CN103566907A - 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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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 the adsorbent of metal ion in aqueous systems, particularly a kind of pyromellitic acid anhydride is modified luffa preparation method and the adsorption applications to heavy metal ion.
Background technology
Along with socioeconomic, develop rapidly, the fast development of industry, also more and more to the heavy metal ion content discharging in our surrounding environment, day by day serious to the pollution of surrounding environment, not only destroyed environment also to people's life with healthyly form potential threat.Different from organic pollution, these materials containing heavy metal not only can not be divided and take off by microorganism in the environment of ours around, can also enter food chain progressively accumulates, even some constantly also can be changed to the thing larger to our human health risk under effect in microorganism, biological metabolism is damaged, and then health and environment are had to very large threat.And water is not inexhaustible.Therefore, prevent and treat tellurian contaminated wastewater, protect environment that we depend on for existence to become the problem of people's concern.Heavy Metal Pollution Control is a current whole world important environmental problem urgently to be resolved hurrily, thereby also becomes a study hotspot of scientific domain.
Shortage of resources and environmental pollution have become two large subject matters of the world today, along with the minimizing day by day of current available resources, and the realizing and utilize the attention be day by day subject to the mankind of renewable resource.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 to environment the benefits such as secondary pollution, therefore received a lot of scientific research personnel's concern, therefore, utilize natural reproducible resource, the friendly type product of development environment and technology will become the inexorable trend of sustainable development.Luffa is vascular bundle in the ripening fruits of the Curcurbitaceae annual herb plant sponge gourd withered old fruit of 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 very abundant regenerated resources of the earth, 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%, to the maximal absorptive capacity of methylene blue, is 316mg/g, high adsorption rate can reach 96.2%, has carboxylic acid characteristic, direct absorption and the wash-out to each metal ion species, organic dyestuff in water body,
Due to the special construction of pyromellitic acid anhydride, it has very high chemism, to heavy metal ion adsorbed, can control by the pH value of system, when different pH values, metal ion is selectively adsorbed.This patent be take cocoanut shell as support material, adopts pyromellitic acid anhydride (PMDA) to carry out chemical modification, on cocoanut shell surface, introduces carboxyl active function groups, and its adsorption capacity to heavy metal ion is obviously strengthened.Acidity by regulation system makes each metal ion species reach separated object.
Summary of the invention
One of object of the present invention is to provide a kind of pyromellitic acid anhydride and modifies luffa absorbent preparation method, and it is larger that the pyromellitic acid anhydride that mainly makes to obtain is modified luffa adsorbent adsorption capacity to heavy metal ion in aqueous systems.
Object of the present invention is achieved through the following technical solutions.
Modify a luffa absorbent preparation method, be characterised in that the method has following processing step:
(1) luffa pretreatment: luffa derives from ripe 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 ~ 40 object sieve, obtains pretreatment luffa;
(2) alkalization luffa: pretreatment luffa is pressed to 100 ~ 250g/L solid-to-liquid ratio, the NaOH solution that is 2 ~ 5% by percentage concentration, soaking at room temperature 24 ~ 36 h, boil again 20 ~ 50min, cooling rear extremely neutral with deionized water washing, put into again isopropyl alcohol and soak 6 ~ 10 h, after suction filtration, at 75 ℃, dry, obtain the luffa that alkalizes;
(3) epoxychloropropane is modified luffa preparation: in 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 ℃ of constant temperature, stirring, back flow reaction 4 ~ 6 h, after cooling, with deionized water washing, suction filtration, till being neutrality to filtrate, with after a small amount of ethanol washing, vacuum drying, obtains epoxychloropropane and modifies luffa.
(4) pyromellitic acid anhydride is modified luffa absorbent preparation: in reactor, by following composition mass percent, add DMF: 68 ~ 88%, pyromellitic acid anhydride: 3.0 ~ 10%, after dissolving completely, add epoxychloropropane to modify luffa: 8 ~ 25%, each component sum is absolutely, after 70 ~ 80 ℃ of isothermal reaction 5 ~ 8 h, suction filtration, use successively DMF, 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 luffa adsorbent.
