CN107126940A - The preparation method of alginate plural gel and its application to heavy mental treatment in water - Google Patents
The preparation method of alginate plural gel and its application to heavy mental treatment in water Download PDFInfo
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- 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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C—CHEMISTRY; METALLURGY
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Abstract
The invention belongs to high polymer material application and preparation technical field, the specifically related to preparation method of alginate plural gel and its application to heavy mental treatment in water, first prepare four kinds of alginates, and polyethylene glycol oxide, 4A molecular sieves and activated carbon are combined respectively, obtain alginate plural gel ball, the alginate plural gel ball warp goes over ion-cleaning, drain after the moisture content of surface, for that can adsorb lead ion and mercury ion in water in heavy mental treatment in water, alginate plural gel of the invention is for the Pb in water2+And Hg2+Serve excellent absorption property, it is to avoid the problem of single adsorption agent causes secondary pollution of water, adsorbent with multiple layers complex structural designs.
Description
Technical field
The invention belongs to high polymer material application and preparation technical field, and in particular to the preparation side of alginate plural gel
Method and its application to heavy mental treatment in water.
Background technology
Water is the source of all life, but the road of " first pollute, then administer " that heavy industry is walked, and urban population are fast
Speed amplification, heavy damage and pollution are caused to water resource, and water process turns into world today's environmental protection therewith needs emphasis badly
The problem of solution.Especially in China, using heavy industry as rely on the economy developed rapidly, the accounting whole world 1/4 population Buddhist monk
The laws and regulations not perfected so that the gesture of comprehensive expansion, the contaminated present situation ten of water resource has been presented in the contaminated phenomenon of water body
Divide troubling, even big city, Drinking Water report not up to standard is also of common occurrence.According to the public and Environmental Research Center
The Chinese water pollution map of issue, by September, 2010, " Chinese water pollution map " has listed the enterprise more than 69000
Industry pollution record 1.Although " 13 planning " has pointed out and adheres to Green Development, the repair process for the water resource being destroyed is still
It is repaiied far Endless Way, at least needs the century-old time to substantially improve.Current domestic water and industrial water are main
Pollutant is heavy metal ion, organic matter, microorganism etc., and wherein the heavy metal ion in industrial wastewater is the important of ambient water quality
Pollution sources 2-5, is mainly derived from the draining of mine tunnel, waste-rock yard leaching water, milltailings draining, non-ferrous metals smelting works' dedusting
Draining, Non-ferrous Metals Processing Factory's pickling waste waters, Electroplate Factory's plating piece washings, pickling iron and steel draining and electrolysis, agricultural chemicals, medicine, oil
The waste water that the industry such as paint, dyestuff is discharged, wherein metal plating waste water is the primary discharge source 5-7 of heavy metal.In addition, life is dirty
Water, percolate, agricultural wastewater and acid rain are also the emission source 8 of heavy metal.Heavy metal especially Pb, Hg, Cd, Cr etc. are most
Has the important pollutant of potential hazard, it causes irrecoverable to the organ such as human body and the heart of animal, lung, liver, nerve, joint
Infringement, the also existence to fishes and shrimps, plant etc. forms grave danger.Therefore cheap water pollution processing adsorbent is developed,
And it is very necessary to put into actual scale application.
From the angle of cost-effective gold and raising heavy metal removing rate, current domestic and international most popular processing method
It is absorption method, it is widely used as a kind of important Chemical Physics method in heavy metal containing wastewater treatment, such as activity
Charcoal, molecular sieve, natural high molecular substance, ion exchange resin and microorganism etc. can be used as adsorbent to handle sewage.
The result of study about heavy metals removal shows both at home and abroad, and it is main research in recent years to develop new adsorbent
Object, and natural algae extract adsorption recovery heavy metal ions in wastewater in the utilization seawater just grown up in recent years
Technology becomes the study hotspot of people.Since 1990s, the United States, Russia, Deng states are to start to use biosorption process
Electroplating wastewater is handled, remarkable effect has been obtained, and start industrially Preliminary Applications.Extracted using sodium alginate as the algae of representative
Thing have wide material sources, it is cheap, have higher clearance to low concentration pollutant, be easily recycled and do not produce two
The advantages of secondary pollution, it is used widely in water treatment field.Sodium alginate ((C5H7O4COONa)n, SA) be alginic acid sodium
Salt, containing free carboxy (- COONa), can occur ion-exchange reactions with heavy metal ion.Sodium alginate is nontoxic with some
Metal cation (such as Ca of environmental protection2+、Cu2+、Zn2+、Fe3+Deng) mixing, can occur curing reaction, can obtain water insoluble tool
There is the polyalcohol hydrogel nanoporous sorbing material of three-dimensional net structure.Carboxyl on its skeleton can occur with heavy metal ion
Exchange, at the same macromolecular chain be mutually wound it is mesoporous can expose more adsorption sites, with adsorb to greatest extent weight
Metal ion, obtained solidfied material can collect recycling again, therefore such material is widely used in the absorption of water process
Agent.
Research shows that sodium alginate all has certain adsorption capacity to heavy metal ion such as mercury, copper, tin, can conduct
The adsorbent of Adsorption of Heavy Metals.Wikinson etc. removes the research table of heavy metal Hg in sewage in calcium alginate fixed pellet algae
It is bright, there is the ability of Adsorption of Mercury as the sodium alginate of carrier gel, in an experiment, 10% suction-operated is served.Yan Guo
Peace has equally also shown that sodium alginate has the conclusion of Adsorption of Heavy Metals ability in an experiment.Zhu Yimin, which have studied, uses sodium alginate
The Cu in aqueous phase is removed as adsorbent2+, and influence of the experiment condition to adsorption effect in adsorption process.Its conclusion is to inhale
Attached process has just reached balance in 10min or so；In pH=6, adsorption effect reaches most preferably.But it is due to that SA has machinery by force
Degree is poor, the shortcomings of being easily bacterially decomposed in water, and easily secondary pollution is caused to water body after dissolving.Therefore, adding has height
The hydrophilic material that intensity and resistance to bacterium corrode fixes SA, is conducive to extending the service life of adsorbent.Polyethylene glycol oxide
(PEO) it is a kind of high molecular polymer, can be with calcium alginate formation copolymer containing substantial amounts of-OH.Simultaneously as PEO contains
There is hydroxy functional group, can also be reacted with heavy metal ion, so that the adsorption capacity of gel ball slightly has raising.And SA and
PEO is hydrophilic polymer, and intersolubility is good, and the research report that both are used in combination at present is less.
