CN106807334A - A kind of preparation method and applications of heavy metal ion adsorbing material - Google Patents
A kind of preparation method and applications of heavy metal ion adsorbing material Download PDFInfo
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- CN106807334A CN106807334A CN201710062889.XA CN201710062889A CN106807334A CN 106807334 A CN106807334 A CN 106807334A CN 201710062889 A CN201710062889 A CN 201710062889A CN 106807334 A CN106807334 A CN 106807334A
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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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- 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
- B01J20/28—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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- 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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
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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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention discloses a kind of preparation method and applications of heavy metal ion adsorbing material, by with percolate as raw material, by it with cigarette stalk in the cellulose that extracts graft copolymerization is carried out to produce percolate tobacco stalk fiber element compound, and by percolate tobacco stalk fiber element compound carry out gelation treatment after, regenerated, percolate tobacco stalk fiber element base aeroge is obtained after exchange of solvent and vacuum drying, obtained percolate tobacco stalk fiber element base aerogel material aperture is big, porosity is high, Stability Analysis of Structures, and there is excellent chelation to the heavy metal in waste water, adsorption efficiency and adsorbance, using percolate with low cost and cigarette stalk, the cost of heavy mental treatment can not only be reduced, the cycling and reutilization of resource can also greatly be realized, promote the protection of environment.
Description
Technical field
The present invention relates to heavy metal ion adsorbing material field, especially a kind of preparation side of heavy metal ion adsorbing material
Method and its application.
Background technology
With the fast development of industry, the wastewater discharge produced in industrial processes also increasingly increases, wherein containing
The industrial wastewater of heavy metal ion and organic dyestuff can cause the severe contamination of water body, jeopardized ecological environment and the mankind are strong
Health, therefore, the treatment to industrial wastewater has caused the great attention of numerous scientific workers.Usually said heavy metal pollution,
The significant element of the bio-toxicities such as lead, copper, mercury is primarily referred to as, the element with certain toxicity also including zinc, tin, cobalt etc., due to
Heavy metal and heavy metal compound are widely used in the industries such as chemical industry, plating, leather, with their applications constantly expansion, heavy metal
Pollution also increasingly increases, due to heavy metal it is difficult to be biodegradable, and with bioconcentration, therefore the pollution caused by it
With continuation, heavy metal in water has become one of environmental problem of most serious in the world today, on the other hand, with weaving
Printing and dyeing, papermaking and the development of printing industry, and people to color aspect the need for more and more higher, current organic dye waste water
Discharge capacity is continuously increased in the proportion of national every profession and trade, and dyestuff species constantly update and increase, its anti-light solution, it is anti-oxidant and
Antibiont degradation property constantly strengthens so that the intractability of dyestuff waste liquid is significantly lifted.
At present, the method for the treatment of industrial wastewater mainly has reducing process, absorption method and ion-exchange-resin process.These methods exist
Played an important role in treatment industrial wastewater, wherein, absorption method is because simple to operate, and removal efficiency is high, wide using scope, ready-made to be
Relatively reliable method for treating waste liquid.
Birdsed of the same feather flock together compound using the traditional synthesis of biomass portion or replacing whole, be near for repairing the pollutant in water body
One of focus of several years environmental science forward positions research, cellulose and sodium humate as natural polymer, in nature
In be widely distributed, and with good chemical adsorptivity, preferable recyclability, biodegradable, moisture-absorption water-retention is made
With；And in above-mentioned two family macromolecules chemical constitution contain great amount of hydroxy group, carboxylate groups and amino, can with the heavy metal in water from
There is suction-operated in son and organic dyestuff, meanwhile, these functional groups can also be crosslinked by chemical modification, form macromolecular
Network structure, can be prevented effectively from the shortcoming that sodium humate meets water dissolves, by cellulose and sodium humate both macromolecular materials
Advantage concentrate in together, so as to increase substantially the adsorption capacity of heavy metal ion.
Further, since the living standard of people is gradually stepped up now, the yield of municipal refuse also increasingly rises, in treatment
Substantial amounts of percolate can be produced during rubbish, due to containing substantial amounts of humic acid in percolate, by itself and agriculture
Crop cigarette stalk carries out production heavy metal absorbent as raw material, not only with low cost, additionally it is possible to realize the recycling of discarded object,
Secondary economic worth is realized, the cost and waste cycling and reutilization to reducing heavy metal treatment all have positive effect.
The content of the invention
In order to solve the deficiencies in the prior art, it is an object of the invention to provide a kind of with low cost, highly effective and safe, production
The preparation method and applications of the heavy metal ion adsorbing material of process is simple.
In order to realize above-mentioned technical purpose, the technical scheme is that：A kind of system of heavy metal ion adsorbing material
Preparation Method, with percolate as raw material, by the cellulose extracted in itself and cigarette stalk carry out graft copolymerization be obtained percolate-
Tobacco stalk fiber compound, after carrying out gelation to percolate-tobacco stalk fiber compound, then it is regenerated, it is molten
Agent exchange and supercritical carbon dioxide are dried, you can heavy metal ion is obtained has the percolate-tobacco rod of adsorptivity fine
The plain base aeroge of dimension.
