standing still or stirring for 12-24 hours, filtering and separating, washing filter residues by distilled water until the pH is neutral, and drying to obtain the modified bean pulp adsorbent. The bean pulp adsorbent modified by the sodium hydroxide is used for absorbing and removing heavy metal copper (Cu2+) in the solution. The modified bean pulp adsorbent as well as the preparation method and the application thereof are simple to operate, low in cost and free from secondary pollution.
Description
Technical field
The invention belongs to technical field of absorbent, relate to a kind of method utilizing adsorbent to remove heavy metal in waste water copper, particularly relate to a kind of method utilizing modification bean pulp adsorbent to remove heavy metal in waste water copper.
Background technology
Copper and compound thereof are widely used in the industries such as plating, five metals processing, mining, petrochemical industry and chemical, mainly through the discharge entered environment of waste water, can not be degraded in the environment, easy generation enrichment, not only causes water pollution also can the healthy and hydrobiological existence of harm humans.It is generally acknowledged that the toxicity of copper itself is very little, but too much copper enters in human body intoxicating phenomenons such as can occurring Nausea and vomiting, Upper abdominal pain, Acute hemolytic crisis and renal tubule distortion, and the toxicity ratio copper of mantoquita is also large, the mantoquita of 10g even can be lethal.The administering method of current Cu in waste water mainly contains chemical precipitation method, electrolysis, ion-exchange, membrane separating method and absorption method etc.Wherein, new polluter can not be produced because absorption method has, there is no obviously advantage and the attention such as secondary pollution.At present, adsorbent at most is the most widely used to be active carbon, but because process for preparing active carbon is complicated, production cost is high, regeneration expense is large and limit the application of its further genralrlization.Therefore be necessary very much to develop novel absorption material that is cheap, efficient, that suit measures to local conditions.China is as the first in the world large agricultural country, and every annual meeting produces a large amount of agricultural wastes, if can not get appropriate disposal, will cause serious secondary pollution to environment.Agricultural wastes have the features such as easy acquisition, renewable, low cost, just can be prepared into efficient adsorbent, be therefore considered to a kind of sorbing material with development potentiality through simple process.
Soya-bean oil is the edible oil that output is maximum in the world, and is also huge as the output of the soyabean expeller of byproduct.On the Chinese side, in 2012 to 2013 years, soya bean enters squeezing amount and is expected to be 6,100 ten thousand tons, and soyabean expeller output is expected to be about 4,800 ten thousand tons.In fact, as a kind of easy acquisition, agricultural wastes that cost is low, soyabean expeller itself has the functional group of more bonding heavy metal ion, and as carboxyl, hydroxyl, amido etc., this becomes a kind of sorbing material having very much development potentiality.Utilize soyabean expeller to prepare sorbent treatment heavy metal in waste water copper, the first theory meeting recycling economy, opens the new way of soyabean expeller resource, and abundance, cheap; Second solves problem of environmental pollution, makes to be purified by heavy metal cuprum polluted waste water, environmentally friendly and do not cause secondary pollution.Under the prerequisite of protection of the environment, reach the effect of turn waste into wealth, control with useless (discarded object) useless (heavy metal wastewater thereby), achieve many things at one stroke.
Summary of the invention
The object of patent of the present invention is to provide the application of a kind of modification bean pulp adsorbent of efficient, low cost, preparation method and Adsorption of Heavy Metal Ions copper.
To achieve these goals, modification bean pulp adsorbent proposed by the invention is the bean pulp adsorbent of NaOH modification, and its preparation method, comprises the following steps:
Get dry soyabean expeller broken, sieve, obtain particle diameter 300 ~ 1200 μm of soyabean expeller powder; This soyabean expeller powder is immersed in sodium hydroxide solution, static or stir 12 ~ 24 hours, isolated by filtration, filter residue with distilled water cleaning to pH in neutral, dry, namely obtain modification bean pulp adsorbent;
The concentration preferably 0.05 ~ 0.25mol/L of above-mentioned sodium hydroxide solution, the consumption of soyabean expeller powder and sodium hydroxide solution is preferably soyabean expeller powder weight (g): sodium hydroxide solution volume (mL) is: 1:10 ~ 1:50, the temperature of modification preferably 20 ~ 50 DEG C.
Modification bean pulp adsorbent of the present invention is used for heavy metal copper (Cu in solution
2+) Adsorption.
