CN106955677A - It is a kind of based on ion liquid modified egg shell/acticarbon and preparation method thereof - Google Patents
It is a kind of based on ion liquid modified egg shell/acticarbon and preparation method thereof Download PDFInfo
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- 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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
- B01J20/041—Oxides or hydroxides
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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
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
Abstract
The present invention provides a kind of based on ion liquid modified egg shell/acticarbon and preparation method thereof, and specific preparation method is:Egg shell is warming up to 550 DEG C of calcinings, adds in distilled water and disperses, silane coupler and tetraethyl orthosilicate is added, regulation to pH to 9 11, heating stirring hydrolysis, washing is dried to obtain egg shell intermediate;Rice husk and rice straw are crushed into sieving, Preliminary activation charcoal is obtained in 400 DEG C of charings, after sodium hydroxide solution modification, then at 380 400 DEG C of insulation 30min, then 750 DEG C of insulation 1h is warming up to, obtains activated carbon intermediate;Egg shell intermediate and activated carbon intermediate are well mixed and form mixture, mixture and PEI ionic liquid are dissolved in distilled water, stirs, filter, dry, it is obtained based on ion liquid modified egg shell/acticarbon.The energy-efficient low stain of preparation method of the present invention, has good adsorption effect to the heavy metal of high concentration and low concentration.
Description
Technical field
The invention belongs to heavy-metal adsorption material technical field, and in particular to a kind of based on ion liquid modified egg
Shell/acticarbon and preparation method thereof.
Background technology
Heavy metal refers to density > 4.5g/cm3Metal, in recent years, with the fast development of China's economy, ore deposit is controlled, machine
Heavy metal wastewater thereby is all produced in many production processes in the techniques such as tool manufacture, chemical industry, electronics, instrument, and due to heavy metal
The unqualified discharge of waste water, result in serious heavy metal ion pollution, to water body, agricultural land soil, human health and ecological ring
Border it is very harmful.
The method of processing heavy metal pollution at present has physical-chemical process, chemical method and bioanalysis, and physical-chemical process is included also
Former method, electrolysis and absorption method, bioanalysis have bio-flocculation process, biochemical process etc., and wherein suction-operated mainly includes physics
Absorption and chemisorbed, when the active force on adsorption molecule and sorbing material surface it is main using Van der Waals force and hydrogen bond to be main when,
Physical absorption being adsorbed as, when there is electron exchange and transfer etc. between binding molecule and sorbing material, chemisorbed is adsorbed as.
The material of conventional physical absorption such as activated carbon, molecular sieve, zeolite etc., all with higher specific surface area or surface
With the highly developed gap structure such as a large amount of micropores, cavity, passage, also there are higher adsorption effect and recyclable effect.Chicken
Eggshell is also good physisorption material, with larger specific surface area and good gas phase and liquid phase adsorption performance, at present
Egg shell also has a small amount of application in adsorbing domain.One kind disclosed in Chinese patent CN1239252C is used as absorption using discarded egg shell
The method of agent Adsorption of Heavy Metals ion, mesh number respectively 20- is obtained by discarded egg shell by washing, boiling, crush, sieve
40th, 40-60,60-100,100-140 egg shell adsorbent, and agent parsing can be parsed by sodium chloride etc., realize recyclable make
With, dosage be 1/250-1/20g/ml, to 800mg/L Pb2+Adsorption rate for 99.97%, 800mg/L Cd2+Suction
Attached rate is 98.86%.Egg shell adsorbent counterweight concentration heavy metal pollution effects prepared by this method are notable, but to relatively low dense
The heavy metal adsorption effect of degree is not good.A kind of efficient heavy ion adsorbent carbon hydroxyl disclosed in Chinese patent CN100384750C
The preparation method of apatite, egg shell is cleaned and reaction is added in phosphoric acid after dries pulverizing forms calcium phosphate, then with urea and
Calcium hydroxide heating response obtains carbonate-hydroxylapatite powder.Cd of the carbonate-hydroxylapatite powder to 80mg/L2+Adsorption rate be
96.49%, 80mg/L Cu2+Adsorption rate be 97.56%, 80mg/L Zn2+Adsorption rate be 98.31%, significantly improve
To the heavy metal adsorption effect to low concentration, but egg shell is intended only as the raw material of calcium carbonate to use in this method, its
The advantage of the structural behaviour of itself is ignored.Therefore how advantage of the egg shell in adsorbing domain is maximized with research
Value.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of based on ion liquid modified egg shell/acticarbon
And preparation method thereof, using egg shell, rice husk and rice straw as raw material, egg shell is calcined and is modified as in the middle of egg shell
Body, rice husk and rice straw secondary clacining are as activated carbon intermediate, then through PEI ionic liquid after both are mixed
Modification prepares energy-efficient adsorbent, has good adsorption effect to the heavy metal of high concentration and low concentration.