Further, it is comprised the following steps：
(1) percolate filtered, after removal of impurities, its pH adjusted to 7~9, be subsequently adding coagulant, and utilize
After agitating device stirs 3~5min with 2000~3000rpm, then 10~15min is stirred with 500~650rpm, after the completion of stirring
Mixed solution is staticly settled, then sediment leach is configured to solution, and the solution ph of configuration is adjusted to 7~9；
(2) cigarette stalk is emedullated after core, crosses 14~20 mesh sieves after crushing, then by the cigarette stalk after sieving with by sodium hydrate solid
The mass fraction that grain dissolution is configured to is 2% sodium hydroxide solution mixing, and mixed solution is heated into 90~150 DEG C,
After carrying out 1~3h of reaction, the solid content in mixed solution is leached；
(3) 5~15min is discongested into the above-mentioned solid content Lampen mill for leaching, after again with toluene washing, adds it to first
4~6h of dipping is carried out in the mixed liquor of benzene and epoxychloropropane, after dipping is finished, solid content is leached again, and use second successively
Alcohol, distilled water are washed, untill being washed till cleaning solution in neutrality, you can tobacco stalk fiber element is obtained；
(4) tobacco stalk fiber element obtained above is added in solution obtained in step (1), and using ultrasonic equipment with
The power of 100~300W carries out 2~5h of assisted reaction, after the completion of reaction, solution is stood into 3~5h at normal temperatures, then by solution
In solid content leach, washed and impregnated with the sodium hydroxide solution that pH value is 9~11, until leachate is in colourless
Only, you can percolate-tobacco stalk fiber element compound is obtained；
(5) percolate obtained above-tobacco stalk fiber element compound is carried out into vacuum under conditions of 60~80 DEG C
After drying 24~48h, then percolate-tobacco stalk fiber element compound is added in ionic liquid, and at 65~85 DEG C
Under the conditions of, 1~3h of reaction is stirred with the mixing speed of 600~800rpm, after the completion of stirring, pour the mixture into shaping mould
In tool, and mould is placed in the ultra low temperature freezer that temperature is -75~-50 DEG C carries out 12~24h of freezen protective；
(6) mixture after step (5) freezen protective and shaping is taken out, and is washed to cleaning solution with deionized water
Untill being detected without precipitation with silver nitrate, then solvent displacement 3~6 times is carried out to the mixture after washing with non solvent liquid, then will
The mixture replaced by solvent carries out freeze-drying, you can be obtained heavy metal example have the percolate of adsorptivity-
Tobacco stalk fiber element base aeroge.
Preferably, the addO-on therapy and mass fraction of each step are as follows：
Preferably, described ionic liquid is 1- butyl -3- methylimidazole villaumites or 1- pi-allyl -3- methylimidazole chlorine
Salt.
Preferably, described coagulant is the polymer of molysite, aluminium salt or molysite and aluminium salt.
Preferably, the solution solid content for being configured using sediment in the step (1) is 40%~60%.
Preferably, in the step (5) by formed in mould mixture be radius 10mm, height 30mm cylinder.
Preferably, described non solvent liquid is the tert-butyl alcohol or acetone.
A kind of application of the heavy metal ion adsorbing material as obtained in above-mentioned preparation method, by heavy metal ion adsorbed material
It is heavy metal ion adsorbed in expecting for percolate.
Use above-mentioned technical scheme beneficial effects of the present invention for：By with percolate as raw material, by itself and cigarette
The cellulose extracted in stalk carries out graft copolymerization to produce percolate-tobacco stalk fiber element compound, and by percolate-
After tobacco stalk fiber element compound carries out gelation treatment, then regenerated, garbage filter is obtained after exchange of solvent and vacuum drying
Liquid-tobacco stalk fiber element base aeroge, obtained percolate-tobacco stalk fiber element base aerogel material aperture is big, porosity
High, Stability Analysis of Structures and there is excellent chelation, adsorption efficiency and adsorbance to the heavy metal in waste water, using cost
Cheap percolate and cigarette stalk, can not only reduce the cost of heavy mental treatment, additionally it is possible to greatly realize resource
Cycling and reutilization, promote environment protection.
Specific embodiment
A kind of preparation method of heavy metal ion adsorbing material, with percolate as raw material, by itself and extraction in cigarette stalk
Cellulose carry out graft copolymerization be obtained percolate-tobacco stalk fiber compound, by multiple to percolate-tobacco stalk fiber
After compound carries out gelation, then it is regenerated, exchange of solvent and supercritical carbon dioxide are dried, you can heavy metal is obtained
Ion has the percolate-cigarette pole fiber element base aeroge of adsorptivity.