Above-mentioned modification bean pulp adsorbent is used for heavy metal copper (Cu in solution
2+) Adsorption optimum condition be: by copper ions (Cu
2+) solution solution regulate pH be that 2 ~ 8(is preferably 5), add modification bean pulp adsorbent, make modification bean pulp adsorbent concentration be 2 ~ 12g/L, adsorb after 24 ~ 48 hours, isolated by filtration, filtrate is adjusted to neutrality, discharge.
The invention has the beneficial effects as follows: adopt modified adsorbent of the present invention for cupric (Cu
2+) solution of ion or wastewater treatment, compared with chemical precipitation method, electrolysis, ion-exchange, membrane separating method etc., simple to operate, cost is low, can not produce secondary pollution.Modification bean pulp adsorbent of the present invention, not only to cupric (Cu
2+) solution that ion concentration is high has good absorption, namely has very high suction-operated to 100 ~ 1000mg/L, and adsorption capacity large (20 DEG C, maximum mono layer adsorption amount Q
0112.36mg/g), to copper (Cu
2+) removal effect significantly (the highest clearance of copper can reach 95.68%, and minimum clearance is also more than 92.65%), described adsorbent is easy to obtain, and is easy to preparation, environmentally friendly, not only makes by heavy metal copper (Cu
2+) waste water that pollutes is purified, and provide new approach for the utilization of soyabean expeller, achieve the recycling of soyabean expeller.
Accompanying drawing explanation
Fig. 1 is that bean pulp adsorbent and modification bean pulp adsorbent are to copper (Cu
2+) clearance compare.
Fig. 2 is that different initial pH is to bean pulp adsorbent and modification bean pulp adsorbent absorbing copper (Cu
2+) impact of effect.
Fig. 3 is copper (Cu
2+) relation curve of adsorption effect and modification bean pulp adsorbent consumption of the present invention.
Fig. 4 is copper (Cu
2+) adsorption effect and copper (Cu
2+) relation curve of initial mass concentration.
Fig. 5 is modification bean pulp adsorbent absorbing copper (Cu
2+) Langmuir adsorption isotherm.
Fig. 6 is modification bean pulp adsorbent absorbing copper (Cu
2+) Freundlich adsorption isotherm.
Fig. 7 is that modification bean pulp adsorbent is at absorbing copper (Cu
2+) before and after infrared spectrogram.
Fig. 8 is that modification bean pulp adsorbent is at absorbing copper (Cu
2+) before and after energy spectrum analysis figure.
Detailed description of the invention
Further illustrate the present invention below in conjunction with specific embodiment, but the present invention is not restricted to embodiment.
Embodiment 1
Get the dry soyabean expeller of certain mass, broken with pulverizer, filter out the soyabean expeller powder of 300 ~ 1200 μm of particle diameters.By this soyabean expeller powder and sodium hydroxide solution according to soyabean expeller powder weight (g): the ratio that sodium hydroxide solution volume (mL) is 1:12.5 is soaked in conical flask, wherein the concentration of sodium hydroxide solution is 0.15mol/L, (120 revs/min) are vibrated after 12 ~ 24 hours in 20 DEG C of water bath with thermostatic control shaking tables, isolated by filtration, filter residue distilled water cleans to pH in neutral, dry (drying or freeze drying), namely obtains modification bean pulp adsorbent.
Comparative example 1
Get the dry soyabean expeller of certain mass, broken with pulverizer, filter out the soyabean expeller of 300 ~ 1200 μm of particle diameters, namely obtain bean pulp adsorbent.
Absorption test case 1
The adsorbent 0.10g that respectively prepared by Example 1 and comparative example 1 adds the 500mg/L copper (Cu that 25mL, pH are 5.0 respectively
2+) in solution, at 20 DEG C, vibrate (150 revs/min) in water bath with thermostatic control shaking table after 24 hours, isolated by filtration, measures residual copper (Cu in filtrate
2+) concentration.
Copper (Cu
2+) clearance as shown in Figure 1.The test result of Fig. 1 shows, the copper (Cu of bean pulp adsorbent
2+) clearance is 49.72%, the copper (Cu of modification bean pulp adsorbent
2+) clearance is 92.65%.Compared with bean pulp adsorbent, modification bean pulp adsorbent of the present invention considerably improves copper (Cu
2+) clearance (improve 42.93%).
Absorption test case 2
The adsorbent 0.10g that respectively prepared by Example 1 and comparative example 1 adds the copper (Cu that solution ph is 1.0,2.0,3.0,4.0,5.0,6.0,7.0,8.0,25mL500mg/L respectively
2+) in solution, at 20 DEG C, vibrate (150 revs/min) in water bath with thermostatic control shaking table after 24 hours, isolated by filtration, measures residual copper (Cu in filtrate
2+) concentration.
