CN110354822A - A kind of preparation method of aminated surface ion trace straw base biological adsorption agent - Google Patents
A kind of preparation method of aminated surface ion trace straw base biological adsorption agent Download PDFInfo
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- CN110354822A CN110354822A CN201910541079.1A CN201910541079A CN110354822A CN 110354822 A CN110354822 A CN 110354822A CN 201910541079 A CN201910541079 A CN 201910541079A CN 110354822 A CN110354822 A CN 110354822A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/268—Polymers created by use of a template, e.g. molecularly imprinted polymers
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The present invention provides a kind of preparation method of aminated surface ion trace straw base biological adsorption agent, belongs to separation of metal ions field, comprising the following steps: (1) by stalk powder, pickling, alkali cleaning obtain pretreated straw powder；(2) strong base solution is added in pretreated straw powder, epoxychloropropane, carries out etherification reaction, is added in weak caustic solution after washed, centrifugation, organic amine is added, carry out open loop grafting amine reaction, the stalk powder of dry surface amine groups；(3) stalk powder of surface amine groups, heavy metallic salt are added in solvent, after carrying out adsorption reaction, crosslinking agent are added and carries out surface imprinted reaction, then is successively washed with EDTA solution, it is freeze-dried to obtain aminated surface ion trace straw base biological adsorption agent.The present invention can realize the separation and enrichment of trace heavy metal ion in complex system using trace straw base biological adsorption agent to the coordination effect and trace effect of heavy metal ion, realize the separation of heavy metal ions in wastewater.
Description
Technical field
The invention belongs to separation of metal ions fields, and in particular to a kind of aminated surface ion trace straw base biology suction
Attached dose of preparation method.
Background technique
With the development of industry, the discharge of plurality of heavy metal waste water has seriously polluted the environment, and causes to the mankind extremely tight
The harm of weight.The alarm bell of heavy metal wastewater thereby improvement has been beaten in the outburst of the events such as " cadmium rice ", " blood lead ", " pain disease ".Currently,
Process for treating heavy-metal waste water is numerous, comprising: the precipitation method, extraction, membrane separation process, electrochemical process, absorption method etc., but these sides
Method there are higher cost, it is complicated for operation, bring secondary pollution, effect is undesirable the problems such as, therefore there is an urgent need to develop a kind of low
The new method of concentration heavy metal wastewater treatment.
In recent years, biosorption process is concerned because having many advantages, such as abundant raw materials, due to secondary pollution is small.Biological adsorption
Method is as a kind of heavy metal containing wastewater treatment technology, mainly using discarded biological such as stalk as in adsorbent removal water body
Heavy metal.Stalk is mainly made of cellulose, hemicellulose and lignin, and surface has hydroxyl abundant, by surface
Different functional groups modification biological adsorbent can be prepared after processing.However, due to complicated components in actual waste water, each component concentration difference
It is not big, serious interference, in single surface modified sorbent complex system relatively difficult to achieve the absorption of specific ion with separate, preparation height
Selectivity organism adsorbent has become the difficult point and hot spot of research.
Summary of the invention
In view of this, the present invention provides a kind of preparation method of aminated surface ion trace straw base biological adsorption agent,
Aminated straw base biological adsorption agent is prepared for using chemical graft process first, recycles aminated straw base biological adsorption agent table
The amido in face and the coordination effect of heavy metal ion and surface ion engram technology are prepared for aminated surface ion trace straw
Stalk base biological adsorption agent.It can be real using coordination effect and trace effect of the trace straw base biological adsorption agent to heavy metal ion
The separation and enrichment of heavy metal in existing complex system, the method is easy to operate, at low cost, can be realized the choosing of heavy metal ion in water
The absorption of selecting property, and adsorption capacity is strong.
The present invention is a kind of preparation method of aminated surface ion trace straw base biological adsorption agent, including following step
It is rapid:
(1) stalk is successively washed, dries, is milled, being sieved and to obtain stalk powder by stalk pretreatment, will
The stalk powder carries out pickling with 0.01 mol/L HCl, 0.01 mol/L NaOH carries out alkali cleaning, deionized water is washed
After obtain pretreated straw powder, stalk can be bagasse, rice straw, cotton stalk, straw, cornstalk etc..
