CN103566907B - Preparation method and application of pyromellitic dianhydride modified loofah sponge adsorbent - Google Patents
Preparation method and application of pyromellitic dianhydride modified loofah sponge adsorbent Download PDFInfo
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- CN103566907B CN103566907B CN201310560612.1A CN201310560612A CN103566907B CN 103566907 B CN103566907 B CN 103566907B CN 201310560612 A CN201310560612 A CN 201310560612A CN 103566907 B CN103566907 B CN 103566907B
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Abstract
The invention discloses a preparation method and application of a pyromellitic dianhydride modified loofah sponge adsorbent. The preparation method is characterized by comprising the following steps of: adding the components by mass percent to a reactor, namely, 68 to 88% of N, N-dimethylformamide, and 3.0 to 10% of pyromellitic dianhydride; adding 8 to 25% by mass of epoxy chloropropane modified loofah sponge after completely dissolving, wherein the sum of all the components is a hundred percent; performing reaction for 5 to 8 hours at constant temperature of 70 to 80 DEG C; carrying out suction filtration; washing the product by N, N-dimethylformamide, 0.1 mol/L NaOH solution and deionized water in sequence; drying to obtain the pyromellitic dianhydride modified loofah sponge adsorbent. The adsorbent can be directly used for adsorbing heavy metal ions in the water body, is high in adsorbing efficiency and outstanding in physical, chemical and mechanical stability, can be applied within a wider acid and alkali range, and is renewable and recyclable; the loofah sponge is natural biopolymer and biodegradable, so that the pyromellitic dianhydride modified loofah sponge adsorbent is a natural green adsorbent.
Description
Technical field
The present invention relates to preparation method and the application technology of metal biosorption agent in aqueous systems, particularly a kind of pyromellitic acid anhydride modifies the adsorption applications of luffa preparation method and heavy metal ion.
Background technology
Develop rapidly along with socioeconomic, the fast development of industry, the heavy metal ion content discharged in our surrounding environment also gets more and more, day by day serious to the pollution of surrounding environment, not only destroys environment and also forms potential threat to the life of people with healthy.Different from organic pollution, not only can not be decomposed by the microorganisms in the environment of these materials containing heavy metal around us, food chain can also be entered progressively accumulate, even some also can be changed to the thing larger to our human health risk under microorganism constantly acts on, the metabolism of biology is damaged, and then has very large threat to health and environment.And water is not inexhaustible.Therefore, prevent and treat tellurian contaminated wastewater, the environment protecting us to depend on for existence has become the problem of the concern of people.Heavy Metal Pollution Control is the important environmental problem of urgently to be resolved hurrily one in the current whole world, thus also becomes a study hotspot of scientific domain.
Shortage of resources and environmental pollution have become two large subject matters of the world today, and along with the minimizing day by day of current available resources, realizing and utilizing of renewable resource is subject to the attention of the mankind day by day.Wherein biosorption process is exactly a kind of Novel waste method for treating water, its raw material sources are very abundant, it is low to produce, resource efficiency is high and can not cause the benefits such as secondary pollution to environment, therefore the concern of a lot of scientific research personnel is received, therefore, utilize natural reproducible resource, development environment friendly product and technology will become the inexorable trend of sustainable development.Luffa is the withered old fruit of vascular bundle in the ripening fruits of Curcurbitaceae annual herb plant sponge gourd sponge gourd in other words.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, luffa is by the net of 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, domestic luffa is modified as the application of adsorbent in adsorption of metal ions.