Natural zeolite (such as 3A, 4A, 5A molecular sieve) is also a kind of price more cheap material.Molecular sieve (is also known as synthesized
Zeolite) it is a kind of many microporous crystals of alumino-silicate.It is made up of basic skeleton structure silica, aluminum-oxygen tetrahedron, with equal
Even micropore, its aperture is suitable with general molecular size.The application of molecular sieve widely, can make efficient drying agent, selection
Property adsorbent, catalyst, ion-exchanger etc..The ion-exchange performance of molecular sieve has benefited from there is metal in its skeleton lattice
Cation (such as Na+, K+, Ca2+, Li+Deng), it can be replaced with other metal cations.Such as the Na in 4A molecular sieves+Can be with
Ca in hard water2+、Mg2+Ion is swapped, so as to reach the purpose of demineralized water.Also can will be harmful on a small quantity in the aqueous solution
Heavy metal ion (such as Pb2+、Hg2+、Cd2+、Cr6+) can be easy to rapidly remove, there is highly important meaning to purifying water.
And natural molecule sieve is nontoxic, to human height's safety.It is non-stimulated to eyes, skin, allergy will not be caused, it is safe and reliable.
It is deposited in soil, does not pollute after washing, but also ecology can be had no adverse effects with improved soil, 4A molecular sieves.
Therefore molecular sieve is also widely used for ion-exchange field.
Activated carbon is more cheap sorbent material, home market price 3-6 members/kilogram.Activated carbon wood chip,
The carbonaceous materials such as shell, lignite are raw material, are made through carbonization and activation.There are powdery (particle diameter is 10~50 μm) and graininess (grain
Footpath is 0.4~2.4mm) two kinds.The general character is porous, and specific surface area is big up to 500~1000m2/ g, the coal mass active carbon of high-quality can
Up to 1300m2/ more than g.Activated carbon can not only remove in water removal to produce the material of stink and organic matter and (such as phenol, benzene, chlorine, agricultural chemicals, wash
Wash agent, haloform etc.), also have stronger to heavy metal ion such as silver, cadmium, chromate, cyanogen, antimony, arsenic, bismuth, tin, mercury, lead, nickel
Adsorption capacity.Studies have reported that, the Macromolecule glueballs of embedding Powdered Activated Carbon is up to 94% to the removal efficiency of Phos, than
The clearance (41%) of single-activity charcoal adds more than 2 times.Therefore active carbon adsorption is widely used in Water purification and useless
The advanced treating of water secondary treatment yielding water.Its major advantage is that degree for the treatment of is high, effect stability.Have the disadvantage that processing cost is high,
And ash content is easily leached in water, easily causes secondary pollution to water body.
The processing direction of the current heavy metal ion in water, urgent need finds one kind and can solve the problem that single adsorption agent such as activated carbon
The absorption for the problems such as using the secondary pollution of water caused, adsorbent with multiple layers complex structural designs under for a long time with sodium alginate
Agent.
The content of the invention
Based on the technical problem proposed in above-mentioned background technology, it is an object of the invention to provide alginate plural gel
Preparation method and its application to heavy mental treatment in water, the alginate plural gel is for the Pb in water2+And Hg2+
Serve excellent absorption property, it is to avoid single adsorption agent causes secondary pollution of water, adsorbent with multiple layers structure design is answered
Miscellaneous the problem of.
To realize above-mentioned technical purpose, the technical solution adopted by the present invention is as follows：
The preparation method of alginate plural gel, specific preparation method is as follows：
The preparation of alginate ball：5mL~10mL sodium alginates are taken, are added dropwise with being stirred continuously lower uniform speed slow respectively
To 20mL~30mL CaCl2、CuCl2、ZnCl2、FeCl3In solution, drip off and stop stirring immediately, stand 2h~24h, obtain
Alginate ball SA-Ca, SA-Cu, SA-Zn, SA-Fe of four kinds of different colours.
The preparation of alginate-polyethylene glycol oxide plural gel ball：Take 5mL~10mL sodium alginates, 2mL~10mL polyoxies
Change ethene, which is placed in magnetic stirring apparatus, to be stirred, and 20mL~30mL CaCl is respectively added slowly under stirring2、CuCl2、
ZnCl2、FeCl3In solution, drip off and stop stirring immediately, stand 2h~24h, the alginate for obtaining four kinds of different colours is combined
Gel ball SA-Ca-PEO, SA-Cu-PEO, SA-Zn-PEO, SA-Fe-PEO.
The preparation of alginate-polyethylene glycol oxide -4A molecular sieve plural gel balls：Take 5mL~10mL sodium alginates, 2mL
~10mL polyethylene glycol oxides and 0.05g~0.2g 4A molecular sieves are placed in magnetic stirring apparatus and stirred, and stirring is lower slow respectively
It is added to 20mL~30mL CaCl2、CuCl2、ZnCl2、FeCl3In solution, drip off and stop stirring immediately, stand 2h~24h,
Obtain alginate plural gel ball SA-Ca-PEO-4AZ, SA-Cu-PEO-4AZ, SA-Zn-PEO- of four kinds of different colours
4AZ、SA-Fe-PEO-4AZ。
The preparation of alginate-polyethylene glycol oxide-activated carbon plural gel ball：Take 5mL~10mL sodium alginates, 2mL~
10mL polyethylene glycol oxides and 0.05g~0.2g activated carbons are placed in magnetic stirring apparatus and stirred, and are respectively added slowly under stirring
To 20mL~30mL CaCl2、CuCl2、ZnCl2、FeCl3In solution, drip off and stop stirring immediately, stand 2h~24h, obtain
Alginate plural gel ball SA-Ca-PEO-AC, SA-Cu-PEO-AC, SA-Zn-PEO-AC, SA-Fe- of four kinds of different colours
PEO-AC。
Further, the mass concentration of the sodium alginate is 2%.
