CN103691408A - Succinic anhydride modified wild reed stem adsorbent as well as preparation and application thereof - Google Patents
Succinic anhydride modified wild reed stem adsorbent as well as preparation and application thereof Download PDFInfo
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Abstract
The invention relates to a succinic anhydride modified wild reed stem adsorbent as well as preparation and an application thereof. The preparation comprises steps as follows: 1) reed stem powder is added into a round-bottom flask, then succinic anhydride is added, pyridine is taken as a solvent, condensation and backflow is performed by an air condenser under the condition of constant temperature oil bath, a Buchner funnel is used for suction filtration after cooling, distilled water and ethanol are used respectively for alternate clean washing, a product is placed into an air dry oven, dried and placed into a dryer for standby application; and 2) the reed stem obtained in the step 1) is stirred in a saturated sodium bicarbonate solution, then subjected to suction filtration by the Buchner funnel and alternate clean washing by the distilled water and ethanol, is dried continuously, packed into a bag and stored in the dryer. A novel adsorbing material obtained by the invention has better adsorption for cationic dye, metal ions and the like, a better method is provided for comprehensive utilization of the reed stem, and certain application prospect is provided.
Description
Technical field
The invention belongs to technical field of water pollution control, be specifically related to preparation method and application that succinic anhydride is modified wild reed straw new adsorbent.
Background technology
Dyeing waste water is that a class COD is high, and colourity is high, and biochemical is poor, and discharge capacity is large and be difficult to one of industrial wastewater of administering, and wherein decolouring is the key of administering.2007, China Dyestuffs, organic pigment output added up to 95.32 ten thousand tons, and in DYE PRODUCTION process, nearly 10～15% dyestuff can directly enter in environment and produce a large amount of waste water from dyestuff with waste water, to environment and healthy generation major hidden danger.The method of industrial dye wastewater treatment using has: absorption method, chemical coagulation method, oxidizing process, filtration method and biological treatment.Wherein, the method for absorption is disposed of sewage, and has easy to operately, and equipment is simple, efficient and with low cost, adsorbent can recycling utilization etc. feature.The modification reed straw new adsorbent that this research is selected, just to Handling Waste Water by Absorbing Way research field expansion.
The plant that reed is a kind of wide adaptability, strong stress resistance, biomass is high, all has growth all over the world.In reed, except containing necessary various high nutrition amino acid, crude protein and carbohydrate, content of cellulose is higher, is one of suitable raw material as biological substance adsorbent.Cellulose and many polymer substances have good affinity, thereby shown certain absorption property, the lignin containing in its structure, cellulose and hemicellulose itself can be used as active group and are applied to wastewater treatment, but compared with low, make its application limited because of its absorption property.At present, application succinic anhydride is modified wild reed straw and be have not been reported for the treatment of waste water as adsorbent.
Summary of the invention
The object of this invention is to provide a kind of operating procedure wild reed straw new adsorbent of modifying with succinic anhydride simple, with low cost and its preparation method and application, improve the absorption property of wild reed straw, strengthen its utilization ratio.
The present invention solves the problems of the technologies described above adopted technical scheme: succinic anhydride is modified wild reed rod adsorbent, and it is following preparation method's products therefrom, includes following steps:
1) getting 2.0g reed straw powder joins in round-bottomed flask, the 3.0g succinic anhydride that adds again accurate weighing, using 40mL pyridine as solvent, under the constant temperature oil bath condition of 120 ℃, use air set pipe condensing reflux 5h, coolingly use Buchner funnel suction filtration afterwards, then by distilled water and volume fraction, be that 95% ethanol is alternately rinsed well respectively, put in air dry oven, at 60 ℃, dry 24h, is placed in drier standby;
2) step 1) gained reed straw is stirred to 0.5h in saturated sodium bicarbonate solution, then use Buchner funnel suction filtration, with distilled water and volume fraction 95% ethanol, alternately rinse well respectively, continue dry 24h at 60 ℃ of temperature, pack in bag, be placed in drier and store.
