CN100566817C - A kind of absorption Biosorption of Heavy Metals agent and preparation method thereof - Google Patents
A kind of absorption Biosorption of Heavy Metals agent and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of absorption Biosorption of Heavy Metals agent of adopting sodium alginate and gelatin embedding sea-tangle powder and preparation method thereof, described biological adsorption agent includes the sea-tangle powder of 80～95 weight portions, the sodium alginate of 2～10 weight portions, the gelatin of 2～8 weight portions and the impurity of surplus, this impurity is calcium alginate, and the particle diameter of described biological adsorption agent is 1.5～3mm.This method is carried out the agent of embedding acquisition absorption Biosorption of Heavy Metals by fresh sea-tangle being carried out vacuum drying, air-flow pulverizing back and sodium alginate and gelatin glue.Biological adsorption agent of the present invention can be handled contain nickel, cobalt, zinc, cadmium, copper and the plumbous heavy metal wastewater thereby of concentration≤100mg/L, and adsorption rate reaches 50～99%.
Description
Technical field
The present invention relates to a kind of method that adopts sodium alginate and gelatin embedding sea-tangle powder to prepare Biosorbent for heavy metals.This biological adsorption agent is biological sorbing material with sea-tangle, and sodium alginate and gelatin are fixation support, is suitable for handling low concentration (≤100mg/L) the waste water that contains heavy metals such as nickel, cobalt, zinc, cadmium, copper and lead.
Background technology
Along with rapid economy development; people also more and more pay attention to environment; how eliminating the harm of heavy metal and reclaiming precious metal in the waste water effectively is face in the current environmental protection work one very distinct issues; the processing method of traditional heavy metal mainly contains chemical precipitation method; electrolysis; ion-exchange; membrane processing method and mixed processing method etc. thereof; but these methods handle low concentration (≤100mg/L) have complex process during heavy metal wastewater thereby; complex operation; the operating cost height; produce defectives such as secondary pollution, press for a kind of technology of simple and effective processing heavy metal wastewater thereby.
Biological adsorption technology becomes a big research focus of field of environment engineering owing to advantages such as the raw material source are abundant, and cost is low, and adsorption plant is simple, and is easy to operate.
In numerous heavy metal biological sorbing materials, it is best that algae is proved to be adsorption effect, especially the brown alga in the middle of the algae, its absorption property and the ion exchange resin that some are synthetic compare favourably, and, can relatively easily reclaim precious metal so that adsorbent reuses also, and desorption effect is relatively good with the heavy metal ion that acid or salt desorb are adsorbed, desorb can not have a strong impact on the adsorption capacity of algae, algae reusable edible.Sea-tangle belongs to a kind of of Larminaria in the brown alga, studies show that its absorption property is better, in the coastal provinces and cities of China breed is arranged all, and output is abundant and cheap.Carry out the research of sea-tangle sorbing material fully, development seaweed bio adsorption technology also is applied to environmental area, has very wide application prospect.
Marine alga is as biological adsorption agent, its softness, shortcoming such as perishable are brought very big inconvenience to adsorption operations, become at present the principal element of restriction marine alga adsorbing metal ions practical application, therefore marine alga need be carried out processing means such as chemical modification and immobilization improves mechanical performance and the chemical stability of marine alga.Investment is a kind of simple method for immobilizing cell, and this method is simple to operate, cell can be locked in the specific macromolecule network structure.This structure can allow substrate infiltration and product diffusion closely to being enough to prevent the cell seepage, and the pair cell activity influence is less, and the intensity of the immobilized cell of making is higher, is the method the most widely of research at present.The selection of carrier is the key of cell fixation embedding techniques, and sodium alginate is a kind of natural macromolecular material, and good biocompatibility is arranged, and to biological nontoxic, mass-transfer performance is good, and can not produce secondary pollution.Gelatin has the effect of suction and support frame, helps the adsorbent moulding, and indeformable.
Summary of the invention
One of purpose of the present invention provides a kind of absorption Biosorption of Heavy Metals agent of adopting sodium alginate and gelatin embedding sea-tangle powder, described biological adsorption agent includes the sea-tangle powder of 80～95 weight portions, the sodium alginate of 2～10 weight portions, the gelatin of 2～8 weight portions and the impurity of surplus, this impurity is calcium alginate, and the particle diameter of described biological adsorption agent is 1.5～3mm.Described biological adsorption agent can be handled contain nickel, cobalt, zinc, cadmium, copper and the plumbous heavy metal wastewater thereby of concentration≤100mg/L, adsorption rate reaches 50～99%, for low concentration≤100mg/L heavy metal wastewater thereby provides a kind of novel environment friendly effective water treatment agent.