Further, the mass concentration of the polyethylene glycol oxide is 0.1%.
Further, the CaCl2Solution, CuCl2Solution, ZnCl2Solution, FeCl3The concentration of solution be 0.5mol/L~
1mol/L。
In addition, the application the invention also discloses alginate plural gel to heavy mental treatment in water, the sea
Alginates plural gel is applied to that in water process heavy metal lead ion and the mercury ion in water can be adsorbed.
Further, the alginate plural gel is using preceding needing with deionized water rinsing 3~5 times, and drains surface
After moisture content, then to mix with the water containing heavy metal ion progress heavy metal ion adsorbed.
Further, suction of SA-Ca, SA-Ca-PEO, SA-Ca-PEO-4AZ, SA-Ca-PEO-AC gel to lead ion
Attached rate is more than 98%.
Further, the alginate plural gel SA-Ca-PEO-4AZ is to the adsorption capacity of lead ion in water
99.1%.
Further, the alginate plural gel SA-Cu-PEO-4AZ to the adsorption capacity of mercury ion in water up to 87%,
The alginate plural gel SA-Cu-PEO-AC is to the adsorption capacity of mercury ion in water up to 85%.
The preparation method of the alginate plural gel ball of the present invention is simple, the alginate plural gel ball prepared
To the Pb in water2+And Hg2+Excellent absorption property is served, and finds to add 4A molecular sieves in alginate ball
It can increase substantially for Pb2+Adsorption capacity, and add activated carbon and serve opposite effect.In alginate
Activated carbon is added in ball or 4A molecular sieves also contribute to improve for Hg2+Adsorption capacity, but depending on alginate salt
Type.
Brief description of the drawings
The nonlimiting examples that the present invention can be provided by accompanying drawing are further illustrated；
Fig. 1 reflects four kinds of compound gel balls of calcium alginate in the present invention to Pb2+Adsorption effect with adsorption time
Change curve；
Fig. 2 reflects four kinds of compound gel balls of copper alginate in the present invention to Pb2+Adsorption effect with adsorption time
Change curve；
Fig. 3 reflects four kinds of compound gel balls of alginic acid zinc in the present invention to Pb2+Adsorption effect with adsorption time
Change curve；
Fig. 4 reflects four kinds of compound gel balls of ferric alginate in the present invention to Pb2+Adsorption effect with adsorption time
Change curve；
Fig. 5 reflects the alginate ball of different metal ions substitution in the present invention to Pb2+Adsorption effect with suction
The change curve of attached time；
Fig. 6, which is reflected, adds the different alginate compound gel balls of 4A molecular sieves to Pb in the present invention2+Absorption effect
Really with the change curve of adsorption time；
Fig. 7 reflects four kinds of compound gel balls of calcium alginate in the present invention to Hg2+Adsorption effect with adsorption time
Change curve；
Fig. 8 reflects four kinds of compound gel balls of copper alginate in the present invention to Hg2+Adsorption effect with adsorption time
Change curve；
Fig. 9 reflects four kinds of compound gel balls of alginic acid zinc in the present invention to Hg2+Adsorption effect with adsorption time
Change curve；
Figure 10 reflects four kinds of compound gel balls of ferric alginate in the present invention to Hg2+Adsorption effect with adsorption time
Change curve；
Figure 11, which is reflected, reflects SA-Ca-PEO-AC, SA-Cu-PEO-4AZ, SA-Zn-PEO-4AZ, SA- in the present invention
Fe-PEO-AC alginate compound gel balls are to Hg2+Adsorption effect with adsorption time change curve；
Embodiment
In order that the present invention may be better understood in those skilled in the art, with reference to the accompanying drawings and examples to this hair
Bright technical scheme is further illustrated.
The preparation method of the alginate plural gel of the present invention is as follows：
The preparation of alginate ball：The sodium alginate for taking 5mL~10mL mass concentrations to be 2%, is stirred continuously down and divides
It is added drop-wise to the CaCl that 20mL~30mL concentration is 0.5mol/L~1mol/L other uniform speed slow2、CuCl2、ZnCl2、FeCl3It is molten
In liquid, drip off and stop stirring immediately, stand 2h~24h, obtain alginate ball SA-Ca, SA- of four kinds of different colours
Cu, SA-Zn, SA-Fe,；
The preparation of alginate-polyethylene glycol oxide plural gel ball：Take the alginic acid that 5mL~10mL mass concentrations are 2%
The polyethylene glycol oxide that sodium, 2mL~10mL mass concentrations are 0.1%, which is placed in magnetic stirring apparatus, to stir, and delays respectively under stirring
It is slow to be added to the CaCl that 20mL~30mL concentration is 0.5mol/L~1mol/L2、CuCl2、ZnCl2、FeCl3In solution, drip off vertical
Stop stirring, stand 2h~24h, obtain alginate plural gel ball SA-Ca-PEO, SA-Cu- of four kinds of different colours
PEO、SA-Zn-PEO、SA-Fe-PEO；
The preparation of alginate-polyethylene glycol oxide -4A molecular sieve plural gel balls：It is 2% to take 5mL~10mL mass concentrations
Sodium alginate, 2mL~10mL mass concentrations for 0.1% polyethylene glycol oxide and 0.05g~0.2g 4A molecular sieves be placed in magnetic force
Stirred in agitator, the CaCl that 20mL~30mL concentration is 0.5mol/L~1mol/L is respectively added slowly under stirring2、
CuCl2、ZnCl2、FeCl3In solution, drip off and stop stirring immediately, stand 2h~24h, obtain the alginic acid of four kinds of different colours
Salt plural gel ball SA-Ca-PEO-4AZ, SA-Cu-PEO-4AZ, SA-Zn-PEO-4AZ, SA-Fe-PEO-4AZ；
The preparation of alginate-polyethylene glycol oxide-activated carbon plural gel ball：It is 2% to take 5mL~10mL mass concentrations
Sodium alginate, 2mL~10mL mass concentrations are placed in magnetic agitation for 0.1% polyethylene glycol oxide and 0.05g~0.2g activated carbons
Stirred in device, the CaCl that 20mL~30mL concentration is 0.5mol/L~1mol/L is respectively added slowly under stirring2、
CuCl2、ZnCl2、FeCl3In solution, drip off and stop stirring immediately, stand 2h~24h, obtain the alginic acid of four kinds of different colours
Salt plural gel ball SA-Ca-PEO-AC, SA-Cu-PEO-AC, SA-Zn-PEO-AC, SA-Fe-PEO-AC.