According to following formulae discovery adsorption capacity:
Wherein: q
efor adsorption capacity, mg/g; C
0for copper (Cu
2+) initial concentration, C
efor copper (Cu during adsorption equilibrium
2+) concentration, mg/L; V is liquor capacity, mL; M is adsorbent mass, g.
Different initial pH is to bean pulp adsorbent and modification bean pulp adsorbent absorbing copper (Cu
2+) impact as shown in Figure 2.As seen from Figure 2, pH is to bean pulp adsorbent and modification bean pulp adsorbent absorbing copper (Cu
2+) impact very large.Soyabean expeller is before modified afterwards to copper (Cu
2+) adsorption effect substantially identical with pH variation tendency: when pH is between 2 ~ 5, adsorption capacity q
eraise along with the increase of pH; Maximum is reached when pH is 5; Reduce along with the increase of pH afterwards.Modification bean pulp adsorbent is at adsorption capacity q corresponding to each pH
eall far away higher than bean pulp adsorbent, show that soyabean expeller adsorption capacity after modification improves greatly.Copper (Cu
2+) pH of solution itself is between 5 ~ 6, and it is best to be adsorbed on effect when pH is 5.0, therefore in adsorption process, only need add a small amount of acid for adjusting pH can obtain good adsorption effect.After pH>6, copper existence form in the solution based on sediment, therefore, non-comparative analysis pH value of solution 8 ~ 14 situation.
Embodiment 2
Get the dry soyabean expeller of certain mass, broken with pulverizer, filter out the soyabean expeller powder of 300 ~ 1200 μm of particle diameters.By this soyabean expeller powder and sodium hydroxide solution according to soyabean expeller powder weight (g): the ratio that sodium hydroxide solution volume (mL) is 1:25 is soaked in conical flask, wherein the concentration of sodium hydroxide solution is 0.10mol/L, (120 revs/min) are vibrated after 12 ~ 24 hours in 20 DEG C of water bath with thermostatic control shaking tables, isolated by filtration, filter residue distilled water cleans to pH in neutral, dry (drying or freeze drying), namely obtains modification bean pulp adsorbent.
Get modification bean pulp adsorbent 0.05,0.10,0.15,0.20,0.25,0.30g respectively and add that 25mL, pH are 5.0,1000mg/L copper (Cu respectively
2+) in solution, at 20 DEG C, vibrate (150 revs/min) in water bath with thermostatic control shaking table after 24 hours, isolated by filtration, measures residual copper (Cu in filtrate
2+) concentration.
Copper (Cu
2+) adsorption effect and modification bean pulp adsorbent consumption of the present invention relation curve as shown in Figure 3.As seen from Figure 3, along with the rising of modification bean pulp adsorbent consumption, copper (Cu
2+) adsorption capacity q
econtinuous decline, and clearance constantly raises.Modification bean pulp adsorbent mass concentration is 6g/L(and consumption is 0.15g) time, both ensure that adsorbent amount was less, in turn ensure that relatively high copper (Cu
2+) clearance.
Embodiment 3
Get the dry soyabean expeller of certain mass, broken with pulverizer, filter out the soyabean expeller powder of 300 ~ 1200 μm of particle diameters.By this soyabean expeller powder and sodium hydroxide solution according to soyabean expeller powder weight (g): the ratio that sodium hydroxide solution volume (mL) is 1:50 is soaked in conical flask, the wherein concentration 0.05mol/L of sodium hydroxide solution, (120 revs/min) are vibrated after 12 ~ 24 hours in 20 DEG C of water bath with thermostatic control shaking tables, isolated by filtration, filter residue distilled water cleans to pH in neutral, dry (drying or freeze drying), namely obtains modification bean pulp adsorbent.
Get modification bean pulp adsorbent 0.15g and add that 25mL, pH are 5.0, copper (Cu respectively
2+) concentration is respectively 100,200,300,400,500mg/L copper (Cu
2+) in solution, at 20 DEG C, vibrate (150 revs/min) in water bath with thermostatic control shaking table after 24 hours, isolated by filtration, measures residual copper (Cu in filtrate
2+) concentration.
Copper (Cu
2+) adsorption effect and copper (Cu
2+) initial mass concentration relation curve as shown in Figure 4.Under the driving of mass concentration gradient, along with copper (Cu
2+) initial mass concentration is increased to 500mg/L by 100mg/L, adsorption capacity q
erise to 78.12mg/g by 16.31mg/g, and clearance only drops to 92.65% by 95.68%, this shows that modification bean pulp adsorbent of the present invention can at wider copper (Cu
2+) there is good adsorption effect within the scope of mass concentration, and heavy metal removing rate does not significantly change, and still keeps higher clearance.