Further, it is comprised the following steps：
(1) percolate filtered, after removal of impurities, its pH adjusted to 7~9, be subsequently adding coagulant, and utilize
After agitating device stirs 3~5min with 2000~3000rpm, then 10~15min is stirred with 500~650rpm, after the completion of stirring
Mixed solution is staticly settled, then sediment leach is configured to solution, and the solution ph of configuration is adjusted to 7~9；
(2) cigarette stalk is emedullated after core, crosses 14~20 mesh sieves after crushing, then by the cigarette stalk after sieving with by sodium hydrate solid
The mass fraction that grain dissolution is configured to is 2% sodium hydroxide solution mixing, and mixed solution is heated into 90~150 DEG C,
After carrying out 1~3h of reaction, the solid content in mixed solution is leached；
(3) 5~15min is discongested into the above-mentioned solid content Lampen mill for leaching, after again with toluene washing, adds it to first
4~6h of dipping is carried out in the mixed liquor of benzene and epoxychloropropane, after dipping is finished, solid content is leached again, and use second successively
Alcohol, distilled water are washed, untill being washed till cleaning solution in neutrality, you can tobacco stalk fiber element is obtained；
(4) tobacco stalk fiber element obtained above is added in solution obtained in step (1), and using ultrasonic equipment with
The power of 100~300W carries out 2~5h of assisted reaction, after the completion of reaction, solution is stood into 3~5h at normal temperatures, then by solution
In solid content leach, washed and impregnated with the sodium hydroxide solution that pH value is 9~11, until leachate is in colourless
Only, you can percolate-tobacco stalk fiber element compound is obtained；
(5) percolate obtained above-tobacco stalk fiber element compound is carried out into vacuum under conditions of 60~80 DEG C
After drying 24~48h, then percolate-tobacco stalk fiber element compound is added in ionic liquid, and at 65~85 DEG C
Under the conditions of, 1~3h of reaction is stirred with the mixing speed of 600~800rpm, after the completion of stirring, pour the mixture into shaping mould
In tool, and mould is placed in the ultra low temperature freezer that temperature is -75~-50 DEG C carries out 12~24h of freezen protective；
(6) mixture after step (5) freezen protective and shaping is taken out, and is washed to cleaning solution with deionized water
Untill being detected without precipitation with silver nitrate, then solvent displacement 3~6 times is carried out to the mixture after washing with non solvent liquid, then will
The mixture replaced by solvent carries out freeze-drying, you can be obtained heavy metal example have the percolate of adsorptivity-
Tobacco stalk fiber element base aeroge.
Preferably, the addO-on therapy and mass fraction of each step are as follows：
Preferably, described ionic liquid is 1- butyl -3- methylimidazole villaumites or 1- pi-allyl -3- methylimidazole chlorine
Salt.
Preferably, described coagulant is the polymer of molysite, aluminium salt or molysite and aluminium salt.
Preferably, the solution solid content for being configured using sediment in the step (1) is 40%~60%.
Preferably, in the step (5) by formed in mould mixture be radius 10mm, height 30mm cylinder.
Preferably, described non solvent liquid is the tert-butyl alcohol or acetone.
A kind of application of the heavy metal ion adsorbing material as obtained in above-mentioned preparation method, by heavy metal ion adsorbed material
It is heavy metal ion adsorbed in expecting for percolate.
Embodiment 1
A kind of preparation method of heavy metal ion adsorbing material, it is comprised the following steps：
(1) 26.97Kg is adjusted to 7 by the percolate pH after filtering, removal of impurities, is subsequently adding 0.03Kg tri-chlorinations
Iron, and using agitating device after stirring 3min under 2000rpm rotating speeds, then 10min is stirred with the rotating speed of 600rpm, stirring is completed
Mixed solution is staticly settled afterwards, then sediment leach the solution for being configured to that solid content is 58%, and by solution ph
Adjust to 7；
(2) 10Kg is emedullated the cigarette stalk after core, crosses 14 mesh sieves after crushing, then by the cigarette stalk after sieving with by 5Kg hydroxides
The mass fraction that the dissolving of sodium solid particle is configured to is 2% sodium hydroxide solution mixing, and mixed solution is heated into 90 DEG C,
After carrying out reaction 1h, the solid content in mixed solution is leached；
(3) 5min is discongested into the above-mentioned solid content Lampen mill for leaching, after again with toluene washing, adds it to by 15Kg
Dipping 4h is carried out in toluene and 5Kg epoxychloropropane mixed liquors, after dipping is finished, solid content is leached again, and use second successively
Alcohol, distilled water are washed, untill being washed till cleaning solution in neutrality, you can tobacco stalk fiber element is obtained；
(4) tobacco stalk fiber element obtained above is added in solution obtained in step (1), and using ultrasonic equipment with
The power of 100W carries out assisted reaction 2h, after the completion of reaction, solution is stood into 3h at normal temperatures, then the solid content in solution is filtered
Go out, washed and impregnated with the sodium hydroxide solution that pH value is 9, untill leachate is in colourless, you can prepared rubbish oozes
Filtrate-tobacco stalk fiber element compound；
(5) percolate obtained above-tobacco stalk fiber element compound is vacuum dried under conditions of 60 DEG C
After 24h, then percolate-tobacco stalk fiber element compound is added in 38Kg 1- butyl -3- methylimidazole villaumites, and
Under conditions of 65 DEG C, reaction 3h is stirred with the mixing speed of 600rpm, after the completion of stirring, pours the mixture into mould
In, and mould is placed in the ultra low temperature freezer that temperature is -75 DEG C carries out freezen protective 12h, it is shaped to radius 10mm, height
Spend the cylinder of 30mm；
(6) mixture after step (5) freezen protective and shaping is taken out, and is washed to cleaning solution with deionized water
Untill being detected without precipitation with silver nitrate, then solvent displacement 6 times is carried out to the mixture after washing with t-butanol solution, then will passed through
The mixture of solvent displacement carries out freeze-drying, you can heavy metal example is obtained has the percolate-cigarette stalk of adsorptivity
Cellulose base aeroge.