In order to solve the above technical problems, the technical scheme is that:
It is a kind of based on ion liquid modified egg shell/acticarbon, it is described based on ion liquid modified egg
Shell/acticarbon includes modified egg shell and modified activated carbon, and the modified egg shell is that egg shell is first passed through after calcining
Silane coupler, tetraethyl orthosilicate and it is ion liquid modified obtain, the modified activated carbon is that rice husk and rice straw are forged first
Secondary clacining is activated through NaOH after burning, then is obtained through ion liquid modified.
As the preferred of above-mentioned technical proposal, the ionic liquid is PEI ionic liquid.
As the preferred of above-mentioned technical proposal, the ionic liquid is amino poly ion liquid polyamines.
The present invention also provides a kind of preparation method based on ion liquid modified egg shell/acticarbon, including
Following steps:
(1) egg shell is warming up to 550 DEG C with 5-10 DEG C/min, and calcined at 550 DEG C after 1-5h, take 0.5-2g to calcine
Egg shell afterwards, which is added in 50ml distilled water, to be disperseed, and adds 2600-3900 μ l silane coupler and tetraethyl orthosilicate, ammonia is added dropwise
Water is adjusted to pH to 9-11, is heated to 60-80 DEG C, stirring hydrolysis 2-5h, washing is dried to obtain egg shell intermediate;
(2) rice husk and rice straw are crushed and sieved, Preliminary activation charcoal is obtained with 400 DEG C of charing 1h in Muffle furnace, will just
Modification 24h in activated carbon immersion sodium hydroxide solution is walked, is taken out, then is placed in Muffle furnace 380-400 DEG C of insulation 30min,
750 DEG C of insulation 1h are warming up to again, obtain activated carbon intermediate;
(3) activated carbon intermediate prepared by the egg shell intermediate and step (2) prepared step (1), which is well mixed, to be formed
Mixture, mixture and PEI ionic liquid are dissolved in 20ml distilled water, stirring, filtering, are dried, be made be based on from
Egg shell/acticarbon of sub- liquid modifying.
As the preferred of above-mentioned technical proposal, in the step (1), calcination time is preferably 2-3h.
As the preferred of above-mentioned technical proposal, in the step (1), the volume of silane coupler and tetraethyl orthosilicate is 1:
1-5, preferably 1:1-2.
As the preferred of above-mentioned technical proposal, in the step (2), the concentration of sodium hydroxide solution is 40-50%.
As the preferred of above-mentioned technical proposal, in the step (2), NaOH and Preliminary activation in sodium hydroxide solution
The mass ratio of charcoal is 3:1-2.
As the preferred of above-mentioned technical proposal, in the step (3), the quality of mixture and PEI ionic liquid
Than for 0.5-3:1.
As the preferred of above-mentioned technical proposal, in the step (3), in mixture in the middle of egg shell intermediate and activated carbon
The mass ratio of body is 1:0.5-1.
Compared with prior art, the invention has the advantages that:
(1) primary raw material based on ion liquid modified egg shell/acticarbon prepared by the present invention is egg
Shell and activated carbon, egg shell have larger specific surface area and excellent liquid phase adsorption performance in itself, are protected after egg shell is calcined
Original porous performance has been stayed, the impurity and organic matter of attachment is eliminated, the main component of egg shell is changed into oxidation from calcium carbonate
Calcium, calcium oxide is handled through silane coupler and tetraethyl orthosilicate again, forms silica on the surface of calcining egg shell, raising is forged
The hydrophobicity of roast chicken eggshell and the absorption property of heavy metal ion, activated carbon is to be used as raw material system by rice husk and rice straw
Standby, containing multistage hole in activated carbon after calcining, multistage hole can be adsorbed to different heavy metals respectively, then be passed through
NaOH is activated, and activated carbon is generated the small molecule such as soluble glass and sodium carbonate, micropore is further left after washing, is carried
The high absorption to small-molecule substance, finally carries out table using PEI ionic liquid to modified egg shell and modified activated carbon
Face is modified, and is formed cationic adsorption agent, is more beneficial in acid condition, Adsorption of Heavy Metals ion, especially chromium ion.
