CN103933950A - Method for preparing loofah sponge immobilized ionic liquid adsorbent - Google Patents
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Abstract
The invention discloses a method for preparing a loofah sponge immobilized ionic liquid adsorbent and application techniques of the adsorbent. The method is characterized by comprising the following steps: removing peels and kernels of a mature loofah fruit, washing by water to remove soil and impurities, drying, smashing, treating the smashed loofah sponge by sodium hydroxide and hydrogen peroxide, drying to obtain an oxidized loofah sponge, adding 62%-72% of epoxy chloropropane and 15%-28% of oxidized loofah sponge in percentage by mass into a reactor, stirring and reacting at the constant temperature of 70-80 DEG C for 40-60 minutes, cooling, adding 4%-10% of pyromellitic dianhydride and 2%-6% of N-ethyl-3methylpyridine bromate ionic liquid, stirring and reacting for 48-60 hours at the constant temperature of 33-37 DEG C, cooling, carrying out suction filtration, washing by deionized water till filtrate is neutral, washing by a little ethyl alcohol and drying in a vacuum drying oven at the temperature of 50 DEG C to obtain the loofah sponge immobilized ionic liquid adsorbent. The adsorbent has the advantages of very high arsenic adsorption capacity, excellent physicochemical and mechanical properties, strong regeneration capacity, high frequency of repeated use, low cost and environmental protection.
Description
Technical field
The present invention relates to a kind of preparation method's of biological adsorption agent technical field, particularly a kind of preparation method of luffa solid-loaded ionic-liquid adsorbent and the application technology to arsenic absorption in water.
Background technology
Ionic liquid is generally that inorganic anion that, structure asymmetric organic cation (as imidazoles, pyridine) relatively large by specific volume and volume are relatively little is (as Cl
-, Br
-deng) material being in a liquid state under room temperature or nearly room temperature that forms.Ionic liquid at room temperature is a kind of fine solvent, can dissolve polarity and nonpolar organic matter, inorganic matter, is easy to separate, and can be recycled.Its liquid scope is very wide, without vapour pressure, non-volatile, can not cause environmental pollution, be described as green solvent.
Ionic liquid is carried out immobilizedly can obtaining supported ion liquid or surface has the solid matter of ionic liquid structure.This had both combined the advantage of solid support material, also solve ionic liquid and be applied to the losing issue in water environment, keep again the physics and chemistry character of ionic liquid itself simultaneously, solved preferably the residual and toxicity problem of ionic liquid in extract, with the separating of extract, solvent cross pollution aspect also there is obvious advantage.Supported ion liquid preparation absorption has been reported, Wang Ruonan etc. have studied load imidazole type ion liquid silica gel and have inhaled material preparation (Wang Ruonan etc., load imidazole type ion liquid silica gel suction material preparation and application study, Chinese environmental detection, 2013,29(2): 69 ~ 72); Peng Changhong etc. studied the arsenic removal of ionic liquid loaded type carbon nanotube adsorption (; The long grand plasma fluid load type carbon nanotube adsorption Study on Removal of Arsenic of Peng, Central South University's journal (natural science edition), 2010,41(2): 416 ~ 421), but ionic liquid supported is had no on luffa to report.
Arsenic is widely distributed at occurring in nature, is present in rock, soil, river, seawater and the atmosphere in the earth's crust.Arsenic-containing ores easily enters water body and moves after weathering, oxidation.Arsenic, as there being more supervirulent element, is extensively present in natural water and drinking water.The existence of arsenic is natural reaction (as: biologically active, geochemical reaction, volcano eruption etc.) and thinks the coefficient result of discharge (as: pesticide, Chemical Manufacture, semiconductor manufacture etc.).Arsenic is a kind of extremely toxic substance, mainly with As (III) and As(V) two kinds of valence states exist.The low-oxidation-state of arsenic is larger than the toxicity of high oxidation state.People's long-term drinking and edible water and food containing arsenic, make arsenic element can cause the mutation in the organ-tissues such as Human Lung, liver, kidney and function at people's cylinder accumulation, serious caused canceration (as: cutaneum carcinoma, lung cancer, liver cancer, kidney, carcinoma of urinary bladder etc.).Therefore, to the waste water arsenic removal in drinking water and industrial production in life, be the important topic that is related to the people's livelihood, be also the focus of domestic and international experts and scholars' research.