Another object of the present invention is to propose a kind of method for preparing the Biosorbent for heavy metals of sodium alginate and gelatin embedding sea-tangle powder, and this preparation method carries out vacuum drying, air-flow pulverizing back and shitosan glue to fresh sea-tangle and carries out the agent of embedding acquisition absorption Biosorption of Heavy Metals.The preparation equipment needed thereby is simple, and operating process is controlled easily.
The method that the present invention prepares the agent of absorption Biosorption of Heavy Metals has following preparation steps:
The first step: the processing of sea-tangle powder
Behind fresh sea-tangle freeze drying 24～72h, adopt the air-flow grinding mode to make the dried sea-tangle powder that particle diameter is 0.3～80 μ m, stand-by;
Described cryodesiccated temperature is-56～-40 ℃, pressure 1～20Pa;
Second step: embedding treatment liquid
Calcium chloride is dissolved in the deionized water, makes embedding treatment liquid through stirring;
The consumption of described calcium chloride is to add 2～5g in every 100ml deionized water;
The 3rd step: system sodium alginate and gelatin glue
Sodium alginate and gelatin are put into deionized water, and stirring under 50～80 ℃ of conditions of temperature makes sodium alginate and gelatin glue;
The consumption of described sodium alginate is to add 0.5～3g in every 100ml acetate;
The consumption of described gelatin is to add 0.5～2g in every 100ml deionized water;
The 4th step: embedding body
Sodium alginate that dried sea-tangle powder that the first step is made and the 3rd step make and gelatin glue mix and make the embedding body;
The consumption of described dried sea-tangle powder is to add 0.7～2g in every 100ml sodium alginate and the gelatin glue;
The 5th step: embedding system biological adsorption agent
The 4th embedding body that make of step is added in the embedding treatment liquid that second step made, solidify 50～250min after, obtain elementary biological adsorption agent after filtration; Use deionized water rinsing then 1～5 time, making the biological adsorption agent that particle diameter is 1.5～3mm behind freeze drying 10～20h under-56～-40 ℃ of conditions.
The specific embodiment
The present invention is described in further detail below in conjunction with embodiment.
A kind of absorption Biosorption of Heavy Metals agent of adopting sodium alginate and gelatin embedding sea-tangle powder of the present invention, described biological adsorption agent includes the sea-tangle powder of 80～95 weight portions, the sodium alginate of 2～10 weight portions, the gelatin of 2～8 weight portions and the impurity (being the micro-calcium alginate that sodium alginate and calcium chloride form) of surplus, and the particle diameter of described biological adsorption agent is 1.5～3mm.
The present invention is a kind of preparation method who adopts the Biosorbent for heavy metals of sodium alginate and gelatin embedding sea-tangle powder, and the concrete operations step is as follows:
The first step: the processing of sea-tangle powder
Behind fresh sea-tangle freeze drying 24～72h, adopt the air-flow grinding mode to make the dried sea-tangle powder that particle diameter is 0.3～80 μ m, stand-by; Described cryodesiccated temperature is-56～-40 ℃, pressure 1～20Pa;
Second step: embedding treatment liquid
Calcium chloride is dissolved in the deionized water, makes embedding treatment liquid through stirring;
The consumption of described calcium chloride is to add 3～5g in every 100ml deionized water;
The 3rd step: system sodium alginate and gelatin glue
Sodium alginate and gelatin are put into deionized water, and stirring under 50～80 ℃ of conditions of temperature makes sodium alginate and gelatin glue;
The consumption of described sodium alginate is to add 0.5～3 in every 100ml deionized water;
The consumption of described gelatin is to add 0.5～2g in every 100ml deionized water;
The 4th step: embedding body
Sodium alginate that dried sea-tangle powder that the first step is made and the 3rd step make and gelatin glue mix and make the embedding body;
The consumption of described dried sea-tangle powder is to add 0.7～2g in every 100ml sodium alginate and the gelatin glue;
The 5th step: embedding system biological adsorption agent
The 4th embedding body that make of step is added in the embedding treatment liquid that second step made, solidify 50～250min after, obtain elementary biological adsorption agent after filtration; Use deionized water rinsing then 1～5 time, making the biological adsorption agent that particle diameter is 1.5～3mm behind freeze drying 10～20h under-56～-40 ℃ of conditions.