Described succinic anhydride is modified the preparation method of wild reed rod adsorbent, includes following steps:
1) getting 2.0g reed straw powder joins in round-bottomed flask, the 3.0g succinic anhydride that adds again accurate weighing, using 40mL pyridine as solvent, under the constant temperature oil bath condition of 120 ℃, use air set pipe condensing reflux 5h, coolingly use Buchner funnel suction filtration afterwards, then by distilled water and volume fraction, be that 95% ethanol is alternately rinsed well respectively, put in air dry oven, at 60 ℃, dry 24h, is placed in drier standby;
2) step 1) gained reed straw is stirred to 0.5h in saturated sodium bicarbonate solution, then use Buchner funnel suction filtration, with distilled water and volume fraction 95% ethanol, alternately rinse well respectively, continue dry 24h at 60 ℃ of temperature, pack in bag, be placed in drier and store.
Succinic anhydride modify wild reed rod adsorbent at industrial dye waste water or in containing metal ion cadmium waste water or containing the plumbous waste water of metal ion as the application of adsorbent.
Press such scheme, described industrial dye waste water is Crystal Violet Dye waste water or methylene blue dye waste water.
Press such scheme, application process is: take 0.01-0.10g succinic anhydride and modify wild reed rod adsorbent, joining concentration is 100-1000mg L
-1crystal violet or methylene blue dye waste water in, take acid or alkali adjusting pH value after 2-10.00, be placed on the water bath chader of 15-70 ℃ and shake 1-24 hour, the concentration of crystal violet in supernatant is measured in centrifugation, according to the concentration difference of crystal violet or methylene blue in water before and after absorption, determine its adsorption effect to crystal violet in water or methylene blue.
Press such scheme, regulating the alkali of pH value is NaOH, and acid is hydrochloric acid.
Press such scheme, the concussion speed of water-bath constant temperature oscillator is 50-300rpm.
Wild reed planting of the present invention is widely distributed, strong adaptability, material is easy to get and is cheap, in its stalk institutional framework, contain the compositions such as a large amount of celluloses and hemicellulose, can to its surface, carry out finishing with the little molecule succinic anhydride of polyfunctional group, increase the absorption property of stalk to pollutants such as the dye of positive ion, metal ions.The chemical modification method of this invention is simple, and reaction unit is easy to get, and method of operating is easily gone, and resulting novel absorption material has good absorption property to the dye of positive ion, metal ion etc.The comprehensive utilization that the present invention is reed straw provides good method, has certain application prospect.
Accompanying drawing explanation
Fig. 1 is the scanning electron microscope diagram (* 4000) of wild reed straw.
The specific embodiment
Below by specific embodiment, further illustrate the present invention, rather than limit the scope of the invention.
Embodiment 1
Succinic anhydride is modified the preparation method of wild reed rod adsorbent, includes following steps:
1) physical treatment of material:
It is 1cm left and right segment that wild reed stalk is cut into length, after soaking, washes away dust with running water, under the condition of 55 ℃, dries 24h, then with mixer, is clayed into power, and crosses 80 mesh sieves, leaves and takes the lower reed straw powder of sieve, is placed in drier standby.
2) getting 2.0g reed straw powder joins in round-bottomed flask, the 3.0g succinic anhydride that adds again accurate weighing, using 40mL pyridine as solvent, under the constant temperature oil bath condition of 120 ℃, use air set pipe condensing reflux 5h, coolingly use Buchner funnel suction filtration afterwards, then by distilled water and volume fraction, be that 95% ethanol is alternately rinsed well respectively, put in air dry oven, at 60 ℃, dry 24h, is placed in drier standby;
3) step 1) gained reed straw is stirred to 0.5h in saturated sodium bicarbonate solution, then use Buchner funnel suction filtration, with distilled water and volume fraction 95% ethanol, alternately rinse well respectively, continue dry 24h at 60 ℃ of temperature, pack in bag, be placed in drier and store.
Embodiment 2
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 100mg L
-1the Crystal Violet Dye aqueous solution, the pH value of dye solution is 6.1, the speed concussion 24h at 25 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (588nm) of crystal violet to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains Crystal Violet is 99.26%.
Embodiment 3
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 200mg L
-1the Crystal Violet Dye aqueous solution, the pH value of dye solution is 6.1, the speed concussion 24h at 25 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (588nm) of crystal violet to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains Crystal Violet is 99.83%.
Embodiment 4
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 300mg L
-1the Crystal Violet Dye aqueous solution, the pH value of dye solution is 6.1, the speed concussion 24h at 25 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (588nm) of crystal violet to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains Crystal Violet is 99.87%.