(2) mechanism of action based on ion liquid modified egg shell/acticarbon prepared by the present invention is physics
Chemisorbed, the adsorbent can be adsorbed to different heavy metal ion, and counterweight concentration and light concentration heavy metal from
Son has a good adsorption effect, and the absorption property of heavy metal chromium ion in acid condition is optimal.
(3) primary raw material based on ion liquid modified egg shell/acticarbon prepared by the present invention is agriculture
With and household castoff, belong to resource reclaim recycling, environmental protection, the adsorbent of preparation takes full advantage of the advantage of raw material,
And transformed, make the absorption property of adsorbent excellent, adsorption efficiency is high, can reach the mesh made rational use of resources with energy-saving and emission-reduction
's.
Embodiment
Describe the present invention in detail below in conjunction with specific embodiment, herein illustrative examples and explanation of the invention
For explaining the present invention, but it is not as a limitation of the invention.
Embodiment 1:
(1) egg shell is warming up to 550 DEG C with 5 DEG C/min, and calcined at 550 DEG C after 1h, take the egg after 1g calcinings
Shell, which is added in 50ml distilled water, to be disperseed, and the volume for adding 2600 μ l is 1:1 silane coupler and tetraethyl orthosilicate, is added dropwise ammoniacal liquor
Regulation is heated to 60 DEG C, stirring hydrolysis 3h, washing is dried to obtain egg shell intermediate to pH to 9.
(2) rice husk and rice straw are crushed and sieved, Preliminary activation charcoal is obtained with 400 DEG C of charing 1h in Muffle furnace, according to
NaOH is 3 with the mass ratio of Preliminary activation charcoal:1, Preliminary activation charcoal is immersed at modified in 40% sodium hydroxide solution
24h is managed, is taken out, then is placed in 380 DEG C of insulation 30min in Muffle furnace, then is warming up to 750 DEG C of insulation 1h, activated carbon intermediate is obtained.
(3) it is 1 according to the mass ratio of egg shell intermediate and activated carbon intermediate:0.5, by egg shell intermediate and activity
Charcoal intermediate is well mixed to form mixture, is 1 by mass ratio:0.5 mixture is dissolved in PEI ionic liquid
In 20ml distilled water, stirring, filtering, be placed in 70 DEG C of baking ovens dry 12h, be made based on ion liquid modified egg shell/
Acticarbon.
Embodiment 2:
(1) egg shell is warming up to 550 DEG C with 10 DEG C/min, and calcined at 550 DEG C after 5h, take the chicken after 0.5g calcinings
Eggshell, which is added in 50ml distilled water, to be disperseed, and the volume for adding 3900 μ l is 1:3 silane coupler and tetraethyl orthosilicate, is added dropwise ammonia
Water is adjusted to pH to 11, is heated to 80 DEG C, stirring hydrolysis 5h, washing is dried to obtain egg shell intermediate.
(2) rice husk and rice straw are crushed and sieved, Preliminary activation charcoal is obtained with 400 DEG C of charing 1h in Muffle furnace, according to
NaOH is 3 with the mass ratio of Preliminary activation charcoal:2, Preliminary activation charcoal is immersed at modified in 50% sodium hydroxide solution
24h is managed, is taken out, then is placed in 400 DEG C of insulation 30min in Muffle furnace, then is warming up to 750 DEG C of insulation 1h, activated carbon intermediate is obtained.
(3) it is 1 according to the mass ratio of egg shell intermediate and activated carbon intermediate:1, by egg shell intermediate and activated carbon
Intermediate is well mixed to form mixture, is 1 by mass ratio:0.5 mixture is dissolved in 20ml with PEI ionic liquid
In distilled water, stirring, filtering are placed in 70 DEG C of baking ovens and dry 12h, be made based on ion liquid modified egg shell/activity
Carbon adsorbent.