(2) pretreated straw powder, epoxychloropropane are added in strong base solution by stalk surface amine groups,
40 ~ 70 DEG C are stirred to react 20 ~ 80 min, carry out etherification reaction, wherein the matter of pretreated straw powder, epoxychloropropane
Amount is than being 1:0.5 ~ 5, and strong base solution can be one of sodium hydroxide solution, potassium hydroxide solution or a variety of, and concentration is 1 ~ 4
mol/ L-1, the solid-to-liquid ratio of pretreated straw powder and strong base solution is 1:(10 ~ 50) and g/mL,；
Obtained solid is added to weak base after washed again, centrifugation (weak base can be the sodium carbonate that concentration is 0.05 ~ 0.8 mol/L)
In solution, stalk powder and Na2CO3The solid-to-liquid ratio of solution is 1:(10 ~ 50) g/mL, organic amine is added under stirring condition, in nitrogen
Atmosphere encloses 0.5 ~ 4 h of reaction at 50 ~ 80 DEG C, carries out the reaction of open loop grafting organic amine, and reaction is finished, and is washed to neutrality, and vacuum is dry
The stalk powder of dry surface amine groups, pretreated straw powder, organic amine mass ratio be 1:0.3 ~ 4, it is contained in organic amine
Nitrogen-atoms number >=4, the molecular formula of organic amine are as follows: NH2(CH2CH2NH)nCH2CH2NH2(n >=2) or C2x+4kH5x+10kNx+2k (x
+ 2k >=4), such as organic amine can be polyvinylamine, triethylene tetramine, tetraethylenepentamine.
Stalk is mainly made of cellulose, hemicellulose and lignin, and surface has hydroxyl abundant, at surface
Different functional groups modification biological adsorbent can be prepared after reason, adsorb different substances, the present invention using this feature by surface at
Reason enables stalk powder surface to adsorb specific heavy metal ion.Step (2) is the modification of stalk powder, passes through highly basic
The hydroxyl Yu epoxychloropropane on stalk powder surface carry out etherification reaction under environment, and open loop grafting then occurs in mild alkaline conditions
The reaction of amine so that stalk powder surface have amido, amido to specific heavy metal ion have it is coordinating, can adsorb weight
Metal ion.
(3) stalk powder of surface amine groups, heavy metallic salt are added in solvent by stalk surface ion trace,
Adsorption reaction is carried out, adsorption reaction 1 ~ 3 hour, the amido on stalk powder surface can be coordinated with heavy metal ion, absorption weight
Metal ion；Crosslinking agent is added and carries out cross-linking reaction, supernatant is removed after centrifugation, then is successively washed with EDTA solution, deionization
Stalk powder after washing crosslinking, the concentration of EDTA can be 0.01 mol/L, freeze-dried to obtain aminated surface ion trace
Straw base biological adsorption agent.Heavy metallic salt is one of soluble copper salt, lead salt, stalk powder, the huge sum of money of surface amine groups
Belonging to the ratio between mass of ion is 1:0.05 ~ 0.5, and crosslinking agent can be glutaraldehyde, and the stalk powders of surface amine groups, crosslinking agent are consolidated
Liquor ratio is 1:(0.5 ~ 5) g/mL.
The surface of the stalk powder of surface amine groups has amido that can be coordinated with heavy metal ion in the step, after coordination
Complex is formed, complexation reaction is usually to carry out according to the ratio of 1:4, and the amount of heavy metal ion is few in the present invention, together
When there is also steric hindrance, so all with heavy metal ion complexation reaction can occur for not all amido, have neither part nor lot in coordination
The amido of reaction and the hydroxyl on stalk surface further react to form comparatively dense reticular structure, cross-linking reaction with crosslinking agent
It finishes, the metal ion of coordination is eluted using eluant, eluent, obtains the aminated surface ion trace straw base in trace hole
Biological adsorption agent.
It is surface imprinted be using surface ion engram technology synthesis adsorbent can specifically select it is certain specific
Ion avoids compared to traditional engram technology and embeds too deep situation, be conducive to the elution of template ion, while can also
Guarantee its recognition performance.Currently, modifying carrier, template ion and function monomer are then formed by complex grafting
Certain functional groups are introduced in carrier surface grafting to its surface, or first, then with after template ion effect, crosslinked, polymerization is most
Ion imprinted polymer is obtained eventually.For the present invention using stalk powder as carrier, it is one that modification biological adsorbent surface functional group is abundant
Kind excellent trace carrier is remarkably improved modified straw adsorbent to heavy metal copper and lead ion by surface imprinted technology
Adsorptive selectivity.