Specific embodiment is as follows：
Alginate plural gel prepares embodiment one
The preparation of alginate ball：The sodium alginate for taking 5mL mass concentrations to be 2%, is stirred continuously lower difference at the uniform velocity
Slowly it is added drop-wise to the CaCl that 20mL concentration is 0.5mol/L2、CuCl2、ZnCl2、FeCl3In solution, drip off and stop stirring immediately
Mix, stand 2h, obtain alginate ball SA-Ca, SA-Cu, SA-Zn, SA-Fe of four kinds of different colours,；
The preparation of alginate-polyethylene glycol oxide plural gel ball：Take sodium alginate, 2mL that 5mL mass concentrations are 2%
The polyethylene glycol oxide that mass concentration is 0.1%, which is placed in magnetic stirring apparatus, to be stirred, and 20mL is respectively added slowly under stirring
Concentration is 0.5mol/L CaCl2、CuCl2、ZnCl2、FeCl3In solution, drip off and stop stirring immediately, stand 2h, obtain four kinds
Alginate plural gel ball SA-Ca-PEO, SA-Cu-PEO, SA-Zn-PEO, SA-Fe-PEO of different colours；
The preparation of alginate-polyethylene glycol oxide -4A molecular sieve plural gel balls：Take the marine alga that 5mL mass concentrations are 2%
Sour sodium, 2mL mass concentrations are placed in magnetic stirring apparatus and stirred for 0.1% polyethylene glycol oxide and 0.05g4A molecular sieves, stir
Mix down the CaCl for being respectively added slowly to that 20mL concentration is 0.5mol/L2、CuCl2、ZnCl2、FeCl3In solution, drip off and stop immediately
Only stir, stand 2h, obtain alginate plural gel ball SA-Ca-PEO-4AZ, SA-Cu-PEO- of four kinds of different colours
4AZ、SA-Zn-PEO-4AZ、SA-Fe-PEO-4AZ；
The preparation of alginate-polyethylene glycol oxide-activated carbon plural gel ball：Take the alginic acid that 5mL mass concentrations are 2%
Sodium, 2mL mass concentrations are placed in magnetic stirring apparatus and stirred for 0.1% polyethylene glycol oxide and 0.05g activated carbons, under stirring
It is respectively added slowly to the CaCl that 20mL concentration is 0.5mol/L2、CuCl2、ZnCl2、FeCl3In solution, drip off and stop stirring immediately
Mix, stand 2h, obtain alginate plural gel ball SA-Ca-PEO-AC, SA-Cu-PEO-AC, SA- of four kinds of different colours
Zn-PEO-AC、SA-Fe-PEO-AC。
Alginate plural gel prepares embodiment two
The preparation of alginate ball：The sodium alginate for taking 10mL mass concentrations to be 2%, is stirred continuously lower difference at the uniform velocity
Slowly it is added drop-wise to the CaCl that 30mL concentration is 1.0mol/L2、CuCl2、ZnCl2、FeCl3In solution, drip off and stop stirring immediately
Mix, stand 24h, obtain alginate ball SA-Ca, SA-Cu, SA-Zn, SA-Fe of four kinds of different colours,；
The preparation of alginate-polyethylene glycol oxide plural gel ball：Take 10mL mass concentrations be 2% sodium alginate,
The polyethylene glycol oxide that 10mL mass concentrations are 0.1%, which is placed in magnetic stirring apparatus, to stir, and is respectively added slowly under stirring
30mL concentration is 1.0mol/L CaCl2、CuCl2、ZnCl2、FeCl3In solution, drip off and stop stirring immediately, stand 24h, obtain
To alginate plural gel ball SA-Ca-PEO, SA-Cu-PEO, SA-Zn-PEO, SA-Fe-PEO of four kinds of different colours；
The preparation of alginate-polyethylene glycol oxide -4A molecular sieve plural gel balls：Take the sea that 10mL mass concentrations are 2%
Mosanom, 10mL mass concentrations are that 0.1% polyethylene glycol oxide and 0.2g 4A molecular sieves are placed in magnetic stirring apparatus and stir equal
It is even, the CaCl that 30mL concentration is 1.0mol/L is respectively added slowly under stirring2、CuCl2、ZnCl2、FeCl3In solution, drip off
Stop stirring immediately, stand 24h, obtain alginate plural gel ball SA-Ca-PEO-4AZ, SA-Cu- of four kinds of different colours
PEO-4AZ、SA-Zn-PEO-4AZ、SA-Fe-PEO-4AZ；
The preparation of alginate-polyethylene glycol oxide-activated carbon plural gel ball：Take the marine alga that 10mL mass concentrations are 2%
Sour sodium, 10mL mass concentrations are placed in magnetic stirring apparatus and stirred for 0.1% polyethylene glycol oxide and 0.2g activated carbons, stir
Under be respectively added slowly to 30mL concentration be 1.0mol/L CaCl2、CuCl2、ZnCl2、FeCl3In solution, drip off and stop immediately
Stirring, stands 24h, obtain the alginate plural gel ball SA-Ca-PEO-AC of four kinds of different colours, SA-Cu-PEO-AC,
SA-Zn-PEO-AC、SA-Fe-PEO-AC。
Alginate plural gel prepares embodiment three
The preparation of alginate ball：The sodium alginate for taking 8mL mass concentrations to be 2%, is stirred continuously lower difference at the uniform velocity
Slowly it is added drop-wise to the CaCl that 25mL concentration is 0.8mol/L2、CuCl2、ZnCl2、FeCl3In solution, drip off and stop stirring immediately
Mix, stand 12h, obtain alginate ball SA-Ca, SA-Cu, SA-Zn, SA-Fe of four kinds of different colours,；
The preparation of alginate-polyethylene glycol oxide plural gel ball：Take sodium alginate, 5mL that 8mL mass concentrations are 2%