The method of various processing arsenic has absorption method, extraction, direct precipitation method, hyperfiltration and ion-exchange etc., and wherein ion-exchange is modal method.Because ion exchange resin has good physicochemical property and abundant ion-exchange group, and can Reusability, so be widely used in the removal of waste water and Arsenic in Drinking Water.Jia Min etc. have studied the adsorbing separation of the immobilized ion exchange resin of N-methylimidazole to arsenic, maximum adsorption capacity is 67.2 mg/g(Jia Min etc., the adsorbing separation of the immobilized ion exchange resin of N-methylimidazole to arsenic, analytical chemistry, 2013,41(1): 57 ~ 62); Fan Wei etc. have studied the absorption property of hydrosulphonyl silane modified graphite oxide to arsenic, and maximum adsorption capacity is 24.45 mg/g(Fan Wei etc., the absorption property of hydrosulphonyl silane modified graphite oxide to arsenic, Environmental Chemistry, 2013,32(5): 810 ~ 818); Gao Po etc. have studied the synthetic of divinyl three amido oxycelluloses and the absorption property to uric acid and arsenic (III), maximum adsorption capacity is 0.411 mg/g(Gao Po etc., divinyl three amido oxycelluloses synthetic and the absorption property to uric acid and arsenic (III), Heilongjiang University's natural science journal, 2009,26(1): 98 ~ 103).These are all that resin, graphite and cellulose are carried out to modification, and the present invention carries out chemical modification to the luffa of natural regeneration.
Shortage of resources and environmental pollution have become two large subject matters of the world today, therefore, utilize natural reproducible resource, and the friendly type product of development environment and technology will become the inexorable trend of sustainable development.Luffa is the vascular bundle withered old fruit of sponge gourd in other words in the ripening fruits of Curcurbitaceae annual herb plant sponge gourd.Sponge gourd is China's summer and autumn Common Vegetables, there is product most provinces and regions, the whole nation, for cultivation product, luffa is the regenerated resources that the earth enriches very much, have that light weight is inexpensive, the feature such as degradable and environmental friendliness, the net that luffa is formed by the thread fiber interweaving of multilayer, body is light, matter is tough and tensile, can not fracture, simultaneously containing xylan, mannosan, galactan etc., and it has hydrophily, also with abundant dentate, be easy to carry out chemical modification, the application in adsorption of metal ions as adsorbent after domestic luffa modification.
Domestic luffa is the application in adsorption of metal ions as adsorbent, application number is to disclose luffa application in adsorption of metal ions as adsorbent to many kinds of metal ions absorption property and luffa in 200810034734.6 patent, and wherein luffa is to Cu
2+and Zn
2+desorption rate all in 40% left and right, luffa is to Cu
2+adsorbance be respectively 0.16mmol/g, to Zn
2+adsorbance be about 0.39mmol/g, in the system that is 1 at pH, desorption rate is respectively 46%, 47%; In the patent that is 200810034735.0 at application number, disclose alkalization modifying method and the application thereof of luffa, its alkali treatment luffa is to Zn
2+adsorbance compared with Cu
2+height, and adsorbance gap is larger, and through Atomic absorption quantitative analysis, luffa is to Cu
2+adsorbance be about 7 ~ 8mg/g, to Zn
2+adsorbance be about 21 ~ 22mg/g; In the patent that is 200810034737.X at application number, disclose the preparation method of etherized luffa and the application in adsorption of metal ions thereof, its etherized luffa is to Fe
3+maximal absorptive capacity be 27.4mg/g.To Zn
2+maximal absorptive capacity be 36.3mg/g; Application number is in 201110276244.9 patent, to disclose citric acid loofah sponge preparation method agent application, and its citric acid loofah sponge is to Cd
2+adsorption capacity can be up to 189mg/g, high adsorption rate can reach 98.5%, to Pb
2+maximal absorptive capacity be 285mg/g, high adsorption rate can reach 99.2%, is 316mg/g to the maximal absorptive capacity of methylene blue, high adsorption rate can reach 96.2%, has carboxylic acid characteristic, directly absorption and the wash-out to each metal ion species, organic dyestuff in water body.Natural macromolecular material is utilized as adsorbent has the advantages such as renewable, degradable, environmental protection close friend, cheapness, is important living resources.