The present invention will pass through process for modifying surface first to have high coordination to heavy metal ion (such as copper ion, lead ion)
The amidine functional group of ability is grafted to stalk surface, then prepares ion blotting adsorbent by surface imprinted mode.In trace
In the process, the heavy metal ion of trace forms complex with the amido on stalk surface first, has neither part nor lot in the amine of complexation reaction
Base and the hydroxyl on stalk surface further react to form comparatively dense reticular structure with crosslinking agent glutaraldehyde, and cross-linking reaction is complete
Finish, is eluted the metal ion of coordination using eluant, eluent, the aminated surface ion trace straw base for obtaining trace hole is raw
Object adsorbent.There are stronger coordination ability, size since trace hole is identical as trace ion size, and to trace ion
Metal ions different, that coordination ability is different are difficult to enter hole, dimension, and surface imprinted adsorbent shows very trace ion
Efficiently separating and recycling for trace heavy metal ion in Complex water body may be implemented in strong adsorptive selectivity.
Beneficial effects of the present invention: aminated straw base biological adsorption agent, then benefit are prepared for using chemical graft process first
With the amido on aminated straw base biological adsorption agent surface and the coordination effect of heavy metal ion and surface ion engram technology
It is prepared for aminated surface ion trace straw base biological adsorption agent.The biological adsorption agent of preparation can to specific heavy metal from
Son is adsorbed, and strong adsorption, can effectively recycle specific metal ion, utilizes the trace straw base biological adsorption agent pair
The coordination effect and trace effect of heavy metal ion can realize the separation and enrichment of heavy metal in complex system, method operation letter
It is single, it is at low cost, realize that the separation of heavy metal ions in wastewater and resource utilization utilize.
Detailed description of the invention
Fig. 1 is a kind of aminated surface ion trace straw base life provided in specific embodiment of the invention embodiment 1
The preparation principle figure for the adsorbent that the preparation method of object adsorbent is prepared；
Fig. 2 is that a kind of aminated surface ion trace straw base biology provided in specific embodiment of the invention embodiment 1 is inhaled
The adsorbent that attached dose of preparation method is prepared is to copper ion selective absorption Capacity Plan；
Fig. 3 is that a kind of aminated surface ion trace straw base biology provided in specific embodiment of the invention embodiment 2 is inhaled
The adsorbent that attached dose of preparation method is prepared is to lead ion selective absorption Capacity Plan.
Specific embodiment
The present invention will be described in detail With reference to embodiment.
Embodiment 1
A kind of preparation method of aminated surface ion trace straw base biological adsorption agent, comprising the following steps:
(1) stalk is successively washed, dries, is milled, being sieved and to obtain stalk powder by stalk pretreatment, will
The stalk powder carries out pickling with 0.01 mol/L HCl, 0.01 mol/L NaOH carries out alkali cleaning, deionized water is washed
After obtain pretreated straw powder, stalk can be straw；
(2) stalk surface amine groups, it is 1 that 10 g pretreated straw powder, 6 g epoxychloropropane, which are added to 100 g concentration,
mol/ L-1Sodium hydroxide solution solution in, 40 DEG C are stirred to react 20 min, after carrying out substitution reaction, then washed, centrifugation
Obtained solid is added in the sodium carbonate liquor that 100g concentration is 0.05 mol/L, and 3g polyvinylamine is added under stirring condition,
React 0.5 h at 50 DEG C of nitrogen atmosphere, carry out cycloaddition reaction, be washed to neutrality, be dried in vacuo surface amine groups stalk
Powder；
(3) copper nitrate of the stalk powder of 1 g surface amine groups, 0.05 g are added to the water by stalk surface ion trace, into
The amido of row adsorption reaction, 1 h of adsorption reaction, stalk powder surface can be coordinated with heavy metal ion, adsorbed heavy metal ion, added
Enter 0.5 mL crosslinking agent glutaraldehyde and carry out cross-linking reaction, supernatant is removed after centrifugation, then successively using concentration can be 0.01 mol/
The EDTA solution of L, deionized water wash the stalk powder after crosslinking, freeze-dried to obtain aminated surface ion trace straw base
Biological adsorption agent.