Domestic luffa is as the application of adsorbent in adsorption of metal ions, application number is disclose luffa in the patent of 200810034734.6 to many kinds of metal ions absorption property and luffa as the application of adsorbent in adsorption of metal ions, and wherein luffa is to Cu
2+and Zn
2+desorption rate all about 40%, luffa is to Cu
2+adsorbance be respectively 0.16mmol/g, to Zn
2+adsorbance be about 0.39mmol/g, be that in the system of 1, desorption rate is respectively 46%, 47% at pH; Be the alkalization modifying method and the application thereof that disclose luffa in the patent of 200810034735.0 at application number, its alkali treatment luffa is to Zn
2+adsorbance comparatively Cu
2+height, and adsorbance gap is comparatively large, 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; Be disclose the preparation method of etherized luffa and the application in adsorption of metal ions thereof in the patent of 200810034737.X at application number, 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 disclose citric acid loofah sponge preparation method agent application in the patent of 201110276244.9, and its citric acid loofah sponge is to Cd
2+adsorption capacity can up to 189mg/g, most high adsorption rate can reach 98.5%, to Pb
2+maximal absorptive capacity be 285mg/g, most high adsorption rate can reach 99.2%, is 316mg/g to the maximal absorptive capacity of methylene blue, and most high adsorption rate can reach 96.2%, has carboxylic acid characteristic, can directly to absorption and the wash-out of metal ion species each in water body, organic dyestuff,
Due to the special construction of pyromellitic acid anhydride, it has very high chemism, and heavy metal ionic adsorption can be controlled by the pH value of system, selectively adsorbs metal ion when different pH value.This patent take cocoanut shell as support material, adopts pyromellitic acid anhydride (PMDA) to carry out chemical modification, introduces carboxyl-reactive functional group, the adsorption capacity of its heavy metal ion is obviously strengthened on cocoanut shell surface.Each metal ion species is made to reach the object of separation by the acidity of regulation system.
Summary of the invention
An object of the present invention is to provide a kind of pyromellitic acid anhydride and modifies loofah adsorbent preparation method, mainly makes the adsorption capacity of the pyromellitic acid anhydride of acquisition modification loofah adsorbent heavy metal ion in aqueous systems larger.
Object of the present invention is achieved through the following technical solutions.
A kind of pyromellitic acid anhydride modifies loofah adsorbent preparation method, is characterised in that the method has following processing step:
(1) luffa pretreatment: luffa derives from ripe sponge gourd fruit, is obtained by peeling stoning, pulverizes, by 20 ~ 40 object sieve, obtain pretreatment luffa after the clear water cleaning, drying that are cut into small pieces by luffa;
(2) alkalize luffa: by pretreatment luffa by 100 ~ 250g/L solid-to-liquid ratio, be the NaOH solution of 2 ~ 5% by percentage concentration, soaking at room temperature 24 ~ 36 h, boil 20 ~ 50min again, deionized water is spent to neutral after cooling, put into isopropyl alcohol again and soak 6 ~ 10 h, dry at 75 DEG C after suction filtration, obtain the luffa that alkalizes;
(3) epoxychloropropane modify luffa preparation: in the reactor, add respectively, water: 25 ~ 40%, epoxychloropropane: 30 ~ 58%, the volume ratio of water and epoxychloropropane between 1:0.75 ~ 2.2, NaOH:3 ~ 8%; Alkalization luffa: 8 ~ 26%, each component sum is absolutely, in 70 ~ 75 DEG C of constant temperature, stirring, back flow reaction 4 ~ 6 h, after cooling, spend deionized water, suction filtration, to filtrate is neutrality, after a small amount of ethanol washing, vacuum drying, obtains epoxychloropropane and modifies luffa.
(4) pyromellitic acid anhydride modifies loofah adsorbent preparation: in the reactor, add by following composition mass percent, DMF: 68 ~ 88%, pyromellitic acid anhydride: 3.0 ~ 10%, add epoxychloropropane after dissolving completely and modify luffa: 8 ~ 25%, each component sum is absolutely, after 70 ~ 80 DEG C of isothermal reaction 5 ~ 8 h, suction filtration, use DMF successively, 0.1 mol L
-1naOH solution, deionized water washed product for several times, is placed in baking oven dry, obtains pyromellitic acid anhydride and modifies loofah adsorbent.
Another object of the present invention is to provide the application that a kind of pyromellitic acid anhydride modifies loofah adsorbent heavy metal ionic adsorption in aqueous systems, feature is: the pyromellitic acid anhydride prepared is modified loofah adsorbent deionized water and soaks 1 ~ 3h, adsorb by static method.