Another object of the present invention be to provide a kind of pyromellitic acid anhydride modify luffa adsorbent in aqueous systems to heavy metal ion adsorbed application, feature is: the pyromellitic acid anhydride preparing is modified to luffa adsorbent and by deionized water, soak 1 ~ 3h, by static method, adsorb.
The pyromellitic acid anhydride preparing can also be modified to luffa adsorbent and soak 1 ~ 3 h by deionized water, by dynamic method, adsorb.
Advantage of the present invention and effect are:
The invention has the beneficial effects as follows: the pyromellitic acid anhydride of acquisition is modified luffa to Cd
2+adsorption capacity can be 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, high adsorption rate can reach 98%, can be directly to the absorption of metal ion species in water body and wash-out, adsorption efficiency is high, and the speed of absorption is fast, selectively strong, desorption performance is good, has good physical and chemical stability and excellent mechanical stability, can within the scope of wider soda acid, use; There is larger adsorption capacity, water penetration is better, the stronger Reusability of power of regeneration is often; The more important thing is that luffa is natural macromolecular material, so not only saved raw-material cost but also realized twice laid; Luffa is that biological raw material can biodegradation, uses this adsorbent environmentally safe; Technique of the present invention 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 is modified luffa.
The specific embodiment
Embodiment 1
(1) luffa pretreatment: luffa derives from ripe 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 ~ 40 object sieve, obtains pretreatment luffa;
(2) alkalization luffa: by 20g pretreatment luffa, the NaOH solution that is 5% by 200mL mass percentage concentration, soaking at room temperature 24 h, boil again 30min, cooling rear extremely neutral with deionized water washing, then put into isopropyl alcohol and soak 8 h, after suction filtration, at 75 ℃, dry, obtain the luffa that alkalizes;
(3) epoxychloropropane is modified luffa preparation: in reactor, add respectively water: 25mL, epoxychloropropane: 50mL, NaOH:5g; Alkalization luffa: 20g, in 70 ℃ of constant temperature, stirring, back flow reaction 5 h, cooling after, with deionized water washing, suction filtration, till being neutrality to filtrate, with after a small amount of ethanol washing, vacuum drying, obtains epoxychloropropane modification luffa.
(4) pyromellitic acid anhydride is modified luffa absorbent preparation: in reactor, add respectively, DMF: 75mL, pyromellitic acid anhydride: 5g, after dissolving completely, add epoxychloropropane to modify luffa: 20g, after 75 ℃ 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 luffa adsorbent.
(1) luffa pretreatment: luffa derives from ripe 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 ~ 40 object sieve, obtains pretreatment luffa;
(2) alkalization luffa: by 20g pretreatment luffa, the NaOH solution that is 3% by 100mL mass percentage concentration, soaking at room temperature 36 h, boil again 40min, cooling rear extremely neutral with deionized water washing, then put into isopropyl alcohol and soak 10 h, after suction filtration, at 75 ℃, dry, obtain the luffa that alkalizes;
(3) epoxychloropropane is modified luffa preparation: in reactor, add respectively water: 25mL, epoxychloropropane: 30mL, NaOH:2g; Alkalization luffa: 8g, in 75 ℃ of constant temperature, stirring, back flow reaction 4h, cooling after, with deionized water washing, suction filtration, till being neutrality to filtrate, with after a small amount of ethanol washing, vacuum drying, obtains epoxychloropropane modification luffa.
(4) pyromellitic acid anhydride is modified luffa absorbent preparation: in reactor, add respectively, DMF: 40mL, pyromellitic acid anhydride: 2g, after dissolving completely, add epoxychloropropane to modify luffa: 8g, after 70 ℃ 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 luffa adsorbent.