Embodiment 2
A kind of preparation method of heavy metal ion adsorbing material, it is comprised the following steps：
(1) 24Kg is adjusted to 8 by the percolate pH after filtering, removal of impurities, is subsequently adding 0.05Kg aluminum sulfate, and
After stirring 3min under 2100rpm rotating speeds using agitating device, then 10min is stirred with the rotating speed of 610rpm, will after the completion of stirring
Mixed solution is staticly settled, then sediment leach is configured to solid content and is 40% solution, and solution ph is adjusted
To 8；
(2) 10Kg is emedullated the cigarette stalk after core, crosses 14 mesh sieves after crushing, then by the cigarette stalk after sieving with by 5.95Kg hydrogen-oxygens
Change sodium solid particle and dissolve the sodium hydroxide solution mixing that the mass fraction being configured to is 2%, and mixed solution is heated to 100
DEG C, after carrying out reaction 5h, the solid content in mixed solution is leached；
(3) 10min is discongested into the above-mentioned solid content Lampen mill for leaching, after again with toluene washing, add it to by
Dipping 4h is carried out in 15Kg toluene and 5Kg epoxychloropropane mixed liquors, after dipping is finished, solid content is leached again, and successively
Washed with ethanol, distilled water, untill being washed till cleaning solution in neutrality, you can tobacco stalk fiber element is obtained；
(4) tobacco stalk fiber element obtained above is added in solution obtained in step (1), and using ultrasonic equipment with
The power of 250W carries out assisted reaction 4h, after the completion of reaction, solution is stood into 3h at normal temperatures, then the solid content in solution is filtered
Go out, washed and impregnated with the sodium hydroxide solution that pH value is 10, untill leachate is in colourless, you can prepared rubbish oozes
Filtrate-tobacco stalk fiber element compound；
(5) percolate obtained above-tobacco stalk fiber element compound is vacuum dried under conditions of 70 DEG C
After 36h, then percolate-tobacco stalk fiber element compound is added in 40Kg 1- pi-allyl -3- methylimidazole villaumites, and
Under conditions of 70 DEG C, reaction 2h is stirred with the mixing speed of 700rpm, after the completion of stirring, pours the mixture into shaping mould
In tool, and mould be placed in the ultra low temperature freezer that temperature is -70 DEG C carry out freezen protective 18h, be shaped to radius 10mm,
The cylinder of height 30mm；
(6) mixture after step (5) freezen protective and shaping is taken out, and is washed to cleaning solution with deionized water
Untill being detected without precipitation with silver nitrate, then solvent displacement 6 times is carried out to the mixture after washing with acetone soln, then will be by molten
The mixture of agent displacement carries out freeze-drying, you can heavy metal example is obtained has the percolate-cigarette stalk of adsorptivity fine
The plain base aeroge of dimension.
Embodiment 3
A kind of preparation method of heavy metal ion adsorbing material, it is comprised the following steps：
(1) 26Kg is adjusted to 8 by the percolate pH after filtering, removal of impurities, is subsequently adding 0.04Kg polyaluminiums
Aluminium, and using agitating device after stirring 5min under 2200rpm rotating speeds, then 12min is stirred with the rotating speed of 500rpm, stirring is completed
Mixed solution is staticly settled afterwards, then sediment leach the solution for being configured to that solid content is 40%, and by solution ph
Adjust to 9；
(2) 10.5Kg is emedullated the cigarette stalk after core, crosses 16 mesh sieves after crushing, then by the cigarette stalk after sieving with by 5.46Kg hydrogen
The mass fraction that the dissolving of sodium oxide molybdena solid particle is configured to is 2% sodium hydroxide solution mixing, and mixed solution is heated to
150 DEG C, after carrying out reaction 2h, the solid content in mixed solution is leached；
(3) 15min is discongested into the above-mentioned solid content Lampen mill for leaching, after again with toluene washing, add it to by
Dipping 6h is carried out in 18Kg toluene and 6Kg epoxychloropropane mixed liquors, after dipping is finished, solid content is leached again, and successively
Washed with ethanol, distilled water, untill being washed till cleaning solution in neutrality, you can tobacco stalk fiber element is obtained；
(4) tobacco stalk fiber element obtained above is added in solution obtained in step (1), and using ultrasonic equipment with
The power of 100W carries out assisted reaction 5h, after the completion of reaction, solution is stood into 4h at normal temperatures, then the solid content in solution is filtered
Go out, washed and impregnated with the sodium hydroxide solution that pH value is 11, untill leachate is in colourless, you can prepared rubbish oozes
Filtrate-tobacco stalk fiber element compound；
(5) percolate obtained above-tobacco stalk fiber element compound is vacuum dried under conditions of 80 DEG C
After 24h, then percolate-tobacco stalk fiber element compound is added in 34Kg 1- butyl -3- methylimidazole villaumites, and
Under conditions of 75 DEG C, reaction 1h is stirred with the mixing speed of 800rpm, after the completion of stirring, pours the mixture into mould
In, and mould is placed in the ultra low temperature freezer that temperature is -60 DEG C carries out freezen protective 28h, it is shaped to radius 10mm, height
Spend the cylinder of 30mm；
(6) mixture after step (5) freezen protective and shaping is taken out, and is washed to cleaning solution with deionized water
Untill being detected without precipitation with silver nitrate, then solvent displacement 5 times is carried out to the mixture after washing with acetone soln, then will be by molten
The mixture of agent displacement carries out freeze-drying, you can heavy metal example is obtained has the percolate-cigarette stalk of adsorptivity fine
The plain base aeroge of dimension.