Embodiment 3:
(1) egg shell is warming up to 550 DEG C with 7.5 DEG C/min, and calcined at 550 DEG C after 3h, take the chicken after 2g calcinings
Eggshell, which is added in 50ml distilled water, to be disperseed, and the volume for adding 3900 μ l is 1:5 silane coupler and tetraethyl orthosilicate, is added dropwise ammonia
Water is adjusted to pH to 10, is heated to 70 DEG C, stirring hydrolysis 2h, washing is dried to obtain egg shell intermediate.
(2) rice husk and rice straw are crushed and sieved, Preliminary activation charcoal is obtained with 400 DEG C of charing 1h in Muffle furnace, according to
NaOH is 3 with the mass ratio of Preliminary activation charcoal:1.5, Preliminary activation charcoal is immersed to modified in 45% sodium hydroxide solution
24h is handled, is taken out, then is placed in 390 DEG C of insulation 30min in Muffle furnace, then is warming up to 750 DEG C of insulation 1h, is obtained in the middle of activated carbon
Body.
(3) it is 1 according to the mass ratio of egg shell intermediate and activated carbon intermediate:0.8, by egg shell intermediate and activity
Charcoal intermediate is well mixed to form mixture, is 1 by mass ratio:3 mixture is dissolved in 20ml with PEI ionic liquid
In distilled water, stirring, filtering are placed in 70 DEG C of baking ovens and dry 12h, be made based on ion liquid modified egg shell/activity
Carbon adsorbent.
Embodiment 4:
(1) egg shell is warming up to 550 DEG C with 5 DEG C/min, and calcined at 550 DEG C after 1h, take the egg after 1g calcinings
Shell, which is added in 50ml distilled water, to be disperseed, and the volume for adding 2600 μ l is 1:1 silane coupler and tetraethyl orthosilicate, is added dropwise ammoniacal liquor
Regulation is heated to 60 DEG C, stirring hydrolysis 3h, washing is dried to obtain egg shell intermediate to pH to 9.
(2) rice husk and rice straw are crushed and sieved, Preliminary activation charcoal is obtained with 400 DEG C of charing 1h in Muffle furnace, according to
NaOH is 3 with the mass ratio of Preliminary activation charcoal:1.2, Preliminary activation charcoal is immersed to modified in 42% sodium hydroxide solution
24h is handled, is taken out, then is placed in 385 DEG C of insulation 30min in Muffle furnace, then is warming up to 750 DEG C of insulation 1h, is obtained in the middle of activated carbon
Body.
(3) it is 1 according to the mass ratio of egg shell intermediate and activated carbon intermediate:0.9, by egg shell intermediate and activity
Charcoal intermediate is well mixed to form mixture, is 1 by mass ratio:0.5 mixture is dissolved in PEI ionic liquid
In 20ml distilled water, stirring, filtering, be placed in 70 DEG C of baking ovens dry 10h, be made based on ion liquid modified egg shell/
Acticarbon.
Embodiment 5:
(1) egg shell is warming up to 550 DEG C with 10 DEG C/min, and calcined at 550 DEG C after 5h, take the chicken after 0.5g calcinings
Eggshell, which is added in 50ml distilled water, to be disperseed, and the volume for adding 3900 μ l is 1:3 silane coupler and tetraethyl orthosilicate, is added dropwise ammonia
Water is adjusted to pH to 11, is heated to 80 DEG C, stirring hydrolysis 5h, washing is dried to obtain egg shell intermediate.
(2) rice husk and rice straw are crushed and sieved, Preliminary activation charcoal is obtained with 400 DEG C of charing 1h in Muffle furnace, according to
NaOH is 3 with the mass ratio of Preliminary activation charcoal:1.7, Preliminary activation charcoal is immersed to modified in 48% sodium hydroxide solution
24h is handled, is taken out, then is placed in 395 DEG C of insulation 30min in Muffle furnace, then is warming up to 750 DEG C of insulation 1h, is obtained in the middle of activated carbon
Body.
(3) it is 1 according to the mass ratio of egg shell intermediate and activated carbon intermediate:0.8, by egg shell intermediate and activity
Charcoal intermediate is well mixed to form mixture, is 1 by mass ratio:0.5 mixture is dissolved in PEI ionic liquid
In 20ml distilled water, stirring, filtering, be placed in 70 DEG C of baking ovens dry 11h, be made based on ion liquid modified egg shell/
Acticarbon.