Embodiment 3
(1) luffa pretreatment: luffa derives from ripe 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 ~ 40 object sieve, obtains pretreatment luffa;
(2) alkalization luffa: by 50g pretreatment luffa, the NaOH solution that is 4% by 200mL mass percentage concentration, soaking at room temperature 30 h, boil again 50min, cooling rear extremely neutral with deionized water washing, then put into isopropyl alcohol and soak 6h, after suction filtration, at 75 ℃, dry, obtain the luffa that alkalizes;
(3) epoxychloropropane is modified luffa preparation: in reactor, add respectively water: 20mL, epoxychloropropane: 30mL, NaOH:4g; Alkalization luffa: 16g, in 70 ℃ of constant temperature, stirring, back flow reaction 6h, cooling after, with deionized water washing, suction filtration, till being neutrality to filtrate, with after a small amount of ethanol washing, vacuum drying, obtains epoxychloropropane modification luffa.
(4) pyromellitic acid anhydride is modified luffa absorbent preparation: in reactor, add respectively, DMF: 43mL, pyromellitic acid anhydride: 2g, after dissolving completely, add epoxychloropropane to modify luffa: 15g, after 80 ℃ 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 luffa adsorbent.
Embodiment 4
(1) luffa pretreatment: luffa derives from ripe 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 ~ 40 object sieve, obtains pretreatment luffa;
(2) alkalization luffa: by 30g pretreatment luffa, the NaOH solution that is 5% by 200mL mass percentage concentration, soaking at room temperature 28 h, boil again 40min, cooling rear extremely neutral with deionized water washing, then put into isopropyl alcohol and soak 7 h, after suction filtration, at 75 ℃, dry, obtain the luffa that alkalizes;
(3) epoxychloropropane is modified luffa preparation: in reactor, add respectively water: 35mL, epoxychloropropane: 33mL, NaOH:6g; Alkalization luffa: 26g, in 75 ℃ of constant temperature, stirring, back flow reaction 5 h, cooling after, with deionized water washing, suction filtration, till being neutrality to filtrate, with after a small amount of ethanol washing, vacuum drying, obtains epoxychloropropane modification luffa.
(4) pyromellitic acid anhydride is modified luffa absorbent preparation: in reactor, add respectively, DMF: 88mL, pyromellitic acid anhydride: 3g, after dissolving completely, add epoxychloropropane to modify luffa: 9g, after 75 ℃ 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 luffa adsorbent.
Embodiment 5
(1) luffa pretreatment: luffa derives from ripe 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 ~ 40 object sieve, obtains pretreatment luffa;
(2) alkalization luffa: by 40g pretreatment luffa, the NaOH solution that is 4% by 200mL mass percentage concentration, soaking at room temperature 30 h, boil again 40min, cooling rear extremely neutral with deionized water washing, then put into isopropyl alcohol and soak 8h, after suction filtration, at 75 ℃, dry, obtain the luffa that alkalizes;
(3) epoxychloropropane is modified luffa preparation: in reactor, add respectively water: 30mL, epoxychloropropane: 55mL, NaOH:4g; Alkalization luffa: 11g, in 70 ℃ of constant temperature, stirring, back flow reaction 5h, cooling after, with deionized water washing, suction filtration, till being neutrality to filtrate, with after a small amount of ethanol washing, vacuum drying, obtains epoxychloropropane modification luffa.
(4) pyromellitic acid anhydride is modified luffa absorbent preparation: in reactor, add respectively, DMF: 34mL, pyromellitic acid anhydride: 3g, after dissolving completely, add epoxychloropropane to modify luffa: 13g, after 75 ℃ 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 luffa adsorbent.
Embodiment 6
Pyromellitic acid anhydride is modified luffa adsorbent application process: the pyromellitic acid anhydride preparing is modified to luffa adsorbent and by deionized water, soaks 2 h, by a kind of be static adsorptive method, as follows to adsorption of metal ions operating procedure:
(1) get simulated wastewater 200 mL that the initial concentration containing lead ion is 600mg/L;
(2) regulate pH value in 1.0 ~ 4.5 scopes;
(3) in simulated water sample, add pyromellitic acid anhydride to modify luffa adsorbent, adsorbent consumption is 1.0g/L water sample, concussion absorption 1h under room temperature;
(4) the static concentration of Aas Determination of Lead In China ion for supernatant, the calculating adsorption capacity of getting.
Result shows, it is 362.17 mgg to the maximum adsorption capacity of lead ion that pyromellitic acid anhydride of the present invention is modified luffa adsorbent
-1.