Summary of the invention
One of object of the present invention is to provide a kind of preparation method of luffa solid-loaded ionic-liquid adsorbent, the carry out adsorbing separation of a kind of luffa solid-loaded ionic-liquid adsorbent obtaining to arsenic in aqueous systems.
Object of the present invention is achieved through the following technical solutions.
A preparation method for luffa solid-loaded ionic-liquid adsorbent, is characterised in that the method has following processing step:
(1) luffa pretreatment: luffa derives from sponge gourd fruit, obtains by peeling stoning, and luffa is cut into small pieces after clear water cleaning, drying and is pulverized, and by 10 ~ 20 object sieve, obtains pretreatment luffa;
(2) oxidation luffa: in reactor, add NaOH: 0.6 ~ 2.0% by following composition mass percentage concentration, deionized water: 59 ~ 78%, after stirring and dissolving, be chilled to room temperature, add 30% hydrogen peroxide: 12 ~ 22%, mix, then add pretreatment luffa: 8 ~ 18%, each component sum is absolutely, soaking at room temperature 24 ~ 30 h, then boil 10 ~ 30min, cooling rear extremely neutral with deionized water washing, suction filtration is dried at 80 ~ 90 DEG C, obtains being oxidized luffa;
(3) preparation of luffa solid-loaded ionic-liquid adsorbent: in reactor, add by following composition mass percentage concentration, epoxychloropropane: 62 ~ 72%, oxidation luffa 15 ~ 28%, in 70 ~ 80 DEG C of constant temperature, stir, reaction 40 ~ 60min, after cooling, add again pyromellitic acid anhydride: 4 ~ 10%, N-ethyl-3 picoline bromate ionic liquid: 2 ~ 6%, each component sum is absolutely, in 35 ± 2 DEG C of constant temperature, stir, reaction 48 ~ 60h, after cooling, suction filtration, wash by deionized water, till being neutrality to filtrate, with after a small amount of ethanol washing, be placed in 50 DEG C of vacuum drying chambers dry, obtain luffa solid-loaded ionic-liquid adsorbent.
Another object of the present invention is to provide luffa solid-loaded ionic-liquid adsorbent to the absorption to arsenic in aqueous systems, and feature is: the luffa solid-loaded ionic-liquid adsorbent deionized water preparing is soaked to 1 ~ 2h, adsorb by static method.
The luffa solid-loaded ionic-liquid adsorbent deionized water preparing is soaked to 1 ~ 2h, adsorb by dynamic method.
Compared with the prior art, tool has the following advantages and beneficial effect in the present invention:
(1) the luffa solid-loaded ionic-liquid adsorbent that the present invention obtains has good physical and chemical stability and excellent mechanical strength, adsorption capacity is large, maximum adsorption capacity reaches 101.25 mg/g, mechanical strength is high, wear-resisting can reaching more than 10 times by Reusability number of times, the speed of absorption is fast, and desorption performance is good, can within the scope of wider soda acid, use.
(2) the luffa solid-loaded ionic-liquid adsorbent that the present invention obtains had both had advantages of solid support material, had also solved ionic liquid and had been applied to the losing issue in water environment.
(3) good stability, is natural green product, regrown material, and discarded object is biodegradable;
(4) the synthetic condition of crossing range request is easily controlled, and energy consumption is low, simple to operate, belongs to process for cleanly preparing, is easy to suitability for industrialized production.