The polyethylene glycol oxide that mass concentration is 0.1%, which is placed in magnetic stirring apparatus, to be stirred, and 25mL is respectively added slowly under stirring
Concentration is 0.8mol/L CaCl2、CuCl2、ZnCl2、FeCl3In solution, drip off and stop stirring immediately, stand 12h, obtain four
Plant alginate plural gel ball SA-Ca-PEO, SA-Cu-PEO, SA-Zn-PEO, SA-Fe-PEO of different colours；
The preparation of alginate-polyethylene glycol oxide -4A molecular sieve plural gel balls：Take the marine alga that 8mL mass concentrations are 2%
Sour sodium, 5mL mass concentrations are placed in magnetic stirring apparatus and stirred for 0.1% polyethylene glycol oxide and 0.1g 4A molecular sieves, stir
Mix down the CaCl for being respectively added slowly to that 25mL concentration is 0.8mol/L2、CuCl2、ZnCl2、FeCl3In solution, drip off and stop immediately
Only stir, stand 12h, obtain alginate plural gel ball SA-Ca-PEO-4AZ, SA-Cu-PEO- of four kinds of different colours
4AZ、SA-Zn-PEO-4AZ、SA-Fe-PEO-4AZ；
The preparation of alginate-polyethylene glycol oxide-activated carbon plural gel ball：Take the alginic acid that 8mL mass concentrations are 2%
Sodium, 5mL mass concentrations are placed in magnetic stirring apparatus and stirred for 0.1% polyethylene glycol oxide and 0.1g activated carbons, under stirring
It is respectively added slowly to the CaCl that 25mL concentration is 0.8mol/L2、CuCl2、ZnCl2、FeCl3In solution, drip off and stop stirring immediately
Mix, stand 12h, obtain alginate plural gel ball SA-Ca-PEO-AC, SA-Cu-PEO-AC, SA- of four kinds of different colours
Zn-PEO-AC、SA-Fe-PEO-AC。
The alginate plural gel of the present invention is applied to that the mercury in water can be adsorbed in the processing of heavy metal ion in water
Ion and lead ion, before use, taking out alginate plural gel deionized water rinsing 3~5 times, and drain surface moisture content
Afterwards, then with the water containing heavy metal ion progress is mixed heavy metal ion adsorbed.Prepared and implemented with alginate plural gel below
Each alginate plural gel that example three is prepared is sample, is applied to the processing of heavy metal ion in water, specifically should
It is as follows with embodiment：
First, Application Example one of the alginate plural gel to heavy metal lead ion processing in water
Gel ball is taken out, with deionized water rinsing 3~5 times, the moisture of bead surface is blotted with filter paper, marine alga is weighed respectively
Each 4g of each gel ball that hydrochlorate plural gel preparation embodiment three is prepared is placed in the Pb (NO that 80mL concentration is 20mg/L3)2It is molten
In liquid.It is respectively respectively to draw 1.5mL absorption at 5min, 15min, 20min, 30min, 60min and 90min time point in adsorption time
Solution afterwards determines Pb with atomic absorption spectrophotometer immediately as detection sample2+Content.Because industrial wastewater is general
In acidity, and acidity is too low can cause the decomposition of alginate ball, therefore this experiment is by Pb (NO3)2The pH of solution is adjusted 4
Between~6.
Analysis of test results is as follows：
1. calcium alginate compounded thing gel ball is to Pb2+Absorption property analysis
Fig. 1 reflects four kinds of compound gel balls of calcium alginate to Pb2+Adsorption effect it is bent with the change of adsorption time
Line, the data shown from Fig. 1：
Four kinds of calcium alginate compounded thing gel ball SA-Ca, SA-Ca-PEO, SA-Ca-PEO-4AZ, SA-Ca-PEO-AC couple
Pb2+There is very strong absorption property, its adsorption efficiency can reach more than 98%, balance is basically reached after absorption 30min.
Four kinds of gel balls are to Pb2+The rate of adsorption and adsorption capacity differ smaller, still, the gel ball after addition 4A molecular sieves
The rate of adsorption is significantly improved, its adsorption capacity be 99.1%, its reason be probably exist inside 4A molecular sieves it is substantial amounts of
Uniform microcellular structure, and with substantial amounts of basic activated site (Na+), it can effectively fix and exchange Pb2+, thus it is right
Pb2+Adsorption effect it is best.And PEO macromolecular chain is mutually wound, although SA can be wrapped up to prevent it from hydrolyzing, but can only
Mesoporous and macroporous structure is formed, the raising influence of the adsorption effect of heavy metal ion is little.To Pb in activated carbon2+Absorption is played to make
Although micropore ratio can reach 80% or so, compared with molecular sieve, do not have basic activated site in AC, thus
Pb can not effectively be fixed2+.Thus, it can be known that for Pb2+Absorption and ion exchange process in, it plays ion exchange
Main component be calcium alginate, addition PEO and activated carbon to Pb2+The raising contribution of adsorption capacity is smaller.