Embodiment 6:
(1) egg shell is warming up to 550 DEG C with 7.5 DEG C/min, and calcined at 550 DEG C after 3h, take the chicken after 2g calcinings
Eggshell, which is added in 50ml distilled water, to be disperseed, and the volume for adding 3900 μ l is 1:5 silane coupler and tetraethyl orthosilicate, is added dropwise ammonia
Water is adjusted to pH to 9.5, is heated to 70 DEG C, stirring hydrolysis 2h, washing is dried to obtain egg shell intermediate.
(2) rice husk and rice straw are crushed and sieved, Preliminary activation charcoal is obtained with 400 DEG C of charing 1h in Muffle furnace, according to
NaOH is 3 with the mass ratio of Preliminary activation charcoal:1.3, Preliminary activation charcoal is immersed to modified in 46% sodium hydroxide solution
24h is handled, is taken out, then is placed in 390 DEG C of insulation 30min in Muffle furnace, then is warming up to 750 DEG C of insulation 1h, is obtained in the middle of activated carbon
Body.
(3) it is 1 according to the mass ratio of egg shell intermediate and activated carbon intermediate:0.9, by egg shell intermediate and activity
Charcoal intermediate is well mixed to form mixture, is 1 by mass ratio:3 mixture is dissolved in 20ml with PEI ionic liquid
In distilled water, stirring, filtering are placed in 70 DEG C of baking ovens and dry 12h, be made based on ion liquid modified egg shell/activity
Carbon adsorbent.
Comparative example 1:
Egg shell is warming up to 550 DEG C with 5 DEG C/min, and calcined at 550 DEG C after 1h, takes the egg shell after 1g calcinings to add
Enter in 50ml distilled water and disperse, the volume for adding 2600 μ l is 1:1 silane coupler and tetraethyl orthosilicate, is added dropwise ammoniacal liquor regulation
To pH to 9,60 DEG C are heated to, stirring hydrolysis 3h, washing is dried to obtain egg shell intermediate.It is 1 by mass ratio:0.5 egg
Shell intermediate is dissolved in 20ml distilled water with PEI ionic liquid, stirring, filtering, is placed in 70 DEG C of baking ovens and is dried
12h, is made based on ion liquid modified egg shell adsorbent.
After testing, what prepared by embodiment 1-6 is made based on ion liquid modified egg shell/acticarbon, comparative example 1
The standby egg shell and activated carbon based on ion liquid modified egg shell adsorbent and prior art is to Cr (VI) ion
Absorption result is as follows:
As seen from the above table, the present invention prepare based on ion liquid modified egg shell/acticarbon in acid bar
Adsorption effect is best under part, and the heavy metal ion of counterweight concentration and light concentration all has good absorption property, with existing skill
The egg shell of art is compared absorption property with activated carbon and significantly improved.
The above-described embodiments merely illustrate the principles and effects of the present invention, not for the limitation present invention.It is any ripe
Know the personage of this technology all can carry out modifications and changes under the spirit and scope without prejudice to the present invention to above-described embodiment.Cause
This, those of ordinary skill in the art is complete without departing from disclosed spirit and institute under technological thought such as
Into all equivalent modifications or change, should by the present invention claim be covered.
Claims (10)
1. it is a kind of based on ion liquid modified egg shell/acticarbon, it is characterised in that:It is described to be based on ionic liquid structural reform
Property egg shell/acticarbon include modified egg shell and modified activated carbon, the modified egg shell is egg shell through forging
After burning first through silane coupler, tetraethyl orthosilicate and it is ion liquid modified obtain, the modified activated carbon is rice husk and paddy rice straw
Stalk activates secondary clacining after calcining first through NaOH, then is obtained through ion liquid modified.
2. according to claim 1 a kind of based on ion liquid modified egg shell/acticarbon, its feature exists
In:The ionic liquid is PEI ionic liquid.
3. according to claim 1 a kind of based on ion liquid modified egg shell/acticarbon, its feature exists
In:The ionic liquid is amino poly ion liquid polyamines.