In this step, sodium alginate can form calcium alginate with calcium chloride, is used for realizing the sea-tangle powder is embedded in the calcium alginate gel material.
In the present invention, the biological sorbing material sea-tangle of employing all has breed in the coastal provinces and cities of China, and output is abundant, and cheap, its absorption property is fine, as a kind of environment-friendly type heavy metal biological sorbing material, has very wide application prospect.The breaking method of fresh sea-tangle is that air-flow is pulverized in first step, and this breaking method powder particle diameter is more even, and the particle more than 90% can reach about 30 μ m, helps the moulding of adsorbent and can improve the absorption property of adsorbent.
In the present invention, the fixation support sodium alginate of employing is a kind of natural macromolecular material, and good biocompatibility is arranged, to biological nontoxic, mass-transfer performance is good, and can not produce secondary pollution, the adsorbent mechanical strength height that makes is a kind of carrier material of promising adsorbent.
In the present invention, the another kind of fixation support gelatin of employing dissolves in hot water (50～80 ℃), forms the thermal reversibility gel, has the effect of suction and support frame.After water-soluble, can attract each other, interweave, form the network structure of folded lamination layer, and condense with temperature decline, sea-tangle is filled fully in the gel space, can keep stable form, bear bigger load, can reduce fragility, help the adsorbent moulding, and indeformable.
In the present invention, what the embedding treatment of the 4th step adopted is the embedding mode of process for fixation, and this embedding mode is simple to operate, less to the influence of sea-tangle cytoactive.
In the present invention, drying means to fresh sea-tangle in the first step is a vacuum freeze drying, this method (is carried out under 1～20Pa) in low temperature (56～-40 ℃) low pressure, moisture is directly by solid-state distillation, dry back adsorbent internal organizational structure and mode of appearance maintain the original state, there is not surperficial sclerosis problem, and inner forms the spongy of porous, help absorption.
The biological adsorption agent spheroid that obtains through preparation method of the present invention is regular little spherical shape, it is little and even to have particle diameter, specific area is big, advantages of good adsorption effect, to characteristics such as temperature, the pH value scope of application be wide, be suitable for the processing that low concentration≤100mg/L contains heavy metal wastewater therebies such as nickel, cobalt, zinc, cadmium, copper and lead.Adsorbent after the absorption can reclaim heavy metal ion with general chemical method desorb, and adsorbent can reuse, and can not produce secondary pollution.
In order to verify the absorption property of the biological adsorption agent spheroid that the present invention makes, estimate adsorption effect by adsorbance and adsorption rate, desorption efficiency is estimated desorption effect, and concrete computational methods are as follows:
Equilibrium adsorption capacity
Adsorption rate
Desorption efficiency
In the formula, q is an equilibrium adsorption capacity, the mg/g of unit; C
0Be the initial concentration of heavy metal ion, the mg/L of unit; C
eThe concentration of heavy metal ion during for adsorption equilibrium, the mg/L of unit; C
iBe the concentration of heavy metal ion in the stripping liquid, the mg/L of unit, stripping liquid are meant 1mol/L hydrochloric acid or 1mol/L nitric acid; V is the volume that contains the solution of heavy metal, the L of unit; W is the quality of biological adsorption agent spheroid, the g of unit.
Embodiment 1:Under the experiment condition to Ni
2+Absorption
The first step: the processing of sea-tangle powder
With fresh sea-tangle freeze drying 24h, be ground into the dried sea-tangle powder of particle diameter 90% through air-flow at 30 μ m, stand-by; Described cryodesiccated temperature is-56 ℃, pressure 15Pa; The freeze drying instrument selects for use moral sky, Beijing to help development in science and technology Co., Ltd, the FD-1PF freeze drier.