Embodiment 4
Get the dry soyabean expeller of certain mass, broken with pulverizer, filter out the soyabean expeller powder of 300 ~ 1200 μm of particle diameters.By this soyabean expeller powder and sodium hydroxide solution according to soyabean expeller powder weight (g): the ratio that sodium hydroxide solution volume (mL) is 1:10 is soaked in conical flask, wherein the concentration of sodium hydroxide solution is 0.25mol/L, (120 revs/min) are vibrated after 12 ~ 24 hours in 20 DEG C of water bath with thermostatic control shaking tables, isolated by filtration, filter residue distilled water cleans to pH in neutral, dry (drying or freeze drying), namely obtains modification bean pulp adsorbent.
Get modification bean pulp adsorbent 0.15g and join that 3 groups of 25mL, pH are 5.0,500mg/L copper (Cu respectively
2+) in solution, respectively at 20 DEG C, 35 DEG C, vibrate (150 revs/min) at 50 DEG C in water bath with thermostatic control shaking table after 24 hours, isolated by filtration, measures residual copper (Cu in filtrate
2+) concentration.
Absorption result Langmuir and the matching of Freundlich adsorption isotherm, as shown in Figure 5,6, fitting result is as shown in table 1 for the adsorption isotherm under different temperatures.
As can be seen from Fig. 5,6 and table 1, Langmuir and Freundlich model all can describe modification bean pulp adsorbent to copper (Cu
2+) adsorption isotherm experiment data, but from fitting coefficient, Langmuir model can describe modification bean pulp adsorbent better to copper (Cu
2+) absorption behavior.As can be seen from Table 1, Q
0increase along with the increase of temperature, and the value of parameter b also increases along with temperature and increases, this shows modification bean pulp adsorbent under the high temperature conditions than under cryogenic to copper (Cu
2+) compatibility higher.
When 20 DEG C, the modification bean pulp adsorbent absorbing copper (Cu calculated with Langmuir thermoisopleth
2+) maximum mono layer adsorption amount Q
0112.36mg/g.Different adsorbent is to copper (Cu
2+) adsorption capacity q
emore as shown in table 2, result shows: modification bean pulp adsorbent of the present invention is to copper (Cu
2+) adsorption capacity q
eenough large, the process of copper-containing wastewater can be widely used in.
Table 1 adsorption isotherm parameter
The different adsorbent of table 2 is to copper (Cu
2+) adsorption capacity q
erelatively
| Adsorbent | Maximum mono layer adsorption amount Q 0(mg/g) |
| Rubber tree wood chip active carbon | 5.73 |
| Activity of activated sludge charcoal | 30.70 |
| Hazelnut shell active carbon | 48.64 |
| Sunflower dead leaf | 89.37 |
| Modification soyabean expeller (the present invention) | 112.36 |
Modification bean pulp adsorbent absorbing copper (Cu
2+) thermodynamics show, modification soyabean expeller is at absorbing copper (Cu at 20 DEG C, 35 DEG C and 50 DEG C
2+) Gibbs free energy (Δ G
o) Fen other Wei – 6.60kJ/mol, – 7.81kJ/mol with – 9.15kJ/mol, be negative value, show modification bean pulp adsorbent absorbing copper (Cu
2+) process all can spontaneously occur under three experimental temperatures.Temperature rises to 35 DEG C, 50 DEG C from 20 DEG C, Gibbs free energy (Δ G
o) Cong – 6.60kJ/mol Jiang Zhi – 7.81kJ/mol, – 9.15kJ/mol thereupon, illustrate that high temperature promotes the generation of adsorption reaction.Enthalpy change (Δ H
o) numerical value be 18.29kJ/mol.Entropy Changes (Δ S
o) numerical value be 84.87J/molK, both be on the occasion of, modification bean pulp adsorbent absorbing copper (Cu is described
2+) be the endothermic reaction, and the resistance of solid liquid interface increases to some extent.The above results shows, technological process of the present invention to operating condition and equipment requirement low, be the method for treating copper-containing waste water of a kind of economy, economize energy, be suitable for propagation and employment.
Embodiment 5
Get the dry soyabean expeller of certain mass, broken with pulverizer, filter out the soyabean expeller powder of 300 ~ 1200 μm of particle diameters.By this soyabean expeller powder and sodium hydroxide solution according to soyabean expeller powder weight (g): the ratio that sodium hydroxide solution volume (mL) is 1:12.5 is soaked in conical flask, wherein the concentration of sodium hydroxide solution is 0.15mol/L, (120 revs/min) are vibrated after 12 ~ 24 hours in 20 DEG C of water bath with thermostatic control shaking tables, isolated by filtration, filter residue distilled water cleans to pH in neutral, dry (drying or freeze drying), namely obtains modification bean pulp adsorbent.