A kind of preparation principle of the preparation method of aminated surface ion trace straw base biological adsorption agent in the present embodiment
Figure by process for modifying surface as shown in Figure 1, will there is the amidine functional group of high coordination ability to be grafted to copper ion first
Stalk surface, the heavy metal ion of trace form complex with the amido on stalk surface again, have neither part nor lot in the amine of complexation reaction
Base and the hydroxyl on stalk surface further react to form comparatively dense reticular structure with crosslinking agent glutaraldehyde, and cross-linking reaction is complete
Finish, is eluted the metal ion of coordination using eluant, eluent, the aminated surface ion trace straw base for obtaining trace hole is raw
Object adsorbent.Fig. 2 is selective absorption Capacity Plan of the biological adsorption agent manufactured in the present embodiment to copper ion, wherein test is made
Test solution is five kinds of Binary constituent solutions, and respectively initial molar concentration is than Cu, Pb solution for Cu:Pb=1:1；Initially
Molar concentration rate is Cu, Cb solution of Cu:Cb=1:1；Initial molar concentration is than Cu, Zn solution for Cu:Zn=1:1；Initially rub
For that concentration than Cu, Mg solution for Cu:Mg=1:1, IMP is adsorbent manufactured in the present embodiment, and N-IMP is that blotting is not used
The same type adsorbent of preparation, IMP group is apparently higher than N-IMP group, the present embodiment to the adsorptivity of copper ion as can be seen from Figure 2
The adsorbent of preparation has good Selective adsorption to copper ion.
Embodiment 2
A kind of preparation method of aminated surface ion trace straw base biological adsorption agent, comprising the following steps:
(1) stalk is successively washed, dries, is milled, being sieved and to obtain stalk powder by stalk pretreatment, will
The stalk powder carries out pickling with 0.01 mol/L HCl, 0.01 mol/L NaOH carries out alkali cleaning, deionized water is washed
After obtain pretreated straw powder, stalk is bagasse；
(2) stalk surface amine groups, it is 4 that 10 g pretreated straw powder, 50 g epoxychloropropane, which are added to 500 g concentration,
mol/ L-1Potassium hydroxide solution solution in, 70 DEG C are stirred to react 80 min, carry out institute after substitution reaction, then washed, centrifugation
It obtains solid to be added in the sodium carbonate liquor that 500 g concentration are 0.8 mol/L, 40 g triethylene tetramines is added under stirring condition,
React 4 h at 80 DEG C of nitrogen atmosphere, carry out cycloaddition reaction, be washed to neutrality, be dried in vacuo surface amine groups stalk
Powder；
(3) plumbi nitras of the stalk powder of 1 g surface amine groups, 0.5 g are added stalk surface ion trace
Into water, adsorption reaction is carried out, the amido of 3 h of adsorption reaction, stalk powder surface can be coordinated with heavy metal ion, be adsorbed
Heavy metal ion is added 5 mL crosslinking agent glutaraldehydes and carries out cross-linking reaction, supernatant is removed after centrifugation, then successively can be with concentration
Wash the stalk powder after crosslinking for the EDTA solution of 0.01 mol/L, deionized water, freeze-dried aminated surface from
Sub- trace straw base biological adsorption agent.
Fig. 3 is selective absorption Capacity Plan of the biological adsorption agent manufactured in the present embodiment to copper ion, wherein test is made
Test solution is five kinds of Binary constituent solutions, and respectively initial molar concentration is than Cu, Pb solution for Pb:Cu=1:1；Initially
Molar concentration rate is Pd, Cb solution of Pd:Cb=1:1；Initial molar concentration is than Pd, Zn solution for Pd:Zn=1:1；Initially rub
For that concentration than Pd, Mg solution for Pd:Mg=1:1, IMP is adsorbent manufactured in the present embodiment, and N-IMP is that blotting is not used
The same type adsorbent of preparation, IMP group is apparently higher than N-IMP group, the present embodiment to the adsorptivity of copper ion as can be seen from Figure 3
The adsorbent of preparation has good Selective adsorption to copper ion.
Embodiment 3
A kind of preparation method of aminated surface ion trace straw base biological adsorption agent, comprising the following steps:
(1) stalk is successively washed, dries, is milled, being sieved and to obtain stalk powder by stalk pretreatment, will
The stalk powder carries out pickling with 0.01 mol/L HCl, 0.01 mol/L NaOH carries out alkali cleaning, deionized water is washed
After obtain pretreated straw powder, stalk is rice straw；
(2) stalk surface amine groups, it is 2 that 10 g pretreated straw powder, 5 g epoxychloropropane, which are added to 200 g concentration,
mol/ L-1Highly basic sodium hydroxide solution in, 55 DEG C are stirred to react 50 min, after carrying out substitution reaction, then washed, centrifugation
Obtained solid is added in the sodium carbonate liquor that 210 g concentration are 0.12 mol/L, and 12 g, tetra- ethylene five is added under stirring condition
Amine, reacts 3 h at 70 DEG C of nitrogen atmosphere, carries out cycloaddition reaction, is washed to neutrality, be dried in vacuo surface amine groups straw
Stalk powder；
(3) plumbi nitras of the stalk powder of 1 g surface amine groups, 0.2 g are added stalk surface ion trace
Into water, adsorption reaction is carried out, the amido of 2 h of adsorption reaction, stalk powder surface can be coordinated with heavy metal ion, be adsorbed
Heavy metal ion is added 2 mL crosslinking agent glutaraldehydes and carries out cross-linking reaction, supernatant is removed after centrifugation, then successively can be with concentration
Wash the stalk powder after crosslinking for the EDTA solution of 0.01 mol/L, deionized water, freeze-dried aminated surface from
Sub- trace straw base biological adsorption agent.