Second step: embedding treatment liquid
Calcium chloride is dissolved in the deionized water, makes embedding treatment liquid through stirring;
The consumption of described calcium chloride is to add 4.25g in every 100ml deionized water;
The 3rd step: system sodium alginate and gelatin glue
Sodium alginate and gelatin are put into deionized water, and stirring under 60 ℃ of conditions of temperature makes sodium alginate and gelatin glue;
The consumption of described sodium alginate is to add 2.1g in every 100ml deionized water;
The consumption of described gelatin is to add 0.5g in every 100ml deionized water;
The 4th step: embedding body
Sodium alginate and gelatin glue that dried sea-tangle powder that the first step is made and the 3rd step make mix, and adopt ultrasonic cell disruptor to pulverize 15min then and make the embedding body; Ultrasonic cell disruptor instrument selection NingBo XinZhi Biology Science Co., Ltd, the JY92-2D ultrasonic cell disruptor.
The consumption of described dried sea-tangle powder is to add 1.5g in every 100ml sodium alginate and the gelatin glue;
The 5th step: embedding system biological adsorption agent
The 4th embedding body and function peristaltic pump that make of step is splashed in the embedding treatment liquid that second step made, make biological adsorption agent after solidifying 120min; Then biological adsorption agent is filtered through filter paper, and adopt deionized water rinsing 2 times, making particle diameter behind the freeze drying 10h is the biological adsorption agent spheroid of 2.5mm.Peristaltic pump instrument selection Cole-Parmer Instrument Company, model 7554-85.
With 0.25g biological adsorption agent spheroid and 100ml concentration is the NiSO of 80mg/L
4Solution joins in the conical flask, after vibration absorption 4h reaches adsorption equilibrium under 25 ℃ of conditions, adopts inductive coupling plasma emission spectrograph (PerkinElmer Instr Ltd., model: Optima 2100/5000) to measure absorption back NiSO
4Ni in the solution
2+Concentration be 29.5mg/L.
Adsorption rate then
Equilibrium adsorption capacity
With the above-mentioned Ni that is adsorbed with
2+The biological adsorption agent spheroid with behind the deionized water rinsing 2 times, put into conical flask; The hydrochloric acid stripping liquid that with 100ml concentration is 1mol/L is then put into conical flask; Behind vibration desorb 4h under 25 ℃ of conditions, adopt inductive coupling plasma emission spectrograph to record Ni in the hydrochloric acid stripping liquid
2+Concentration be 48mg/L, then desorption efficiency
Adsorbent after the desorb can repeat absorption-desorption circulation about five times.
In the present invention, at the biological adsorption agent spheroid to Ni
2+Absorption property, adopt Lang Gemiuer (Langmuir) equation at constant temperature match biological adsorption agent spheroid absorption Ni
2+Isothermal absorption draw the biological adsorption agent spheroid to Ni
2+Maximal absorptive capacity be 39.43mg/g.And absorption adapts to pH=3～8 and 15～55 ℃ of scopes of temperature of broad, to low concentration Ni
2+The adsorption effect of (≤100mg/L) is better.
Embodiment 2:
The first step: the processing of sea-tangle powder
With fresh sea-tangle freeze drying 72h, be ground into the dried sea-tangle powder of particle diameter 0.3～30 μ m through air-flow, stand-by; Described cryodesiccated temperature is-40 ℃, pressure 20Pa;
Second step: embedding treatment liquid
Calcium chloride is dissolved in the deionized water, makes embedding treatment liquid through stirring;
The consumption of described calcium chloride is to add 4g in every 100ml deionized water;
The 3rd step: system sodium alginate and gelatin glue
Sodium alginate and gelatin are put into deionized water, and stirring under 75 ℃ of conditions of temperature makes sodium alginate and gelatin glue;
The consumption of described sodium alginate is to add 4g in every 100ml acetate;
The consumption of described gelatin is to add 2g in every 100ml deionized water;
The 4th step: embedding body
Sodium alginate and gelatin glue that dried sea-tangle powder that the first step is made and the 3rd step make mix, and adopt ultrasonic cell disruptor to pulverize 40min then and make the embedding body;
The consumption of described dried sea-tangle powder is to add 2.6g in every 100ml sodium alginate and the gelatin glue;
The 5th step: embedding system biological adsorption agent
The 4th embedding body that make of step is added in the embedding treatment liquid that second step made, solidify 4h after, filter out biological adsorption agent; Use deionized water rinsing then 3 times, making particle diameter behind freeze drying 20h under-40 ℃ of conditions is the biological adsorption agent spheroid of 1.5mm.