Embodiment 5
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 400mg L
-1the Crystal Violet Dye aqueous solution, the pH value of dye solution is 6.1, the speed concussion 24h at 25 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (588nm) of crystal violet to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains Crystal Violet is 99.51%.
Embodiment 6
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 500mg L
-1the Crystal Violet Dye aqueous solution, the pH value of dye solution is 6.1, the speed concussion 24h at 25 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (588nm) of crystal violet to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains Crystal Violet is 96.59%.
Embodiment 7
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 400mg L
-1the Crystal Violet Dye aqueous solution, with hydrochloric acid, regulating the pH value of dye solution is 4.0, the speed concussion 24h at 25 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (588nm) of crystal violet to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains Crystal Violet is 99.16%.
Embodiment 8
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 400mg L
-1the Crystal Violet Dye aqueous solution, with hydrochloric acid, regulating the pH value of dye solution is 5.0, the speed concussion 24h at 25 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (588nm) of crystal violet to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains Crystal Violet is 98.17%.
Embodiment 9
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 400mg L
-1the Crystal Violet Dye aqueous solution, regulating the pH value of dye solution is 7, the speed concussion 24h at 25 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (588nm) of crystal violet to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains Crystal Violet is 97.35%.
Embodiment 10
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 400mg L
-1the Crystal Violet Dye aqueous solution, with NaOH, regulating the pH value of dye solution is 8, the speed concussion 24h at 25 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (588nm) of crystal violet to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains Crystal Violet is 99.16%.
Embodiment 11
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 400mg L
-1the Crystal Violet Dye aqueous solution, with NaOH, regulating the pH value of dye solution is 9, the speed concussion 24h at 25 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (588nm) of crystal violet to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains Crystal Violet is 98.27%.
Embodiment 12
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 400mg L
-1the Crystal Violet Dye aqueous solution, with NaOH, regulating the pH value of dye solution is 10, the speed concussion 24h at 25 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (588nm) of crystal violet to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains Crystal Violet is 9.32%.
Embodiment 13
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 400mg L
-1the Crystal Violet Dye aqueous solution, the pH value of dye solution is 6.1, the speed concussion 24h at 20 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (588nm) of crystal violet to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains Crystal Violet is 99.38%.
Embodiment 14
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 400mg L
-1the Crystal Violet Dye aqueous solution, the pH value of dye solution is 6.1, the speed concussion 24h at 30 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (588nm) of crystal violet to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains Crystal Violet is 99.77%.
Embodiment 15
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 400mg L
-1the Crystal Violet Dye aqueous solution, the pH value of dye solution is 6.1, the speed concussion 24h at 40 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (588nm) of crystal violet to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains Crystal Violet is 99.75%.
Embodiment 16
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 400mg L
-1the Crystal Violet Dye aqueous solution, the pH value of dye solution is 6.1, the speed concussion 24h at 50 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (588nm) of crystal violet to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains Crystal Violet is 99.68%.
Embodiment 17
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 400mg L
-1the Crystal Violet Dye aqueous solution, the pH value of dye solution is 6.1, the speed concussion 24h at 60 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (588nm) of crystal violet to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains Crystal Violet is 99.44%.
The prepared adsorbent of embodiment 1 is applied to the absorption of other common dyestuffs and heavy metal ion:
Embodiment 18
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 100mg L
-1the methylene blue dye aqueous solution, the pH value of dye solution is 6.5, the speed concussion 24h at 25 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (670nm) of methylene blue to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains dyestuff methylene blue is 99.85%.
Embodiment 19
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 200mg L
-1the methylene blue dye aqueous solution, the pH value of dye solution is 6.5, the speed concussion 24h at 25 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (670nm) of methylene blue to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains dyestuff methylene blue is 99.82%.
Embodiment 20
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 300mg L
-1the methylene blue dye aqueous solution, the pH value of dye solution is 6.5, the speed concussion 24h at 25 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (670nm) of methylene blue to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains dyestuff methylene blue is 99.84%.
Embodiment 21
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 400mg L
-1the methylene blue dye aqueous solution, the pH value of dye solution is 6.5, the speed concussion 24h at 25 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (670nm) of methylene blue to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains dyestuff methylene blue is 99.81%.
Embodiment 22
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 500mg L
-1the methylene blue dye aqueous solution, the pH value of dye solution is 6.5, the speed concussion 24h at 25 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (670nm) of methylene blue to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains dyestuff methylene blue is 99.51%.