The pyromellitic acid anhydride prepared can also be modified loofah adsorbent deionized water and soak 1 ~ 3 h, adsorb by dynamic method.
Advantage of the present invention and effect are:
The invention has the beneficial effects as follows: the pyromellitic acid anhydride of acquisition modifies luffa to Cd
2+adsorption capacity can up to 181.78 mgg
-1, to Pb
2+maximal absorptive capacity be 362.17 mgg
-1, to Cu
2+maximal absorptive capacity be 171.71 mgg
-1, most high adsorption rate can reach 98%, can directly to absorption and the wash-out of metal ion species in water body, adsorption efficiency is high, and the speed of absorption is fast, by force selective, desorption performance is good, has good physical and chemical stability and excellent mechanical stability, can use within the scope of wider soda acid; Have larger adsorption capacity, water penetration is better, the stronger Reusability of power of regeneration often; The more important thing is that luffa is natural macromolecular material, so not only saved raw-material cost but also achieved twice laid; Luffa is that biological raw material can biodegradation, uses this adsorbent environmentally safe; Present invention process is simple, and condition is easy to control, and production cost is low, is easy to the advantages such as suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is the raw-material ESEM of luffa (SEM) figure
Fig. 2 is ESEM (SEM) figure that pyromellitic acid anhydride modifies luffa.
Detailed description of the invention
Embodiment 1
(1) luffa pretreatment: luffa derives from ripe sponge gourd fruit, is obtained by peeling stoning, pulverizes, by 20 ~ 40 object sieve, obtain pretreatment luffa after the clear water cleaning, drying that are cut into small pieces by luffa;
(2) alkalize luffa: by 20g pretreatment luffa, be the NaOH solution of 5% by 200mL mass percentage concentration, soaking at room temperature 24 h, boil 30min again, spend deionized water after cooling to neutral, then put into isopropyl alcohol and soak 8 h, dry at 75 DEG C after suction filtration, obtain the luffa that alkalizes;
(3) luffa preparation modified by epoxychloropropane: in the reactor, add respectively, water: 25mL, epoxychloropropane: 50mL, NaOH:5g; Alkalization luffa: 20g, in 70 DEG C of constant temperature, stirring, back flow reaction 5 h, after cooling, spends deionized water, suction filtration, and to filtrate is neutrality, after a small amount of ethanol washing, vacuum drying, obtains epoxychloropropane and modify luffa.
(4) pyromellitic acid anhydride modifies loofah adsorbent preparation: in the reactor, add respectively, DMF: 75mL, pyromellitic acid anhydride: 5g, add epoxychloropropane after dissolving completely and modify luffa: 20g, after 75 DEG C of isothermal reaction 6 h, suction filtration, uses N successively, dinethylformamide, 0.1 mol L
-1naOH solution, deionized water washed product for several times, is placed in baking oven dry, obtains pyromellitic acid anhydride and modifies loofah adsorbent.
Embodiment 2
(1) luffa pretreatment: luffa derives from ripe sponge gourd fruit, is obtained by peeling stoning, pulverizes, by 20 ~ 40 object sieve, obtain pretreatment luffa after the clear water cleaning, drying that are cut into small pieces by luffa;
(2) alkalize luffa: by 20g pretreatment luffa, be the NaOH solution of 3% by 100mL mass percentage concentration, soaking at room temperature 36 h, boil 40min again, spend deionized water after cooling to neutral, then put into isopropyl alcohol and soak 10 h, dry at 75 DEG C after suction filtration, obtain the luffa that alkalizes;
(3) luffa preparation modified by epoxychloropropane: in the reactor, add respectively, water: 25mL, epoxychloropropane: 30mL, NaOH:2g; Alkalization luffa: 8g, in 75 DEG C of constant temperature, stirring, back flow reaction 4h, after cooling, spends deionized water, suction filtration, and to filtrate is neutrality, after a small amount of ethanol washing, vacuum drying, obtains epoxychloropropane and modify luffa.