Embodiment 4
A kind of preparation method of heavy metal ion adsorbing material, it is comprised the following steps：
(1) 28Kg is adjusted to 8 by the percolate pH after filtering, removal of impurities, is subsequently adding 0.03Kg ferric trichlorides,
And using agitating device after stirring 3min under 2300rpm rotating speeds, then 10min is stirred with the rotating speed of 630rpm, after the completion of stirring
Mixed solution is staticly settled, then sediment leach is configured to solid content and is 40% solution, and solution ph is adjusted
Save to 7；
(2) 12Kg is emedullated the cigarette stalk after core, crosses 14 mesh sieves after crushing, then by the cigarette stalk after sieving with by 5Kg hydroxides
The mass fraction that the dissolving of sodium solid particle is configured to is 2% sodium hydroxide solution mixing, and mixed solution is heated into 100
DEG C, after carrying out reaction 2h, the solid content in mixed solution is leached；
(3) 5min is discongested into the above-mentioned solid content Lampen mill for leaching, after again with toluene washing, add it to by
Dipping 4h is carried out in 15.3Kg toluene and 5.1Kg epoxychloropropane mixed liquors, after dipping is finished, solid content is leached again, and
Washed with ethanol, distilled water successively, untill being washed till cleaning solution in neutrality, you can tobacco stalk fiber element is obtained；
(4) tobacco stalk fiber element obtained above is added in solution obtained in step (1), and using ultrasonic equipment with
The power of 300W carries out assisted reaction 2h, after the completion of reaction, solution is stood into 3h at normal temperatures, then the solid content in solution is filtered
Go out, washed and impregnated with the sodium hydroxide solution that pH value is 9, untill leachate is in colourless, you can prepared rubbish oozes
Filtrate-tobacco stalk fiber element compound；
(5) percolate obtained above-tobacco stalk fiber element compound is vacuum dried under conditions of 75 DEG C
After 22h, then percolate-tobacco stalk fiber element compound is added in 34.57Kg 1- butyl -3- methylimidazole villaumites, and
Under conditions of 90 DEG C, reaction 2h is stirred with the mixing speed of 700rpm, after the completion of stirring, pours the mixture into shaping mould
In tool, and mould be placed in the ultra low temperature freezer that temperature is -55 DEG C carry out freezen protective 18h, be shaped to radius 10mm,
The cylinder of height 30mm；
(6) mixture after step (5) freezen protective and shaping is taken out, and is washed to cleaning solution with deionized water
Untill being detected without precipitation with silver nitrate, then solvent displacement 4 times is carried out to the mixture after washing with t-butanol solution, then will passed through
The mixture of solvent displacement carries out freeze-drying, you can heavy metal example is obtained has the percolate-cigarette stalk of adsorptivity
Cellulose base aeroge.
Embodiment 5
A kind of preparation method of heavy metal ion adsorbing material, it is comprised the following steps：
(1) 24Kg is adjusted to 9 by the percolate pH after filtering, removal of impurities, is subsequently adding 0.03Kg aluminum sulfate, and
After stirring 5min under 2400rpm rotating speeds using agitating device, then 15min is stirred with the rotating speed of 640rpm, will after the completion of stirring
Mixed solution is staticly settled, then sediment leach is configured to solid content and is 50% solution, and solution ph is adjusted
To 9；
(2) 15Kg is emedullated the cigarette stalk after core, crosses 20 mesh sieves after crushing, then by the cigarette stalk after sieving with by 6Kg hydroxides
The mass fraction that the dissolving of sodium solid particle is configured to is 2% sodium hydroxide solution mixing, and mixed solution is heated into 100
DEG C, after carrying out reaction 3h, the solid content in mixed solution is leached；
(3) 10min is discongested into the above-mentioned solid content Lampen mill for leaching, after again with toluene washing, add it to by
Dipping 6h is carried out in 15Kg toluene and 5Kg epoxychloropropane mixed liquors, after dipping is finished, solid content is leached again, and successively
Washed with ethanol, distilled water, untill being washed till cleaning solution in neutrality, you can tobacco stalk fiber element is obtained；
(4) tobacco stalk fiber element obtained above is added in solution obtained in step (1), and using ultrasonic equipment with
The power of 150W carries out assisted reaction 4h, after the completion of reaction, solution is stood into 5h at normal temperatures, then the solid content in solution is filtered
Go out, washed and impregnated with the sodium hydroxide solution that pH value is 10, untill leachate is in colourless, you can prepared rubbish oozes
Filtrate-tobacco stalk fiber element compound；
(5) percolate obtained above-tobacco stalk fiber element compound is vacuum dried under conditions of 80 DEG C
After 48h, then percolate-tobacco stalk fiber element compound is added in 34.97Kg 1- pi-allyl -3- methylimidazole villaumites,
And under conditions of 80 DEG C, reaction 1.5h is stirred with the mixing speed of 650rpm, after the completion of stirring, pour the mixture into
In pattern tool, and mould is placed in the ultra low temperature freezer that temperature is -50 DEG C carries out freezen protective 24h, be shaped to radius
The cylinder of 10mm, height 30mm；
(6) mixture after step (5) freezen protective and shaping is taken out, and is washed to cleaning solution with deionized water
Untill being detected without precipitation with silver nitrate, then solvent displacement 3 times is carried out to the mixture after washing with acetone soln, then will be by molten
The mixture of agent displacement carries out freeze-drying, you can heavy metal example is obtained has the percolate-cigarette stalk of adsorptivity fine
The plain base aeroge of dimension.