Embodiment 23
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 400mg L
-1the methylene blue dye aqueous solution, with hydrochloric acid, regulating the pH value of dye solution is 4.0, the speed concussion 24h at 25 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (670nm) of methylene blue to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains dyestuff methylene blue is 99.80%.
Embodiment 24
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 400mg L
-1the methylene blue dye aqueous solution, with hydrochloric acid, regulating the pH value of dye solution is 5.0, the speed concussion 24h at 25 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (670nm) of methylene blue to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains dyestuff methylene blue is 99.89%.
Embodiment 25
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 400mg L
-1the methylene blue dye aqueous solution, regulating the pH value of dye solution is 6.0, the speed concussion 24h at 25 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (670nm) of methylene blue to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains dyestuff methylene blue is 99.89%.
Embodiment 26
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 400mg L
-1the methylene blue dye aqueous solution, with NaOH, regulating the pH value of dye solution is 7.0, the speed concussion 24h at 25 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (670nm) of methylene blue to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains dyestuff methylene blue is 99.92%.
Embodiment 27
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 400mg L
-1the methylene blue dye aqueous solution, with NaOH, regulating the pH value of dye solution is 8.0, the speed concussion 24h at 25 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (670nm) of methylene blue to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains dyestuff methylene blue is 99.92%.
Embodiment 28
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 400mg L
-1the methylene blue dye aqueous solution, with NaOH, regulating the pH value of dye solution is 9.0, the speed concussion 24h at 25 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (670nm) of methylene blue to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains dyestuff methylene blue is 99.88%.
Embodiment 29
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 400mg L
-1the methylene blue dye aqueous solution, with NaOH, regulating the pH value of dye solution is 10.0, the speed concussion 24h at 25 ℃ of water bath chaders with 150rpm.When absorption reaches after balance, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, the supernatant obtaining is surveyed under the maximum absorption wavelength (670nm) of methylene blue to its absorbance with spectrophotometer, detect the wherein concentration of excess dye, thereby draw the amount of adsorbing on adsorbent, calculate the adsorption capacity of this new adsorbent.The clearance that obtains dyestuff methylene blue is 99.83%.
Embodiment 30
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 25mg L
-1metal ion cadmium (Cd
+ 2) the aqueous solution, the pH value of metal ion solution is 5.0, speed concussion 1h at 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, and the supernatant obtaining is detected to the wherein concentration of residual metallic ion with atomic absorption spectrophotometer, thereby the clearance that obtains metal ion cadmium is 97.70%.
Embodiment 31
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 50mg L
-1metal ion cadmium (Cd
+ 2) the aqueous solution, the pH value of metal ion solution is 5.0, speed concussion 1h at 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, and the supernatant obtaining is detected to the wherein concentration of residual metallic ion with atomic absorption spectrophotometer, thereby the clearance that obtains metal ion cadmium is 98.79%.
Embodiment 32
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 100mg L
-1metal ion cadmium (Cd
+ 2) the aqueous solution, the pH value of metal ion solution is 5.0, speed concussion 1h at 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, and the supernatant obtaining is detected to the wherein concentration of residual metallic ion with atomic absorption spectrophotometer, thereby the clearance that obtains metal ion cadmium is 94.98%.
Embodiment 33
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 50mg L
-1plumbous (the Pb of metal ion
+ 2) the aqueous solution, the pH value of metal ion solution is 6.2, speed concussion 1h at 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, and the supernatant obtaining is detected to the wherein concentration of residual metallic ion with atomic absorption spectrophotometer, thereby the clearance that obtains metal ion cadmium is 99.21%.
Embodiment 34
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 100mg L
-1plumbous (the Pb of metal ion
+ 2) the aqueous solution, the pH value of metal ion solution is 6.2, speed concussion 1h at 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, and the supernatant obtaining is detected to the wherein concentration of residual metallic ion with atomic absorption spectrophotometer, thereby the clearance that obtains metal ion cadmium is 99.61%.