Detailed description of the invention
Embodiment 1
(1) luffa pretreatment: luffa derives from sponge gourd fruit, obtains by peeling stoning, and luffa is cut into small pieces after clear water cleaning, drying and is pulverized, and by 10 object sieve, obtains pretreatment luffa;
(2) oxidation luffa: in reactor, add respectively 1.0 g NaOH, 70mL deionized water, after stirring and dissolving, be chilled to room temperature, add 18mL30% hydrogen peroxide, mix, add again 12g pretreatment luffa, soaking at room temperature 28 h, then boil 20min, cooling rear extremely neutral with deionized water washing, suction filtration is dried at 85 DEG C, obtains being oxidized luffa;
(3) preparation of luffa solid-loaded ionic-liquid adsorbent: in reactor, add respectively 40mL epoxychloropropane, 15g is oxidized luffa, in 70 DEG C of constant temperature, stirring, reaction 60min, after cooling, add again 4mL pyromellitic acid anhydride and 3gN-ethyl--picoline bromate ionic liquid, in 35 ± 2 DEG C of constant temperature, stirring, reaction 50h, after cooling, suction filtration, washs by deionized water, till being neutrality to filtrate, with after a small amount of ethanol washing, be placed in 50 DEG C of vacuum drying chambers and be dried, obtain luffa solid-loaded ionic-liquid adsorbent.
Embodiment 2
(1) luffa pretreatment: luffa derives from sponge gourd fruit, obtains by peeling stoning, and luffa is cut into small pieces after clear water cleaning, drying and is pulverized, and by 20 object sieve, obtains pretreatment luffa;
(2) oxidation luffa: in reactor, add respectively 0.6g NaOH, 62mL deionized water, after stirring and dissolving, be chilled to room temperature, add 22mL30% hydrogen peroxide, mix, add again 15g pretreatment luffa, soaking at room temperature 30 h, then boil 20min, cooling rear extremely neutral with deionized water washing, suction filtration is dried at 90 DEG C, obtains being oxidized luffa;
(3) preparation of luffa solid-loaded ionic-liquid adsorbent: in reactor, add respectively 55mL epoxychloropropane, 18g is oxidized luffa, in 75 DEG C of constant temperature, stirring, reaction 50min, after cooling, add again 5mL pyromellitic acid anhydride and 2gN-ethyl--picoline bromate ionic liquid, in 35 ± 2 DEG C of constant temperature, stirring, reaction 48h, after cooling, suction filtration, washs by deionized water, till being neutrality to filtrate, with after a small amount of ethanol washing, be placed in 50 DEG C of vacuum drying chambers and be dried, obtain luffa solid-loaded ionic-liquid adsorbent.
Embodiment 3
(1) luffa pretreatment: luffa derives from sponge gourd fruit, obtains by peeling stoning, and luffa is cut into small pieces after clear water cleaning, drying and is pulverized, and by 10 object sieve, obtains pretreatment luffa;
(2) oxidation luffa: in reactor, add respectively 1.5 g NaOH, 78mL deionized water, after stirring and dissolving, be chilled to room temperature, add 12mL30% hydrogen peroxide, mix, add again 8g pretreatment luffa, soaking at room temperature 24 h, then boil 30min, cooling rear extremely neutral with deionized water washing, suction filtration is dried at 80 DEG C, obtains being oxidized luffa;
(3) preparation of luffa solid-loaded ionic-liquid adsorbent: in reactor, add respectively 25mL epoxychloropropane, 8g is oxidized luffa, in 80 DEG C of constant temperature, stirring, reaction 40min, after cooling, add again 2mL pyromellitic acid anhydride and 1gN-ethyl--picoline bromate ionic liquid, in 35 ± 2 DEG C of constant temperature, stirring, reaction 55h, after cooling, suction filtration, washs by deionized water, till being neutrality to filtrate, with after a small amount of ethanol washing, be placed in 50 DEG C of vacuum drying chambers and be dried, obtain luffa solid-loaded ionic-liquid adsorbent.