Embodiment 6
A kind of preparation method of heavy metal ion adsorbing material, it is comprised the following steps：
(1) 25Kg is adjusted to 8 by the percolate pH after filtering, removal of impurities, is subsequently adding 0.03Kg polyaluminiums
Aluminium, and using agitating device after stirring 3min under 2500rpm rotating speeds, then 10min is stirred with the rotating speed of 650rpm, stirring is completed
Mixed solution is staticly settled afterwards, then sediment leach the solution for being configured to that solid content is 40%, and by solution ph
Adjust to 7；
(2) 10Kg is emedullated the cigarette stalk after core, crosses 14 mesh sieves after crushing, then by the cigarette stalk after sieving with by 5.4Kg hydrogen-oxygens
Change sodium solid particle and dissolve the sodium hydroxide solution mixing that the mass fraction being configured to is 2%, and mixed solution is heated to 150
DEG C, after carrying out reaction 2h, the solid content in mixed solution is leached；
(3) 15min is discongested into the above-mentioned solid content Lampen mill for leaching, after again with toluene washing, add it to by
Dipping 6h is carried out in 18Kg toluene and 6Kg epoxychloropropane mixed liquors, after dipping is finished, solid content is leached again, and successively
Washed with ethanol, distilled water, untill being washed till cleaning solution in neutrality, you can tobacco stalk fiber element is obtained；
(4) tobacco stalk fiber element obtained above is added in solution obtained in step (1), and using ultrasonic equipment with
The power of 300W carries out assisted reaction 2h, after the completion of reaction, solution is stood into 3h at normal temperatures, then the solid content in solution is filtered
Go out, washed and impregnated with the sodium hydroxide solution that pH value is 10, untill leachate is in colourless, you can prepared rubbish oozes
Filtrate-tobacco stalk fiber element compound；
(5) percolate obtained above-tobacco stalk fiber element compound is vacuum dried under conditions of 70 DEG C
After 36h, then percolate-tobacco stalk fiber element compound is added in 35.57Kg 1- butyl -3- methylimidazole villaumites, and
Under conditions of 85 DEG C, reaction 3h is stirred with the mixing speed of 600rpm, after the completion of stirring, pours the mixture into shaping mould
In tool, and mould be placed in the ultra low temperature freezer that temperature is -75 DEG C carry out freezen protective 12h, be shaped to radius 10mm,
The cylinder of height 30mm；
(6) mixture after step (5) freezen protective and shaping is taken out, and is washed to cleaning solution with deionized water
Untill being detected without precipitation with silver nitrate, then solvent displacement 3 times is carried out to the mixture after washing with t-butanol solution, then will passed through
The mixture of solvent displacement carries out freeze-drying, you can heavy metal example is obtained has the percolate-cigarette stalk of adsorptivity
Cellulose base aeroge.
Embodiment 7
A kind of preparation method of heavy metal ion adsorbing material, it is comprised the following steps：
(1) 27Kg is adjusted to 8 by the percolate pH after filtering, removal of impurities, is subsequently adding 0.05Kg ferric trichlorides,
And using agitating device after stirring 3min under 2600rpm rotating speeds, then 10min is stirred with the rotating speed of 640rpm, after the completion of stirring
Mixed solution is staticly settled, then sediment leach is configured to solid content and is 40% solution, and solution ph is adjusted
Save to 8；
(2) 11Kg is emedullated the cigarette stalk after core, crosses 14 mesh sieves after crushing, then by the cigarette stalk after sieving with by 5.95Kg hydrogen-oxygens
Change sodium solid particle and dissolve the sodium hydroxide solution mixing that the mass fraction being configured to is 2%, and mixed solution is heated to 100
DEG C, after carrying out reaction 2h, the solid content in mixed solution is leached；
(3) 5min is discongested into the above-mentioned solid content Lampen mill for leaching, after again with toluene washing, adds it to by 15Kg
Dipping 4h is carried out in toluene and 5Kg epoxychloropropane mixed liquors, after dipping is finished, solid content is leached again, and use second successively
Alcohol, distilled water are washed, untill being washed till cleaning solution in neutrality, you can tobacco stalk fiber element is obtained；
(4) tobacco stalk fiber element obtained above is added in solution obtained in step (1), and using ultrasonic equipment with
The power of 250W carries out assisted reaction 2h, after the completion of reaction, solution is stood into 3h at normal temperatures, then the solid content in solution is filtered
Go out, washed and impregnated with the sodium hydroxide solution that pH value is 9, untill leachate is in colourless, you can prepared rubbish oozes
Filtrate-tobacco stalk fiber element compound；
(5) percolate obtained above-tobacco stalk fiber element compound is vacuum dried under conditions of 65 DEG C
After 28h, then percolate-tobacco stalk fiber element compound is added in 36Kg 1- butyl -3- methylimidazole villaumites, and
Under conditions of 70 DEG C, reaction 2h is stirred with the mixing speed of 700rpm, after the completion of stirring, pours the mixture into mould
In, and mould is placed in the ultra low temperature freezer that temperature is -65 DEG C carries out freezen protective 19h, it is shaped to radius 10mm, height
Spend the cylinder of 30mm；
(6) mixture after step (5) freezen protective and shaping is taken out, and is washed to cleaning solution with deionized water
Untill being detected without precipitation with silver nitrate, then solvent displacement 5 times is carried out to the mixture after washing with t-butanol solution, then will passed through
The mixture of solvent displacement carries out freeze-drying, you can heavy metal example is obtained has the percolate-cigarette stalk of adsorptivity
Cellulose base aeroge.