(4) pyromellitic acid anhydride modifies loofah adsorbent preparation: in the reactor, add respectively, DMF: 40mL, pyromellitic acid anhydride: 2g, add epoxychloropropane after dissolving completely and modify luffa: 8g, after 70 DEG C of isothermal reaction 8 h, suction filtration, uses N successively, dinethylformamide, 0.1 mol L
-1naOH solution, deionized water washed product for several times, is placed in baking oven dry, obtains pyromellitic acid anhydride and modifies loofah adsorbent.
Embodiment 3
(1) luffa pretreatment: luffa derives from ripe sponge gourd fruit, is obtained by peeling stoning, pulverizes, by 20 ~ 40 object sieve, obtain pretreatment luffa after the clear water cleaning, drying that are cut into small pieces by luffa;
(2) alkalize luffa: by 50g pretreatment luffa, be the NaOH solution of 4% by 200mL mass percentage concentration, soaking at room temperature 30 h, boil 50min again, spend deionized water after cooling to neutral, then put into isopropyl alcohol and soak 6h, dry at 75 DEG C after suction filtration, obtain the luffa that alkalizes;
(3) luffa preparation modified by epoxychloropropane: in the reactor, add respectively, water: 20mL, epoxychloropropane: 30mL, NaOH:4g; Alkalization luffa: 16g, in 70 DEG C of constant temperature, stirring, back flow reaction 6h, after cooling, spends deionized water, suction filtration, and to filtrate is neutrality, after a small amount of ethanol washing, vacuum drying, obtains epoxychloropropane and modify luffa.
(4) pyromellitic acid anhydride modifies loofah adsorbent preparation: in the reactor, add respectively, DMF: 43mL, pyromellitic acid anhydride: 2g, add epoxychloropropane after dissolving completely and modify luffa: 15g, after 80 DEG C of isothermal reaction 5 h, suction filtration, uses N successively, dinethylformamide, 0.1 mol L
-1naOH solution, deionized water washed product for several times, is placed in baking oven dry, obtains pyromellitic acid anhydride and modifies loofah adsorbent.
Embodiment 4
(1) luffa pretreatment: luffa derives from ripe sponge gourd fruit, is obtained by peeling stoning, pulverizes, by 20 ~ 40 object sieve, obtain pretreatment luffa after the clear water cleaning, drying that are cut into small pieces by luffa;
(2) alkalize luffa: by 30g pretreatment luffa, be the NaOH solution of 5% by 200mL mass percentage concentration, soaking at room temperature 28 h, boil 40min again, spend deionized water after cooling to neutral, then put into isopropyl alcohol and soak 7 h, dry at 75 DEG C after suction filtration, obtain the luffa that alkalizes;
(3) luffa preparation modified by epoxychloropropane: in the reactor, add respectively, water: 35mL, epoxychloropropane: 33mL, NaOH:6g; Alkalization luffa: 26g, in 75 DEG C of constant temperature, stirring, back flow reaction 5 h, after cooling, spends deionized water, suction filtration, and to filtrate is neutrality, after a small amount of ethanol washing, vacuum drying, obtains epoxychloropropane and modify luffa.
(4) pyromellitic acid anhydride modifies loofah adsorbent preparation: in the reactor, add respectively, DMF: 88mL, pyromellitic acid anhydride: 3g, add epoxychloropropane after dissolving completely and modify luffa: 9g, after 75 DEG C of isothermal reaction 7h, suction filtration, uses N successively, dinethylformamide, 0.1 mol L
-1naOH solution, deionized water washed product for several times, is placed in baking oven dry, obtains pyromellitic acid anhydride and modifies loofah adsorbent.
Embodiment 5
(1) luffa pretreatment: luffa derives from ripe sponge gourd fruit, is obtained by peeling stoning, pulverizes, by 20 ~ 40 object sieve, obtain pretreatment luffa after the clear water cleaning, drying that are cut into small pieces by luffa;
(2) alkalize luffa: by 40g pretreatment luffa, be the NaOH solution of 4% by 200mL mass percentage concentration, soaking at room temperature 30 h, boil 40min again, spend deionized water after cooling to neutral, then put into isopropyl alcohol and soak 8h, dry at 75 DEG C after suction filtration, obtain the luffa that alkalizes;
(3) luffa preparation modified by epoxychloropropane: in the reactor, add respectively, water: 30mL, epoxychloropropane: 55mL, NaOH:4g; Alkalization luffa: 11g, in 70 DEG C of constant temperature, stirring, back flow reaction 5h, after cooling, spends deionized water, suction filtration, and to filtrate is neutrality, after a small amount of ethanol washing, vacuum drying, obtains epoxychloropropane and modify luffa.