2. copper alginate compound gel ball is to Pb2+Absorption property analysis
Fig. 2 reflects four kinds of compound gel balls of copper alginate to Pb2+Adsorption effect it is bent with the change of adsorption time
Line, the data shown from Fig. 2：
Four kinds of copper alginate compound gel balls SA-Cu, SA-Cu-PEO, SA-Cu-PEO-4AZ, SA-Cu-PEO-AC couple
Pb2+Absorption adsorption time be 30min when reach adsorption equilibrium, more than 80% is reached to the clearance of lead ion.Its
Middle SA-Cu-PEO-4AZ has the optimal rate of adsorption and adsorption capacity, has reached that absorption is flat when adsorption time is 15min
Weighing apparatus, the clearance to lead ion is 98.6%.From the point of view of the rate of adsorption, each gel ball is to Pb under experimental conditions2+Absorption effect
Sequentially it is really：SA-Cu-PEO-4AZ>SA-Cu>SA-Cu-PEO>SA-Cu-PEO-AC.It is worth noting that, adding in SA-Ca
Plus after PEO and activated carbon, for Cu2+Clearance declined on the contrary.Its reason is probably for Pb2+Absorption and
In ion exchange process, because PEO molecular weight is too big, cause rigidity excessive, with SA copolymerization not exclusively, and produce less Jie
Porosity, the raising for adsorption capacity is limited.Although the micropore in activated carbon can be with physical absorption Pb2+, but be due to desorption speed
Degree is too fast, and chemical bond (ionic bond) stabilization that physisorption power is produced not as ion exchange, on the contrary due to activated carbon
Grain occupies the segment space of marine alga acid group, causes on apparent for Pb2+Clearance declined.
3. alginic acid zinc complexes gel ball is to Pb2+Absorption property analysis
Fig. 3 reflects four kinds of compound gel balls of alginic acid zinc to Pb2+Adsorption effect it is bent with the change of adsorption time
Line, the data shown from Fig. 3：
Four kinds of alginic acid zinc complexes gel balls SA-Zn, SA-Zn-PEO, SA-Zn-PEO-4AZ, SA-Zn-PEO-AC couple
Pb2+Absorption peak is reached to the clearance of lead ion when adsorption time is 30min.Each gel ball is to Pb2+Absorption effect
Sequentially it is really：SA-Zn-PEO-4AZ>SA-Zn-PEO>SA-Zn>SA-Zn-PEO-AC.Each gel ball is to Pb2+Adsorption capacity become
Change trend is with copper alginate compound gel ball to Pb2+Adsorption capacity change it is consistent.
4. ferric alginate compound gel ball is to Pb2+Absorption property analysis
Fig. 4 reflects four kinds of compound gel balls of ferric alginate to Pb2+Adsorption effect it is bent with the change of adsorption time
Line, the data shown from Fig. 4：
Four kinds of alginic acid zinc complexes gel balls SA-Fe, SA-Fe-PEO, SA-Fe-PEO-4AZ, SA-Fe-PEO-AC couple
Pb2+The adsorption efficiency of absorption, which is increased over time, constantly to be increased, and adsorption equilibrium is basically reached in 60min.This be because
With the increase of adsorption time, to adsorb the Pb in gel ball surface2+Constantly enter the inside of gel ball, gel ball surface
Adsorption site can proceed again absorption, therefore, over time constantly increase and decrease, gel ball is to Pb2+Clearance not yet
Increase disconnectedly.Each gel ball is to Pb2+Adsorption effect order be：SA-Zn-PEO-4AZ>SA-Zn-PEO>SA-Zn>SA-Zn-
PEO-AC.Each gel ball is to Pb2+Adsorption capacity variation tendency and copper alginate compound gel ball and alginic acid zinc complexes
Gel ball is to Pb2+Adsorption capacity change it is consistent.
5. four kinds of alginate compound gel balls are to Pb2+Absorption property compare
Fig. 5 reflects the alginate ball of different metal ions substitution to Pb2+Adsorption effect with adsorption time
Change curve, Fig. 6 reflects the different alginate compound gel balls of addition 4A molecular sieves to Pb2+Adsorption effect with absorption
The change curve of time, the data shown from Fig. 5 and Fig. 6：
In the case of other conditions identical, each alginate and its compound have very big to the adsorption effect of lead ion
Difference.As shown in figure 5, each gel ball is to Pb2+The rate of adsorption order be：SA-Cu>SA-Ca>SA-Zn>SA-Fe, adsorption capacity
Sequentially it is：SA-Ca>SA-Cu>SA-Zn>SA-Fe.In addition, in four kinds of alginate compound gel balls, to Pb2+Absorption effect
Really optimal is compound 4A molecular sieves in gel ball material.As shown in fig. 6, each gel ball is to Pb2+The rate of adsorption order be：
SA-Cu-PEO-4AZ>SA-Ca-PEO-4AZ>SA-Zn-PEO-4AZ>SA-Fe-PEO-4AZ, adsorption capacity order be：SA-Ca-
PEO-4AZ>SA-Cu-PEO-4AZ>SA-Zn-PEO-4AZ>SA-Fe-PEO-4AZ。
Analysis is understood above, and 4A molecular sieves are added in alginate ball can increase substantially for Pb2+Suction
Attached ability, and activated carbon is added for Pb2+The raising of adsorption capacity do not contribute substantially but.
2nd, the Application Example two that alginate plural gel is handled metal mercury ions in water
Gel ball is taken out, with deionized water rinsing 3~5 times, the moisture of bead surface is blotted with filter paper, marine alga is weighed respectively
Each 1g of each gel ball that hydrochlorate plural gel preparation embodiment three is prepared is placed in the Hg (NO that 100mL concentration is 50 μ g/L3)2
In solution.It is respectively respectively to draw 1mL absorption at 5min, 15min, 20min, 30min, 60min and 90min time point in adsorption time
Solution afterwards determines Hg with cold-atomic fluorescence mercury meter immediately as detection sample2+Content.Equally, it is simulation industrial wastewater
Acidity, by Hg (NO3)2The pH of adsorption liquid is adjusted between 4~6.