Embodiment 8
A kind of preparation method of heavy metal ion adsorbing material, it is comprised the following steps：
(1) 26Kg is adjusted to 8 by the percolate pH after filtering, removal of impurities, is subsequently adding 0.04Kg aluminum sulfate, and
After stirring 3min under 2900rpm rotating speeds using agitating device, then 10min is stirred with the rotating speed of 630rpm, will after the completion of stirring
Mixed solution is staticly settled, then sediment leach is configured to solid content and is 40% solution, and solution ph is adjusted
To 8；
(2) 10Kg is emedullated the cigarette stalk after core, crosses 14 mesh sieves after crushing, then by the cigarette stalk after sieving with by 5Kg hydroxides
The mass fraction that the dissolving of sodium solid particle is configured to is 2% sodium hydroxide solution mixing, and mixed solution is heated into 100
DEG C, after carrying out reaction 2h, the solid content in mixed solution is leached；
(3) 5min is discongested into the above-mentioned solid content Lampen mill for leaching, after again with toluene washing, adds it to by 15Kg
Dipping 5h is carried out in toluene and 5Kg epoxychloropropane mixed liquors, after dipping is finished, solid content is leached again, and use second successively
Alcohol, distilled water are washed, untill being washed till cleaning solution in neutrality, you can tobacco stalk fiber element is obtained；
(4) tobacco stalk fiber element obtained above is added in solution obtained in step (1), and using ultrasonic equipment with
The power of 120W carries out assisted reaction 4h, after the completion of reaction, solution is stood into 3h at normal temperatures, then the solid content in solution is filtered
Go out, washed and impregnated with the sodium hydroxide solution that pH value is 10, untill leachate is in colourless, you can prepared rubbish oozes
Filtrate-tobacco stalk fiber element compound；
(5) percolate obtained above-tobacco stalk fiber element compound is vacuum dried under conditions of 60 DEG C
After 24h, then percolate-tobacco stalk fiber element compound is added in 38.96Kg 1- pi-allyl -3- methylimidazole villaumites,
And under conditions of 65 DEG C, reaction 1h is stirred with the mixing speed of 800rpm, after the completion of stirring, pour the mixture into shaping
In mould, and mould is placed in the ultra low temperature freezer that temperature is -75 DEG C carries out freezen protective 12h；
(6) mixture after step (5) freezen protective and shaping is taken out, and is washed to cleaning solution with deionized water
Untill being detected without precipitation with silver nitrate, then solvent displacement 4 times is carried out to the mixture after washing with t-butanol solution, then will passed through
The mixture of solvent displacement carries out freeze-drying, you can heavy metal example is obtained has the percolate-cigarette stalk of adsorptivity
Cellulose base aeroge.
Embodiment 9
A kind of preparation method of heavy metal ion adsorbing material, it is comprised the following steps：
(1) 25Kg is adjusted to 8 by the percolate pH after filtering, removal of impurities, is subsequently adding 0.05Kg aluminum sulfate, and
After stirring 3min under 3000rpm rotating speeds using agitating device, then 10min is stirred with the rotating speed of 610rpm, will after the completion of stirring
Mixed solution is staticly settled, then sediment leach is configured to solid content and is 60% solution, and solution ph is adjusted
To 7；
(2) 11Kg is emedullated the cigarette stalk after core, crosses 14 mesh sieves after crushing, then by the cigarette stalk after sieving with by 5Kg hydroxides
The mass fraction that the dissolving of sodium solid particle is configured to is 2% sodium hydroxide solution mixing, and mixed solution is heated into 150
DEG C, after carrying out reaction 2h, the solid content in mixed solution is leached；
(3) 15min is discongested into the above-mentioned solid content Lampen mill for leaching, after again with toluene washing, add it to by
Dipping 6h is carried out in 18Kg toluene and 6Kg epoxychloropropane mixed liquors, after dipping is finished, solid content is leached again, and successively
Washed with ethanol, distilled water, untill being washed till cleaning solution in neutrality, you can tobacco stalk fiber element is obtained；
(4) tobacco stalk fiber element obtained above is added in solution obtained in step (1), and using ultrasonic equipment with
The power of 300W carries out assisted reaction 2h, after the completion of reaction, solution is stood into 3h at normal temperatures, then the solid content in solution is filtered
Go out, washed and impregnated with the sodium hydroxide solution that pH value is 10, untill leachate is in colourless, you can prepared rubbish oozes
Filtrate-tobacco stalk fiber element compound；
(5) percolate obtained above-tobacco stalk fiber element compound is vacuum dried under conditions of 80 DEG C
After 24h, then percolate-tobacco stalk fiber element compound is added in 34.95Kg 1- butyl -3- methylimidazole villaumites, and
Under conditions of 65 DEG C, reaction 1h is stirred with the mixing speed of 800rpm, after the completion of stirring, pours the mixture into shaping mould
In tool, and mould be placed in the ultra low temperature freezer that temperature is -50 DEG C carry out freezen protective 24h, be shaped to radius 10mm,
The cylinder of height 30mm；
(6) mixture after step (5) freezen protective and shaping is taken out, and is washed to cleaning solution with deionized water
Untill being detected without precipitation with silver nitrate, then solvent displacement 3 times is carried out to the mixture after washing with t-butanol solution, then will passed through
The mixture of solvent displacement carries out freeze-drying, you can heavy metal example is obtained has the percolate-cigarette stalk of adsorptivity
Cellulose base aeroge.