It is similar in the test result and embodiment 2 of the adsorbent prepared in the present embodiment.
The present invention uses chemical graft process to be prepared for aminated straw base biological adsorption agent first, recycles aminated stalk
The amido on base biological adsorption agent surface and the coordination effect of heavy metal ion and surface ion engram technology are prepared for aminated
Surface ion trace straw base biological adsorption agent.The biological adsorption agent of preparation can adsorb specific heavy metal ion,
And strong adsorption, specific metal ion can be effectively recycled, using the trace straw base biological adsorption agent to heavy metal ion
Coordination effect and trace effect can realize the separation and enrichment of heavy metal in complex system, the method is easy to operate, at low cost, real
The separation of existing heavy metal ions in wastewater and resource utilization utilize.
The present invention is not limited to above-mentioned specific embodiment, and the invention may be variously modified and varied.All foundations
Technical spirit of the invention should be included in the present invention to embodiment of above any modification, equivalent replacement, improvement and so on
Protection scope.
Claims (10)
1. a kind of preparation method of aminated surface ion trace straw base biological adsorption agent, which is characterized in that including following step
It is rapid:
(1) stalk is successively washed, dries, is milled, being sieved and to obtain stalk powder by stalk pretreatment, by the stalk powder
Carry out pickling, alkali cleaning obtains pretreated straw powder；
(2) pretreated straw powder, epoxychloropropane are added in strong base solution by stalk surface amine groups, be etherified anti-
It answers, obtained solid is added in weak caustic solution after washed, centrifugation, and organic amine is added under stirring condition, is carried out open loop and is grafted amine
Reaction, be washed to neutrality, be dried in vacuo surface amine groups stalk powder；
(3) stalk powder of surface amine groups, heavy metallic salt are added in solvent, are adsorbed by stalk surface ion trace
After reaction, crosslinking agent is added and carries out cross-linking reaction, supernatant is removed after centrifugation, then successively washed with EDTA solution, deionized water
Stalk powder after crosslinking, it is freeze-dried to obtain aminated surface ion trace straw base biological adsorption agent.
2. a kind of preparation method of aminated surface ion trace straw base biological adsorption agent according to claim 1,
It is characterized in that, the time of adsorption reaction described in step (3) is 1 ~ 3h.
3. a kind of preparation method of aminated surface ion trace straw base biological adsorption agent according to claim 1,
It is characterized in that, the crosslinking agent is glutaraldehyde.
4. a kind of preparation method of aminated surface ion trace straw base biological adsorption agent according to claim 1,
It is characterized in that, the stalk powder of surface amine groups, heavy metal ion mass ratio are 1:0.05 ~ 0.5 in step (3).
5. a kind of preparation method of aminated surface ion trace straw base biological adsorption agent according to claim 1,
It is characterized in that, the stalk powder of surface amine groups, the solid-to-liquid ratio of crosslinking agent are 1:(0.5 ~ 5) g/mL.
6. a kind of preparation method of aminated surface ion trace straw base biological adsorption agent according to claim 1,
It is characterized in that, step (3) heavy metallic salt is one of soluble copper salt, lead salt.
7. a kind of preparation method of aminated surface ion trace straw base biological adsorption agent according to claim 1,
It is characterized in that, institute's nitrogen atom number >=4 in organic amine described in step (2).
8. a kind of preparation method of aminated surface ion trace straw base biological adsorption agent according to claim 1,
It is characterized in that, step (2) strong base solution is one of sodium hydroxide solution, potassium hydroxide solution or a variety of.
9. a kind of preparation method of aminated surface ion trace straw base biological adsorption agent according to claim 8,
It is characterized in that, the concentration of step (2) described strong base solution is 1 ~ 4 mol/ L-1。
10. a kind of preparation method of aminated surface ion trace straw base biological adsorption agent according to claim 8,
It is characterized in that, the mass ratio of step (2) the pretreated straw powder and epoxychloropropane is 1:(0.5 ~ 5) g/mL.
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