With same method, detect pyromellitic acid anhydride modification luffa adsorbent the maximum adsorption capacity of cadmium ion and copper ion is respectively to 181.78 mgg
-1with 171.71 mgg
-1.
It is relevant that adsorption capacity and pyromellitic acid anhydride are modified the factors such as pH value of carboxyl-content consumption in luffa adsorbent, adsorption temp, solution system.
Embodiment 7
Another kind is dynamic adsorption method, adopts pyromellitic acid anhydride to modify luffa adsorbent and carries out water treatment by the method for Dynamic Adsorption, as follows to adsorption of metal ions operating procedure:
(1) soaked pyromellitic acid anhydride is modified to luffa adsorbent wet method and packed into adsorption column;
(2) get simulated wastewater 200 mL that the initial concentration containing lead ion is 600mg/L;
(3) regulate pH value in 1.0 ~ 4.5 scopes;
(4) solution passes through adsorption column with the flow velocity of 5 mL/min;
(5) use 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 is modified luffa adsorbent
-1.
With same method, detect pyromellitic acid anhydride modification luffa adsorbent the maximum adsorption capacity of cadmium ion and copper ion is respectively to 181.78 mgg
-1with 171.71 mgg
-1.
The rule of its absorption is the same, and adsorption capacity is modified luffa adsorbent carboxyl-content consumption, adsorption temp, the pH value of solution system, the factors such as flow velocity of solution are relevant with pyromellitic acid anhydride.
Pyromellitic acid anhydride is modified luffa to Cd
2+adsorption capacity can be 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, high adsorption rate can reach 98%.
Claims (5)
1. pyromellitic acid anhydride is modified a luffa absorbent preparation method, it is characterized in that: be that the method has following processing step:
(1) luffa pretreatment: luffa derives from ripe 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 ~ 40 object sieve, obtains pretreatment luffa;
(2) alkalization luffa: pretreatment luffa is pressed to 100 ~ 250g/L solid-to-liquid ratio, the NaOH solution that is 2 ~ 5% by percentage concentration, soaking at room temperature 24 ~ 36 h, boil again 20 ~ 50min, cooling rear extremely neutral with deionized water washing, put into again isopropyl alcohol and soak 6 ~ 10 h, after suction filtration, at 75 ℃, dry, obtain the luffa that alkalizes;
(3) epoxychloropropane is modified luffa preparation: in reactor, add respectively water: 25 ~ 40%, and epoxychloropropane: 30 ~ 58%,, NaOH:3 ~ 8%; Alkalization luffa: 8 ~ 26%, each component sum is absolutely, in 70 ~ 75 ℃ of constant temperature, stirring, back flow reaction 4 ~ 6 h, after cooling, with deionized water washing, suction filtration, till being neutrality to filtrate, with after a small amount of ethanol washing, vacuum drying, obtains epoxychloropropane and modifies luffa;
(4) pyromellitic acid anhydride is modified luffa absorbent preparation: in reactor, by following composition mass percent, add DMF: 68 ~ 88%, pyromellitic acid anhydride: 3.0 ~ 10%, after dissolving completely, add epoxychloropropane to modify luffa: 8 ~ 25%, each component sum is absolutely, after 70 ~ 80 ℃ of isothermal reaction 5 ~ 8 h, suction filtration, use successively DMF, 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 luffa adsorbent.
2. according to a kind of pyromellitic acid anhydride described in claim 1, modify luffa absorbent preparation method, it is characterized in that: the water in step (3) and the volume ratio of epoxychloropropane are between 1:0.75 ~ 2.2.
3. according to a kind of pyromellitic acid anhydride described in claim 1, modify luffa absorbent preparation method, it is characterized in that: the pyromellitic acid anhydride in step (4) will keep dry.
4. according to a kind of pyromellitic acid anhydride described in claim 1, modify luffa absorbent preparation method, it is characterized in that: the DMF in step (4) will be gone out moisture before using.
5. according to the pyromellitic acid anhydride of claim 1 preparation, modify luffa adsorbent applies lead ion, cadmium ion, copper absorption in water.
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