Analysis of test results is as follows：
1. calcium alginate compounded thing gel ball is to Hg2+Absorption property analysis
Fig. 7 reflects calcium alginate compounded thing gel ball to the change curve of the adsorption effect of mercury ion with adsorption time,
The data shown from Fig. 7：
Four kinds of calcium alginate compounded thing gel ball SA-Ca, SA-Ca-PEO, SA-Ca-PEO-4AZ, SA-Ca-PEO-AC couple
Hg2+There is preferable adsorption effect, and adsorption rate can reach more than 58% after 30min.Wherein SA-Ca-PEO-AC's
The rate of adsorption and adsorption capacity are maximum, and SA-PEO adsorption efficiencies are worst.Four kinds of gel balls are to Hg2+Adsorption effect order be：SA-
Ca-PEO-AC>SA-Ca-PEO-4AZ>SA-Ca>SA-Ca-PEO.For Hg2+Adsorption process in, activated carbon and 4A molecules
Micropore in sieve is to Hg2+Physical absorption serve important function, and this effect may be more than Ca2+With Hg2+Ion hand over
Change.And the specific surface area of activated carbon is more much larger than 4A molecular sieve, with more micropores.And it is mesoporous and big in PEO strands
Hole is for Hg2+Absorption may not contribute, simply play a part of fixed calcium alginate.
2. copper alginate compound gel ball is to Hg2+Absorption property analysis
Fig. 8 reflects four kinds of compound gel balls of copper alginate to Hg2+Adsorption effect it is bent with the change of adsorption time
Line, the data shown from Fig. 8：
Four kinds of copper alginate compound gel balls SA-Cu, SA-Cu-PEO, SA-Cu-PEO-4AZ, SA-Cu-PEO-AC couple
Hg2+There is preferable adsorption effect, wherein, adsorption capacity maximum is SA-Cu-PEO-4AZ, next to that SA-Cu-PEO-AC,
It is SA-Cu-PEO again, that worst is SA-Cu.When adsorption time is 60min, SA-Cu-PEO-4AZ clearance is up to
It is only 76% that 87%, SA-Cu-PEO-AC, which is 85%, SA-Cu-PEO to the maximum to be 78%, SA-Cu to the maximum,.Copper alginate for
Hg2+Ion exchange power occupy prior effect, thus SA-Cu- than the physisorption power of micropore in additive
PEO-4AZ is than SA-Cu-PEO-AC for Hg2+Clearance it is higher.In addition, the hydroxyl in PEO molecules can be with Hg2+Generate network
Compound, so that the absorption property of copper alginate slightly has raising.
3. alginic acid zinc complexes gel ball is to Hg2+Absorption property analysis
Fig. 9 reflects four kinds of compound gel balls of alginic acid zinc to Hg2+Adsorption effect it is bent with the change of adsorption time
Line, the data shown from Fig. 9：
Alginic acid zinc complexes gel ball is for Hg2+The rate of adsorption it is very fast, reaction 20min is that can reach adsorption equilibrium.
Four kinds of absorption bead adsorption capacities it is maximum be SA-Zn-PEO-4AZ, next to that SA-Zn-PEO, followed by SA-Zn-PEO-AC,
That worst is SA-Zn.Four kinds of compound gel balls of alginic acid zinc are larger to the clearance difference of mercury ion.Adsorb flat when reaching
During weighing apparatus, the SA-Zn-PEO-4AZ rate of adsorption and adsorption capacity is maximum, is 74.26%.
4. ferric alginate compound gel ball is to Hg2+Absorption property analysis
Figure 10 reflects four kinds of compound gel balls of ferric alginate to Hg2+Adsorption effect it is bent with the change of adsorption time
Line, the data shown from Figure 10：
Four kinds of ferric alginate compound gel balls SA-Fe, SA-Fe-PEO, SA-Fe-PEO-4AZ, SA-Fe-PEO-AC couple
Hg2+Absorption reach adsorption equilibrium when adsorption time is 30min, four kinds of bead adsorption effects most preferably SA-Fe-PEO-
AC, next to that SA-Fe-PEO-4AZ, is SA-Fe again, that worst is SA-Fe-PEO.Wherein SA-Fe-PEO-AC clearance
It is only 62.3% to be up to 80%, SA-Fe-PEO-4AZ to be 76%, SA-Fe to the maximum to be 67.4%, SA-Fe-PEO to the maximum.
5. four kinds of alginate compound gel balls are to Hg2+Absorption property compare
Under the same conditions, we will be extracted for Hg in all kinds of alginate compound gel balls2+Adsorption effect
Best sample, such as Figure 11 reflect SA-Ca-PEO-AC, SA-Cu-PEO-4AZ, SA-Zn-PEO-4AZ, SA-Fe-PEO-AC
Alginate compound gel ball is to Hg2+Adsorption effect with the change curve of adsorption time, the data shown from Figure 11：
Each gel ball is to Hg2+The rate of adsorption order be：SA-Cu-PEO-4AZ>SA-Fe-PEO-AC>SA-Ca-PEO-AC
>SA-Zn-PEO-4AZ, adsorption capacity order be：SA-Zn-PEO-4AZ>SA-Ca-PEO-AC>SA-Fe-PEO-AC>SA-Cu-
PEO-4AZ, the two order is just the opposite.
More than analysis understand, added in alginate ball 4A molecular sieves or activated carbon can increase substantially for
Hg2+Adsorption capacity.Each marine alga acid metal salt and its compound are for Hg2+Absorption-ion exchange mechanism compare Pb2+'s
Absorption is increasingly complex, is the process of the mutual containing of the ion exchange of physical absorption and alginate of micropore in additive.