Embodiment 4
(1) luffa pretreatment: luffa derives from sponge gourd fruit, obtains by peeling stoning, and luffa is cut into small pieces after clear water cleaning, drying and is pulverized, and by 20 object sieve, obtains pretreatment luffa;
(2) oxidation luffa: in reactor, add respectively 1.2 g NaOH, 73mL deionized water, after stirring and dissolving, be chilled to room temperature, add 15mL30% hydrogen peroxide, mix, add again 10g pretreatment luffa, soaking at room temperature 26h, then boil 25min, cooling rear extremely neutral with deionized water washing, suction filtration is dried at 85 DEG C, obtains being oxidized luffa;
(3) preparation of luffa solid-loaded ionic-liquid adsorbent: in reactor, add respectively 35mL epoxychloropropane, 8g is oxidized luffa, in 75 DEG C of constant temperature, stirring, reaction 50min, after cooling, add again 3mL pyromellitic acid anhydride and 3gN-ethyl--picoline bromate ionic liquid, in 35 ± 2 DEG C of constant temperature, stirring, reaction 60h, after cooling, suction filtration, washs by deionized water, till being neutrality to filtrate, with after a small amount of ethanol washing, be placed in 50 DEG C of vacuum drying chambers and be dried, obtain luffa solid-loaded ionic-liquid adsorbent.
Embodiment 5
(1) luffa pretreatment: luffa derives from sponge gourd fruit, obtains by peeling stoning, and luffa is cut into small pieces after clear water cleaning, drying and is pulverized, and by 10 object sieve, obtains pretreatment luffa;
(2) oxidation luffa: in reactor, add respectively 0.8 g NaOH, 77mL deionized water, after stirring and dissolving, be chilled to room temperature, add 12mL30% hydrogen peroxide, mix, add again 10g pretreatment luffa, soaking at room temperature 25h, then boil 20min, cooling rear extremely neutral with deionized water washing, suction filtration is dried at 85 DEG C, obtains being oxidized luffa;
(3) preparation of luffa solid-loaded ionic-liquid adsorbent: in reactor, add respectively 65mL epoxychloropropane, 20g is oxidized luffa, in 80 DEG C of constant temperature, stirring, reaction 40min, after cooling, add again 10mL pyromellitic acid anhydride and 5gN-ethyl--picoline bromate ionic liquid, in 35 ± 2 DEG C of constant temperature, stirring, reaction 58h, after cooling, suction filtration, washs by deionized water, till being neutrality to filtrate, with after a small amount of ethanol washing, be placed in 50 DEG C of vacuum drying chambers and be dried, obtain luffa solid-loaded ionic-liquid adsorbent.
Embodiment 6
Take 0.50g luffa solid-loaded ionic-liquid adsorbent and be placed in 250mL tool plug conical flask, adding 100mL concentration is in 600mg/L arsenic standard solution, taking the pH value of diluted acid or alkali regulation system in 2.0 ~ 10.0 scopes, at room temperature concussion absorption 20 ~ 30min, get supernatant, by the concentration of electrochemical method determining arsenic, according to the concentration difference of arsenic in water before and after absorption, calculate the adsorption capacity of luffa solid-loaded ionic-liquid adsorbent, the prepared luffa solid-loaded ionic-liquid of embodiment 1 ~ 5 adsorbent is listed table 1. in to the adsorption capacity result of arsenic
PH value adsorbent in 3.0 ~ 7.5 scopes is maximum and stable to the adsorption capacity of arsenic as seen from Table 1, at room temperature concussion absorption 30 min, and this absorption of arsyl is complete, and the adsorption capacity of arsenic can reach 101.25 mg/g.
Adsorption capacity and the clearance measurement result of table 1 luffa solid-loaded ionic-liquid adsorbent to arsenic
Adsorbent title | pH | Adsorption time (min) | Arsenic adsorption capacity (mg/g) | Arsenic removal rate (%) |
Embodiment 1 | 2.0 | 20 | 101.25 | 95.82 |
Embodiment 1 | 3.0 | 30 | 100.21 | 97.62 |
Embodiment 2 | 4.0 | 25 | 99.89 | 95.60 |
Embodiment 2 | 5.0 | 20 | 100.12 | 98.20 |
Embodiment 3 | 6.0 | 25 | 101.12 | 97.98 |
Embodiment 3 | 7.0 | 30 | 101.01 | 98.65 |
Embodiment 4 | 7.5 | 20 | 99.98 | 97.89 |
Embodiment 4 | 8.0 | 25 | 100.62 | 96.12 |
Embodiment 5 | 9.0 | 30 | 100.87 | 99.10 |
Embodiment 5 | 10.0 | 25 | 101.15 | 98.21 |
Embodiment 7
Take 1.0g luffa solid-loaded ionic-liquid adsorbent and be placed in 250mL tool plug conical flask, adding 100mL concentration is in 200mg/L arsenic standard solution, taking the pH value of diluted acid or alkali regulation system in 3.0 ~ 7.5 scopes, at room temperature concussion absorption 30min, get supernatant, by the concentration of electrochemical method determining arsenic, according to the concentration difference of arsenic in water before and after absorption, calculate the clearance of luffa solid-loaded ionic-liquid adsorbent to arsenic, the prepared luffa solid-loaded ionic-liquid of embodiment 1 ~ 5 adsorbent to the clearance result of arsenic list in this adsorbent of table 1. to arsenic the clearance in water all more than 95.6%, reach as high as 99.1%.