4. a kind of preparation method based on ion liquid modified egg shell/acticarbon, it is characterised in that including following
Step:
(1) egg shell is warming up to 550 DEG C with 5-10 DEG C/min, and calcined at 550 DEG C after 1-5h, taken after 0.5-2g calcinings
Egg shell, which is added in 50ml distilled water, to be disperseed, and adds 2600-3900 μ l silane coupler and tetraethyl orthosilicate, and ammoniacal liquor is added dropwise and adjusts
Section is heated to 60-80 DEG C, stirring hydrolysis 2-5h, washing is dried to obtain egg shell intermediate to pH to 9-11;
(2) rice husk and rice straw are crushed and sieved, obtained Preliminary activation charcoal with 400 DEG C of charing 1h in Muffle furnace, will tentatively live
Property charcoal immersion sodium hydroxide solution in modification 24h, take out, then be placed in Muffle furnace 380-400 DEG C of insulation 30min, then rise
Temperature obtains activated carbon intermediate to 750 DEG C of insulation 1h;
(3) activated carbon intermediate prepared by the egg shell intermediate and step (2) prepared step (1), which is well mixed, forms mixing
Thing, mixture and PEI ionic liquid are dissolved in 20ml distilled water, stirred, filter, are dried, are made and are based on ionic liquid
Modifies egg shell/acticarbon.
5. a kind of preparation method based on ion liquid modified egg shell/acticarbon according to claim 4,
It is characterized in that:In the step (1), calcination time is preferably 2-3h.
6. a kind of preparation method based on ion liquid modified egg shell/acticarbon according to claim 4,
It is characterized in that:In the step (1), the volume of silane coupler and tetraethyl orthosilicate is 1:1-5, preferably 1:1-2.
7. a kind of preparation method based on ion liquid modified egg shell/acticarbon according to claim 4,
It is characterized in that:In the step (2), the concentration of sodium hydroxide solution is 40-50%.
8. a kind of preparation method based on ion liquid modified egg shell/acticarbon according to claim 4,
It is characterized in that:In the step (2), NaOH and the mass ratio of Preliminary activation charcoal are 3 in sodium hydroxide solution:1-2.
9. a kind of preparation method based on ion liquid modified egg shell/acticarbon according to claim 4,
It is characterized in that:In the step (3), mixture is 0.5-3 with the mass ratio of PEI ionic liquid:1.
10. a kind of preparation side based on ion liquid modified egg shell/acticarbon according to claim 4
Method, it is characterised in that:In the step (3), the mass ratio of egg shell intermediate and activated carbon intermediate is 1 in mixture:
0.5-1。
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Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108499546A (en) * | 2018-04-25 | 2018-09-07 | 安徽天顺环保设备股份有限公司 | A kind of preparation method of heavy metal absorbent |
CN108579677A (en) * | 2018-05-07 | 2018-09-28 | 金肯职业技术学院 | A kind of preparation method of rice hull carbon |
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CN113813918A (en) * | 2021-10-11 | 2021-12-21 | 福建省海凝环保科技有限公司 | Epoxy acrylate polymer-based activated carbon prepared based on zinc-containing ionic liquid and application thereof in copper ion adsorption |
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Cited By (6)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN108499546A (en) * | 2018-04-25 | 2018-09-07 | 安徽天顺环保设备股份有限公司 | A kind of preparation method of heavy metal absorbent |
CN108579677A (en) * | 2018-05-07 | 2018-09-28 | 金肯职业技术学院 | A kind of preparation method of rice hull carbon |
CN110252256A (en) * | 2019-06-28 | 2019-09-20 | 河北科技大学 | A kind of magnetic ionic liquids, its application and modified activated carbon and preparation method thereof |
CN110252256B (en) * | 2019-06-28 | 2021-11-05 | 河北科技大学 | Magnetic ionic liquid, application thereof, modified activated carbon and preparation method thereof |
CN113813918A (en) * | 2021-10-11 | 2021-12-21 | 福建省海凝环保科技有限公司 | Epoxy acrylate polymer-based activated carbon prepared based on zinc-containing ionic liquid and application thereof in copper ion adsorption |
CN113813918B (en) * | 2021-10-11 | 2023-09-01 | 福建省海凝环保科技有限公司 | Epoxy acrylate polymer-based activated carbon prepared based on zinc-containing ionic liquid and application of activated carbon in copper ion adsorption |
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