Embodiment 35
50mg embodiment 1 gained succinic anhydride is modified to wild reed straw and insert in 250mL tool plug conical flask, adding 50mL concentration is 200mg L
-1plumbous (the Pb of metal ion
+ 2) the aqueous solution, the pH value of metal ion solution is 6.2, speed concussion 1h at 25 ℃ of water bath chaders with 150rpm, then, take out conical flask, inclining, it is separated with solid by solution solution rotating speed with 10000rpm on centrifuge, and the supernatant obtaining is detected to the wherein concentration of residual metallic ion with atomic absorption spectrophotometer, thereby the clearance that obtains metal ion cadmium is 99.77%.
Claims (7)
1. succinic anhydride is modified wild reed rod adsorbent, and it is following preparation method's products therefrom, includes following steps:
1) getting 2.0g reed straw powder joins in round-bottomed flask, the 3.0g succinic anhydride that adds again accurate weighing, using 40mL pyridine as solvent, under the constant temperature oil bath condition of 120 ℃, use air set pipe condensing reflux 5h, coolingly use Buchner funnel suction filtration afterwards, then by distilled water and volume fraction, be that 95% ethanol is alternately rinsed well respectively, put in air dry oven, at 60 ℃, dry 24h, is placed in drier standby;
2) step 1) gained reed straw is stirred to 0.5h in saturated sodium bicarbonate solution, then use Buchner funnel suction filtration, with distilled water and volume fraction 95% ethanol, alternately rinse well respectively, continue dry 24h at 60 ℃ of temperature, pack in bag, be placed in drier and store.
2. succinic anhydride claimed in claim 1 is modified the preparation method of wild reed rod adsorbent, includes following steps:
1) getting 2.0g reed straw powder joins in round-bottomed flask, the 3.0g succinic anhydride that adds again accurate weighing, using 40mL pyridine as solvent, under the constant temperature oil bath condition of 120 ℃, use air set pipe condensing reflux 5h, coolingly use Buchner funnel suction filtration afterwards, then by distilled water and volume fraction, be that 95% ethanol is alternately rinsed well respectively, put in air dry oven, at 60 ℃, dry 24h, is placed in drier standby;
2) step 1) gained reed straw is stirred to 0.5h in saturated sodium bicarbonate solution, then use Buchner funnel suction filtration, with distilled water and volume fraction 95% ethanol, alternately rinse well respectively, continue dry 24h at 60 ℃ of temperature, pack in bag, be placed in drier and store.
Succinic anhydride claimed in claim 1 modify wild reed rod adsorbent at industrial dye waste water or in containing metal ion cadmium waste water or containing the plumbous waste water of metal ion as the application of adsorbent.
4. application according to claim 3, is characterized in that described industrial dye waste water is Crystal Violet Dye waste water or methylene blue dye waste water.
5. application according to claim 4, is characterized in that application process is: take 0.01-0.10g succinic anhydride and modify wild reed rod adsorbent, joining concentration is 100-1000mg L
-1crystal violet or methylene blue dye waste water in, take acid or alkali adjusting pH value after 2-10.00, be placed on the water bath chader of 15-70 ℃ and shake 1-24 hour, the concentration of crystal violet in supernatant is measured in centrifugation, according to the concentration difference of crystal violet or methylene blue in water before and after absorption, determine its adsorption effect to crystal violet in water or methylene blue.
6. application according to claim 5, is characterized in that regulating the alkali of pH value is NaOH, and acid is hydrochloric acid.
7. application according to claim 5, the concussion speed that it is characterized in that water-bath constant temperature oscillator is 50-300rpm.
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| CN103877947A (en) * | 2014-04-16 | 2014-06-25 | 湖南大学 | Preparation method and application of efficient corn straw adsorbent |
| CN109081341A (en) * | 2018-09-30 | 2018-12-25 | 江苏斯沃得环保科技有限公司 | A kind of preparation method of mesoporous activated carbon |
| CN110560009A (en) * | 2019-09-18 | 2019-12-13 | 武汉工程大学 | Preparation method and application of pea shell-based biosorbent modified by maleic anhydride |
| CN115739035A (en) * | 2022-12-05 | 2023-03-07 | 南京信息工程大学 | Method for modifying kenaf straws by succinic anhydride |
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| CN110560009B (en) * | 2019-09-18 | 2022-03-15 | 武汉工程大学 | Preparation method and application of pea shell-based biosorbent modified by maleic anhydride |
| CN115739035A (en) * | 2022-12-05 | 2023-03-07 | 南京信息工程大学 | Method for modifying kenaf straws by succinic anhydride |
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