(4) pyromellitic acid anhydride modifies loofah adsorbent preparation: in the reactor, add respectively, DMF: 34mL, pyromellitic acid anhydride: 3g, add epoxychloropropane after dissolving completely and modify luffa: 13g, after 75 DEG C of isothermal reaction 5 h, suction filtration, uses N successively, dinethylformamide, 0.1 mol L
-1naOH solution, deionized water washed product for several times, is placed in baking oven dry, obtains pyromellitic acid anhydride and modifies loofah adsorbent.
Embodiment 6
Pyromellitic acid anhydride modifies loofah adsorbent application process: the pyromellitic acid anhydride prepared being modified loofah adsorbent deionized water and soaks 2 h, is static adsorptive method by one, as follows to adsorption of metal ions operating procedure:
(1) initial concentration got containing lead ion is simulated wastewater 200 mL of 600mg/L;
(2) adjust ph is in 1.0 ~ 4.5 scopes;
(3) in simulated water sample, add pyromellitic acid anhydride modify loofah adsorbent, adsorbent amount is 1.0g/L water sample, concussion absorption 1h under room temperature;
(4) static concentration of getting supernatant Aas Determination of Lead In China ion, calculates adsorption capacity.
Result shows, it is 362.17 mgg to the maximum adsorption capacity of lead ion that pyromellitic acid anhydride of the present invention modifies loofah adsorbent
-1.
Detect the maximum adsorption capacity of pyromellitic acid anhydride modification loofah adsorbent to cadmium ion and copper ion in the same way and be respectively 181.78 mgg
-1with 171.71 mgg
-1.
Adsorption capacity and pyromellitic acid anhydride modify carboxyl-content consumption in loofah adsorbent, adsorption temp, solution system the factor such as pH value relevant.
Embodiment 7
Another kind is dynamic adsorption method, and the method adopting pyromellitic acid anhydride to modify loofah adsorbent Dynamic Adsorption carries out water treatment, as follows to adsorption of metal ions operating procedure:
(1) soaked pyromellitic acid anhydride is modified loofah adsorbent wet method and load adsorption column;
(2) initial concentration got containing lead ion is simulated wastewater 200 mL of 600mg/L;
(3) adjust ph is in 1.0 ~ 4.5 scopes;
(4) solution passes through adsorption column with the flow velocity of 5 mL/min;
(5) by the concentration of the lead ion on aas determination efflux and post.
Result shows, it is 362.17 mgg to the maximum adsorption capacity of lead ion that pyromellitic acid anhydride of the present invention modifies loofah adsorbent
-1.
Detect the maximum adsorption capacity of pyromellitic acid anhydride modification loofah adsorbent to cadmium ion and copper ion in the same way and be respectively 181.78 mgg
-1with 171.71 mgg
-1.
The rule of its absorption is the same, and it is relevant that adsorption capacity and pyromellitic acid anhydride modify the factors such as loofah adsorbent carboxyl-content consumption, adsorption temp, the pH value of solution system, the flow velocity of solution.
Pyromellitic acid anhydride modifies luffa to Cd
2+adsorption capacity can up to 181.78 mgg
-1, to Pb
2+maximal absorptive capacity be 362.17 mgg
-1, to Cu
2+maximal absorptive capacity be 171.71 mgg
-1, most high adsorption rate can reach 98%.