The above embodiments are merely illustrative of the technical solutions of the present invention and it is unrestricted, although with reference to preferred embodiment to this hair
It is bright to be described in detail, it will be understood by those within the art that, technical scheme can be modified
Or equivalent substitution, without departing from the objective and scope of technical solution of the present invention, it all should cover the claim in the present invention
Among scope.The technology of the invention not being described in detail, shape, construction part are known technology.
Claims (9)
1. the preparation method of alginate plural gel, it is characterised in that specific preparation method is as follows：
The preparation of alginate ball：5mL~10mL sodium alginates are taken, are added drop-wise to being stirred continuously lower uniform speed slow respectively
20mL~30mL CaCl2、CuCl2、ZnCl2、FeCl3In solution, drip off and stop stirring immediately, stand 2h~24h, obtain four
Plant alginate ball SA-Ca, SA-Cu, SA-Zn, SA-Fe of different colours；
The preparation of alginate-polyethylene glycol oxide plural gel ball：Take 5mL~10mL sodium alginates, 2mL~10mL polyoxyethylenes
Alkene is placed in magnetic stirring apparatus and stirred, and 20mL~30mL CaCl is respectively added slowly under stirring2、CuCl2、ZnCl2、
FeCl3In solution, drip off and stop stirring immediately, stand 2h~24h, obtain the alginate plural gel ball of four kinds of different colours
SA-Ca-PEO、SA-Cu-PEO、SA-Zn-PEO、SA-Fe-PEO；
The preparation of alginate-polyethylene glycol oxide -4A molecular sieve plural gel balls：Take 5mL~10mL sodium alginates, 2mL~
10mL polyethylene glycol oxides and 0.05g~0.2g4A molecular sieves are placed in magnetic stirring apparatus and stirred, and stirring is lower slowly to be added respectively
Enter the CaCl to 20mL~30mL2、CuCl2、ZnCl2、FeCl3In solution, drip off and stop stirring immediately, stand 2h~24h, obtain
To the alginate plural gel ball SA-Ca-PEO-4AZ of four kinds of different colours, SA-Cu-PEO-4AZ, SA-Zn-PEO-4AZ,
SA-Fe-PEO-4AZ；
The preparation of alginate-polyethylene glycol oxide-activated carbon plural gel ball：Take 5mL~10mL sodium alginates, 2mL~10mL
Polyethylene glycol oxide and 0.05g~0.2g activated carbons are placed in magnetic stirring apparatus and stirred, and are respectively added slowly under stirring
20mL~30mL CaCl2、CuCl2、ZnCl2、FeCl3In solution, drip off and stop stirring immediately, stand 2h~24h, obtain four
Plant alginate plural gel ball SA-Ca-PEO-AC, SA-Cu-PEO-AC, SA-Zn-PEO-AC, SA-Fe- of different colours
PEO-AC。
2. the preparation method of alginate plural gel according to claim 1, it is characterised in that the sodium alginate
Mass concentration is 2%.
3. the preparation method of alginate plural gel according to claim 2, it is characterised in that the polyethylene glycol oxide
Mass concentration be 0.1%.
4. the preparation method of alginate plural gel according to claim 3, it is characterised in that the CaCl2Solution,
CuCl2Solution, ZnCl2Solution, FeCl3The concentration of solution is 0.5mol/L~1mol/L.
5. application of the alginate plural gel according to claim 4 to heavy mental treatment in water, its feature exists
In the alginate plural gel is applied to that in water process heavy metal lead ion and the mercury ion in water can be adsorbed.
6. application of the alginate plural gel according to claim 5 to heavy mental treatment in water, its feature exists
In, the alginate plural gel using preceding needing with deionized water rinsing 3~5 times, and drain after the moisture content of surface, then with containing
The water mixing of heavy metal ion carries out heavy metal ion adsorbed.
7. application of the alginate plural gel according to claim 6 to heavy mental treatment in water, its feature exists
In SA-Ca, SA-Ca-PEO, SA-Ca-PEO-4AZ, SA-Ca-PEO-AC gel is to the adsorption rate of lead ion 98%
More than.
8. application of the alginate plural gel according to claim 6 to heavy mental treatment in water, its feature exists
In the alginate plural gel SA-Ca-PEO-4AZ is 99.1% to the adsorption capacity of lead ion in water.
9. application of the alginate plural gel according to claim 6 to heavy mental treatment in water, its feature exists
In, the alginate plural gel SA-Cu-PEO-4AZ to the adsorption capacity of mercury ion in water up to 87%, the alginate
Plural gel SA-Cu-PEO-AC is to the adsorption capacity of mercury ion in water up to 85%.
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| CN109351350A (en) * | 2018-12-27 | 2019-02-19 | 安徽工业大学 | A kind of method that emulsion polymerization prepares sodium alginate micro ball adsorbent |
| CN112645403A (en) * | 2020-10-14 | 2021-04-13 | 南昌航空大学 | Underground water heavy metal treatment system and method based on porous polymer |
| CN113248321A (en) * | 2021-05-19 | 2021-08-13 | 东华大学 | Preparation method of light-operated slow-release fulvic acid fertilizer capable of repairing heavy metals |
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| CN108514867A (en) * | 2018-04-18 | 2018-09-11 | 北京化工大学 | A kind of preparation of the sodium alginate gel ball of detection formaldehyde |
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| CN108940219A (en) * | 2018-07-12 | 2018-12-07 | 浙江正洁环境科技有限公司 | A kind of anti-acid heavy metal absorbent and preparation method thereof |
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| CN112645403A (en) * | 2020-10-14 | 2021-04-13 | 南昌航空大学 | Underground water heavy metal treatment system and method based on porous polymer |
| CN113248321A (en) * | 2021-05-19 | 2021-08-13 | 东华大学 | Preparation method of light-operated slow-release fulvic acid fertilizer capable of repairing heavy metals |
| CN115193398A (en) * | 2022-05-16 | 2022-10-18 | 王之风 | Modified coconut shell carbon gel ball for adsorbing heavy metal ions |
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