Embodiment 3:
Get 0.25g embodiment 1 preparation the biological adsorption agent spheroid, with 100ml concentration be the Co that contains of 100mg/L
2+, Zn
2+, Cd
2+, Cu
2+And Pb
2+Metallic solution join in the conical flask, transfer pH=7 ± 0.5, after vibration absorption 5h reaches adsorption equilibrium under 25 ℃ of conditions, adopt inductively coupled plasma emission spectrography to measure Co in the solution of absorption back
2+, Zn
2+, Cd
2+, Cu
2+And Pb
2+The concentration of ion, this adsorbent are to the characterization of adsorption such as the following table of each metal ion:
Embodiment 4:
(A) adopt the inductive coupling plasma emission spectrograph device that certain Electroplate Factory's chemical nickeling ageing liquid of obtaining is measured, this aging liquid contains Ni
2+Concentration be 12g/L, pH=4.36.
(B) choose the biological adsorption agent spheroid 0.25g that embodiment 2 makes.
(C) 0.25g biological adsorption agent spheroid of (B) step and the aging liquid of (A) step chemical nickel plating of 100ml are joined in the conical flask, after vibration absorption 4h reaches adsorption equilibrium under 25 ℃ of conditions, adopt in the chemical nickeling ageing liquid after inductive coupling plasma emission spectrograph is measured absorption to contain Ni
2+Concentration be 11.65g/L;
To Ni
2+Equilibrium adsorption capacity
Embodiment 5:
Choose biological adsorption agent spheroid 0.5g that embodiment 2 makes the water inlet sewage of certain Electroplate Factory's sewage plant of obtaining is carried out the adsorption effect experiment, measure through inductively coupled plasma emission spectrography, this sewage contains Ni
2+Concentration be 10.4mg/L, surpass country and allow discharge standard (1mg/L), pH=6.72.
Adopt the adsorption method identical with embodiment 1 to carry out adsorption treatment then, absorption is Ni in the waste water afterwards
2+Concentration is 0.98mg/L, reaches country and allows discharge standard.
Claims (2)
1, a kind of absorption Biosorption of Heavy Metals agent of adopting sodium alginate and gelatin embedding sea-tangle powder, it is characterized in that: described biological adsorption agent is made up of the sea-tangle powder of 80～95 weight portions, the sodium alginate of 2～10 weight portions and the gelatin of 2～8 weight portions and the calcium alginate impurity of surplus, and the particle diameter of described biological adsorption agent is 1.5～3mm; The preparation method of described biological adsorption agent is:
The first step: the processing of sea-tangle powder
Behind fresh sea-tangle freeze drying 24～72h, adopt the air-flow grinding mode to make the dried sea-tangle powder that particle diameter is 0.3～80 μ m, stand-by;
Described cryodesiccated temperature is-56～-40 ℃, pressure 1～20Pa;
Second step: embedding treatment liquid
Calcium chloride is dissolved in the deionized water, makes embedding treatment liquid through stirring;
The consumption of described calcium chloride is to add 2～5g in every 100ml deionized water;
The 3rd step: system sodium alginate and gelatin glue
Sodium alginate and gelatin are put into deionized water, and stirring under 50～80 ℃ of conditions of temperature makes sodium alginate and gelatin glue;
The consumption of described sodium alginate is to add 0.5～3g in every 100ml deionized water;
The consumption of described gelatin is to add 0.5～2g in every 100ml deionized water;
The 4th step: embedding body
Sodium alginate that dried sea-tangle powder that the first step is made and the 3rd step make and gelatin glue mix and make the embedding body;
The consumption of described dried sea-tangle powder is to add 0.7～2g in every 100ml sodium alginate and the gelatin glue;
The 5th step: embedding system biological adsorption agent
The 4th embedding body that make of step is added in the embedding treatment liquid that second step made, solidify 50～250min after, obtain elementary biological adsorption agent after filtration; Use deionized water rinsing then 1～5 time, making the biological adsorption agent that particle diameter is 1.5～3mm behind freeze drying 10～20h under-56～-40 ℃ of conditions.
2, according to the agent of the described absorption Biosorption of Heavy Metals of claim 1, it is characterized in that: described biological adsorption agent can be handled contain nickel, cobalt, zinc, cadmium, copper and the plumbous heavy metal wastewater thereby of concentration≤100mg/L, and adsorption rate reaches 50～99%.
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