Claims (1)
1. pyromellitic acid anhydride modifies a loofah adsorbent preparation method, and it is characterized in that, the method has following processing step:
(1) luffa pretreatment: luffa derives from ripe sponge gourd fruit, is obtained by peeling stoning, pulverizes, by 20 ~ 40 object sieve, obtain pretreatment luffa after the clear water cleaning, drying that are cut into small pieces by luffa;
(2) alkalize luffa: by pretreatment luffa by 100 ~ 250g/L solid-to-liquid ratio, be the NaOH solution of 2 ~ 5% by mass percentage concentration, soaking at room temperature 24 ~ 36h, boil 20 ~ 50min again, deionized water is spent to neutral after cooling, put into isopropyl alcohol again and soak 6 ~ 10h, dry at 75 DEG C after suction filtration, obtain the luffa that alkalizes;
(3) luffa preparation modified by epoxychloropropane: in the reactor, add by mass percentage, water: 25 ~ 40%, epoxychloropropane: 30 ~ 58%, NaOH:3 ~ 8%, alkalization luffa: 8 ~ 26%, each component sum is absolutely, in 70 ~ 75 DEG C of constant temperature, stirring, back flow reaction 4 ~ 6h, after cooling, spend deionized water, suction filtration, to filtrate is neutrality, after a small amount of ethanol washing, vacuum drying, obtains epoxychloropropane and modifies luffa;
(4) pyromellitic acid anhydride modifies loofah adsorbent preparation: in the reactor, add by following composition mass percent, DMF: 68 ~ 88%, pyromellitic acid anhydride: 3.0 ~ 10%, add epoxychloropropane after dissolving completely and modify luffa: 8 ~ 25%, each component sum is absolutely, after 70 ~ 80 DEG C of isothermal reaction 5 ~ 8h, suction filtration, use DMF successively, 0.1molL
-1naOH solution, deionized water washed product for several times, is placed in baking oven dry, obtains pyromellitic acid anhydride and modifies loofah adsorbent.
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| CN103933950B (en) * | 2014-05-07 | 2015-10-21 | 济南大学 | A kind of preparation method of luffa solid-loaded ionic-liquid adsorbent |
| CN104084143A (en) * | 2014-07-23 | 2014-10-08 | 武汉理工大学 | Preparation method of function material in biomass water treatment environment |
| CN104815618A (en) * | 2015-04-27 | 2015-08-05 | 宁夏医科大学 | Preparation method of astragalus residue bio-absorbent |
| CN105618001B (en) * | 2016-02-17 | 2017-09-22 | 济南大学 | A kind of preparation of Cocoamidopropyl betaine modified loofah sponge adsorbent |
| CN106423108A (en) * | 2016-09-24 | 2017-02-22 | 北京益净环保设备科技有限公司 | Granular adsorbent for adsorbing thiophene and preparation method thereof |
| CN109569526A (en) * | 2018-12-14 | 2019-04-05 | 肇庆医学高等专科学校 | A kind of modified pomelo peel of pyromellitic acid anhydride is to medicine wastewater treatment method |
| CN110038526A (en) * | 2019-03-21 | 2019-07-23 | 济南大学 | A kind of preparation method for the magnetic porous wool adsorbent of separating-purifying catechin |
| CN115228444A (en) * | 2022-06-08 | 2022-10-25 | 湖北科技学院 | Radiation preparation method of loofah sponge-based adsorbent capable of efficiently adsorbing cationic dye |
| CN115634672B (en) * | 2022-11-03 | 2024-01-26 | 内蒙古农业大学 | Pyromellitic anhydride modified polyvinyl amine gel and preparation method, application and regeneration method thereof |
| CN118162115B (en) * | 2024-05-13 | 2024-08-16 | 常熟理工学院 | Multifunctional group modified loofah sponge heavy metal adsorbent and preparation method thereof |
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| CN101239306A (en) * | 2008-03-18 | 2008-08-13 | 上海大学 | Method for preparing etherification luffa and application of it in metallic ion adsorption |
| CN101480606B (en) * | 2008-12-26 | 2011-07-20 | 合肥学院 | Adsorbing substance for absorbing heavy metal ion and preparation method thereof |
| CN102430393B (en) * | 2011-09-19 | 2013-12-25 | 济南大学 | Citric acid loofah sponge preparation method and application |
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