Get modification bean pulp adsorbent 0.15g and add 25mL, pH=5.0,500mg/L copper (Cu
2+) in solution, vibrate (150 revs/min) at 25 DEG C in water bath with thermostatic control shaking table after 24 hours, isolated by filtration, will adsorb copper (Cu
2+) the freeze drying of modification bean pulp adsorbent.
Modification bean pulp adsorbent before and after adsorbing in the present embodiment is characterized.
Infrared spectrum analysis
In the present embodiment, modification bean pulp adsorbent is at absorbing copper (Cu
2+) before and after infrared spectrogram as shown in Figure 7, can find out that modification bean pulp adsorbent is at absorbing copper (Cu
2+) before and after spectrogram have obvious similitude, illustrate this sorbent structure stablize.At 3435cm
-1the absworption peak at place represents the overlap of the stretching vibration of O – H and N – H, at 2924cm
-1place is CH
2antisymmetric vibration, at 1637cm
-1place is for C – O in protein is in conjunction with C – N(I type amido) stretching vibration, 1427cm
-1the absworption peak at place is the combination of the deformation vibration of O – H in the symmetrical stretching vibration of C=O in carboxylic acid and alcohol, l085cm
-1the absworption peak at place can represent the flexural vibrations of polysaccharide C – O, 876cm
-1place can represent the symmetrical stretching vibration of Si – O in silicate.The above results shows, modification bean pulp adsorbent surface is containing main functional group such as carboxyl, hydroxyl, amido and silicate groups.At modification bean pulp adsorbent absorbing copper (Cu
2+) after, 3435cm
-1, 2924cm
-1, 1637cm
-1, 1427cm
-1, l085cm
-1, 876cm
-1the absworption peak at place all reduces, and shows that carboxyl, hydroxyl, amido and silicate group take part in copper (Cu jointly
2+) absorption.
Energy spectrum analysis
In the present embodiment, modification bean pulp adsorbent is at absorbing copper (Cu
2+) before and after energy spectrum analysis figure as shown in Figure 8, a figure be adsorb before, b figure be adsorb after.A figure shows modification bean pulp adsorbent of the present invention itself not containing copper, and has the power spectrum peak of 3 coppers in b figure, shows modification bean pulp adsorbent absorbing copper (Cu
2+) process in have a large amount of copper (Cu
2+) be attached to adsorbent surface.EDAX results shows, modification bean pulp adsorbent achieves really to copper (Cu
2+) absorption.
Above-described embodiment shows, the preparation of modification bean pulp adsorbent is simple, to copper (Cu
2+) adsorption capacity large, adsorption operations condition is easy to realize, and can be widely used in the process of copper-containing wastewater.
Claims (1)
1. modification bean pulp adsorbent is used for copper ion Cu in solution
2+the method of Adsorption, it is characterized in that, comprise the following steps:
(1) dry soyabean expeller is got broken, sieve, obtain particle diameter 300 ~ 1200 μm of soyabean expeller powder, this soyabean expeller powder is immersed in sodium hydroxide solution, static or stir 12 ~ 24 hours, isolated by filtration, filter residue with distilled water cleaning to pH in neutral, drying, obtains the bean pulp adsorbent of NaOH modification; Wherein, the concentration of described sodium hydroxide solution is 0.05 ~ 0.25mol/L, and the consumption of soyabean expeller powder and sodium hydroxide solution is: soyabean expeller powder weight g: sodium hydroxide solution volume mL is 1:10 ~ 1:50; The temperature of described modification is 20 ~ 50 DEG C;
(2) by copper ions Cu
2+the solution of solution regulates pH to be 5, and add modification bean pulp adsorbent, make modification bean pulp adsorbent concentration be 2 ~ 12g/L, adsorb after 24 ~ 48 hours, isolated by filtration, filtrate is adjusted to neutrality, discharge; Described copper ion Cu
2+in solution, the concentration of copper is 100 ~ 1000mg/L.
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| CN109607895B (en) * | 2018-11-30 | 2021-10-08 | 河北彩客化学股份有限公司 | Method for treating aniline-containing chemical wastewater |
| CN110711562B (en) * | 2019-10-24 | 2022-04-29 | 北京石油化工学院 | Preparation method of nano adsorbent using soybean extract as template |
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