Claims (4)
1. a preparation method for luffa solid-loaded ionic-liquid adsorbent, is characterised in that the method has following processing step:
(1) luffa pretreatment: luffa derives from sponge gourd fruit, obtains by peeling stoning, and luffa is cut into small pieces after clear water cleaning, drying and is pulverized, and by 10 ~ 20 object sieve, obtains pretreatment luffa;
(2) oxidation luffa: in reactor, add NaOH: 0.6 ~ 2.0% by following composition mass percentage concentration, deionized water: 59 ~ 78%, after stirring and dissolving, be chilled to room temperature, add 30% hydrogen peroxide: 12 ~ 22%, mix, then add pretreatment luffa: 8 ~ 18%, each component sum is absolutely, soaking at room temperature 24 ~ 30 h, then boil 10 ~ 30min, cooling rear extremely neutral with deionized water washing, suction filtration is dried at 80 ~ 90 DEG C, obtains being oxidized luffa;
(3) preparation of luffa solid-loaded ionic-liquid adsorbent: in reactor, add by following composition mass percentage concentration, epoxychloropropane: 62 ~ 72%, oxidation luffa 15 ~ 28%, in 70 ~ 80 DEG C of constant temperature, stir, reaction 40 ~ 60min, after cooling, add again pyromellitic acid anhydride: 4 ~ 10%, N-ethyl-3 picoline bromate ionic liquid: 2 ~ 6%, each component sum is absolutely, in 35 ± 2 DEG C of constant temperature, stir, reaction 48 ~ 60h, after cooling, suction filtration, wash by deionized water, till being neutrality to filtrate, with after a small amount of ethanol washing, be placed in 50 DEG C of vacuum drying chambers dry, obtain luffa solid-loaded ionic-liquid adsorbent.
2. according to the preparation method of a kind of luffa solid-loaded ionic-liquid adsorbent described in claim 1, it is characterized in that: when luffa is sponge gourd fruit maturation, pericarp flavescence, inner drying up, pluck, remove crust and pulp.
3. according to the preparation method of a kind of luffa solid-loaded ionic-liquid adsorbent described in claim 1, it is characterized in that: described N-ethyl-3 picoline bromate is that 1:10 ~ 12 are for optimum with oxidation luffa mass ratio.
4. according to luffa solid-loaded ionic-liquid adsorbent prepared in claim 1, it is characterized in that the application of luffa solid-loaded ionic-liquid adsorbent to arsenic adsorbing separation in water.
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CN114797795A (en) * | 2021-01-22 | 2022-07-29 | 西南科技大学 | By using GMA/H 3 PO 4 Method for treating uranium-containing wastewater by using modified natural fibers |
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CN106629969A (en) * | 2016-11-09 | 2017-05-10 | 广州城辉环保科技有限公司 | Adsorption material used for removing heavy metal ions in landfill leachate, and preparation method thereof |
CN108939117A (en) * | 2018-07-05 | 2018-12-07 | 吴亚琴 | A kind of preparation method of deodorant for refrigerator |
CN114797795A (en) * | 2021-01-22 | 2022-07-29 | 西南科技大学 | By using GMA/H 3 PO 4 Method for treating uranium-containing wastewater by using modified natural fibers |
CN114797795B (en) * | 2021-01-22 | 2024-01-05 | 西南科技大学 | Using GMA/H 3 PO 4 Method for treating uranium-containing wastewater by modified natural fibers |
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