Performance test
Percolate obtained in 0.5g embodiments 1~9-tobacco stalk fiber element base aeroge is taken to be added separately to 1L concentration and be
In the lead ion of 50mg/L, copper ion and arsenic ion, after 25 DEG C of shaking tables concussion 24h, detect lead ion in each solution, copper from
The residual concentration of son and arsenic ion, and calculate percolate-tobacco stalk fiber element base aeroge to lead ion, copper ion and arsenic from
The adsorption rate of son, acquired results are as follows：
The above is embodiments of the invention, for the ordinary skill in the art, religion of the invention
Lead, without departing from the principles and spirit of the present invention all impartial changes done according to scope of the present invention patent, repair
Change, replace and modification, should all belong to covering scope of the invention.
Claims (9)
1. a kind of preparation method of heavy metal ion adsorbing material, it is characterised in that：With percolate as raw material, by itself and cigarette
The cellulose extracted in stalk carries out graft copolymerization and percolate-tobacco stalk fiber compound is obtained, by percolate-cigarette
After stalk fiber compound carries out gelation, then it is regenerated, exchange of solvent and supercritical carbon dioxide are dried, you can be obtained
Heavy metal ion has the percolate-cigarette pole fiber element base aeroge of adsorptivity.
2. the preparation method of a kind of heavy metal ion adsorbing material according to claim 1, it is characterised in that：It include with
Lower step：
（1）Percolate is filtered, after removal of impurities, its pH is adjusted to 7~9, be subsequently adding coagulant, and using stirring
After device stirs 3~5min with 2000~3000rpm, then 10~15min is stirred with 500~650rpm, will be mixed after the completion of stirring
Solution left standstill precipitation is closed, then sediment leach is configured to solution, and the solution ph of configuration is adjusted to 7~9；
（2）Cigarette stalk is emedullated after core, 14~20 mesh sieves are crossed after crushing, then by the cigarette stalk after sieving with by sodium hydrate solid particle
The mass fraction that dissolving is configured to is 2% sodium hydroxide solution mixing, and mixed solution is heated into 90~150 DEG C, carries out anti-
After answering 1~3h, the solid content in mixed solution is leached；
（3）5~15min is discongested into the above-mentioned solid content Lampen mill for leaching, after again with toluene washing, add it to toluene and
4~6h of dipping is carried out in the mixed liquor of epoxychloropropane, after dipping is finished, solid content is leached again, and successively with ethanol, steaming
Distilled water is washed, untill being washed till cleaning solution in neutrality, you can tobacco stalk fiber element is obtained；
（4）Tobacco stalk fiber element obtained above is added to step（1）In obtained solution, and using ultrasonic equipment with 100
The power of~300W carries out 2~5h of assisted reaction, after the completion of reaction, solution is stood into 3~5h at normal temperatures, then by solution
Solid content is leached, and is washed and is impregnated with the sodium hydroxide solution that pH value is 9~11, untill leachate is in colourless, i.e.,
Percolate-tobacco stalk fiber element compound can be obtained；
（5）By percolate obtained above-tobacco stalk fiber element compound under conditions of 60~80 DEG C, it is vacuum dried
After 24~48h, then percolate-tobacco stalk fiber element compound is added in ionic liquid, and in 65~85 DEG C of condition
Under, 1~3h of reaction is stirred with the mixing speed of 600~800rpm, after the completion of stirring, pour the mixture into mould
In, and mould is placed in the ultra low temperature freezer that temperature is -75~-50 DEG C carries out 12~24h of freezen protective；
（6）By step（5）Mixture after freezen protective and shaping takes out, and is washed with deionized water to cleaning solution nitre
Untill sour silver detection is without precipitation, then solvent displacement 3~6 times is carried out to the mixture after washing with non solvent liquid, then will passed through
The mixture of solvent displacement carries out freeze-drying, you can heavy metal example is obtained has the percolate-cigarette stalk of adsorptivity
Cellulose base aeroge.
3. the preparation method of a kind of heavy metal ion adsorbing material according to claim 2, it is characterised in that：
The addO-on therapy and mass fraction of each step are as follows：
Percolate 24%~28%；
Coagulant 0.03%~0.05%；
Cigarette stalk 10%~15%；
NaOH 5%~6%；
Toluene 15%~18%；
Epoxychloropropane 5%~6%；
Ionic liquid 34%~40%.
4. the preparation method of a kind of heavy metal ion adsorbing material according to Claims 2 or 3, it is characterised in that：It is described
Ionic liquid be 1- butyl -3- methylimidazole villaumites or 1- pi-allyl -3- methylimidazole villaumites.
5. the preparation method of a kind of heavy metal ion adsorbing material according to Claims 2 or 3, it is characterised in that：It is described
Coagulant be the polymer of molysite, aluminium salt or molysite and aluminium salt.
6. the preparation method of a kind of heavy metal ion adsorbing material according to Claims 2 or 3, it is characterised in that：It is described
Step（1）The middle solution solid content configured using sediment is 40%~60%.
7. the preparation method of a kind of heavy metal ion adsorbing material according to Claims 2 or 3, it is characterised in that：It is described
Step（5）It is middle by formed in mould mixture be radius 10mm, height 30mm cylinder.
8. the preparation method of a kind of heavy metal ion adsorbing material according to Claims 2 or 3, it is characterised in that：It is described
Non solvent liquid be the tert-butyl alcohol or acetone.
9. a kind of application of heavy metal ion adsorbing material obtained in preparation method as described in claim 1,2 or 3, its feature
It is：Heavy metal ion adsorbing material is used for heavy metal ion adsorbed in percolate.
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