CN103301884A - Preparation method and application of modified active carbon fiber based on 8-hydroxyquinoline ferrum - Google Patents
Preparation method and application of modified active carbon fiber based on 8-hydroxyquinoline ferrum Download PDFInfo
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- CN103301884A CN103301884A CN2013102348344A CN201310234834A CN103301884A CN 103301884 A CN103301884 A CN 103301884A CN 2013102348344 A CN2013102348344 A CN 2013102348344A CN 201310234834 A CN201310234834 A CN 201310234834A CN 103301884 A CN103301884 A CN 103301884A
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- oxine
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- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 title claims abstract description 64
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 229920000049 Carbon (fiber) Polymers 0.000 title claims abstract description 20
- MCJGNVYPOGVAJF-UHFFFAOYSA-N quinolin-8-ol Chemical compound C1=CN=C2C(O)=CC=CC2=C1 MCJGNVYPOGVAJF-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000004917 carbon fiber Substances 0.000 title claims abstract description 11
- 239000005725 8-Hydroxyquinoline Substances 0.000 title abstract 2
- 229960003540 oxyquinoline Drugs 0.000 title abstract 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims abstract description 30
- 239000002351 wastewater Substances 0.000 claims abstract description 19
- 238000006243 chemical reaction Methods 0.000 claims abstract description 15
- 238000005406 washing Methods 0.000 claims abstract description 8
- 239000003960 organic solvent Substances 0.000 claims abstract description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 37
- 239000000975 dye Substances 0.000 claims description 27
- 229910052742 iron Inorganic materials 0.000 claims description 19
- -1 oxine iron modified activated carbon Chemical class 0.000 claims description 14
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 13
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 12
- 150000004880 oxines Chemical class 0.000 claims description 10
- 238000012986 modification Methods 0.000 claims description 8
- 230000004048 modification Effects 0.000 claims description 8
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims description 8
- YDEUKNRKEYICTH-UHFFFAOYSA-N 5-aminoquinolin-8-ol Chemical compound C1=CC=C2C(N)=CC=C(O)C2=N1 YDEUKNRKEYICTH-UHFFFAOYSA-N 0.000 claims description 6
- VZBQXRRQMCCPPP-UHFFFAOYSA-N iron quinoline Chemical compound [Fe].N1=CC=CC2=CC=CC=C12 VZBQXRRQMCCPPP-UHFFFAOYSA-N 0.000 claims description 6
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 6
- 230000003197 catalytic effect Effects 0.000 claims description 5
- 230000000694 effects Effects 0.000 claims description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- SJEYSFABYSGQBG-UHFFFAOYSA-M Patent blue Chemical compound [Na+].C1=CC(N(CC)CC)=CC=C1C(C=1C(=CC(=CC=1)S([O-])(=O)=O)S([O-])(=O)=O)=C1C=CC(=[N+](CC)CC)C=C1 SJEYSFABYSGQBG-UHFFFAOYSA-M 0.000 claims description 3
- 239000000980 acid dye Substances 0.000 claims description 3
- 239000000203 mixture Substances 0.000 claims description 3
- 239000000985 reactive dye Substances 0.000 claims description 3
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 2
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 claims description 2
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 claims description 2
- 229910020366 ClO 4 Inorganic materials 0.000 claims description 2
- 229920000297 Rayon Polymers 0.000 claims description 2
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 2
- 239000010426 asphalt Substances 0.000 claims description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 claims description 2
- 229910052794 bromium Inorganic materials 0.000 claims description 2
- 229910052801 chlorine Inorganic materials 0.000 claims description 2
- 239000000460 chlorine Substances 0.000 claims description 2
- 229910052740 iodine Inorganic materials 0.000 claims description 2
- 239000011630 iodine Substances 0.000 claims description 2
- 150000002505 iron Chemical class 0.000 claims description 2
- 229920001568 phenolic resin Polymers 0.000 claims description 2
- 239000005011 phenolic resin Substances 0.000 claims description 2
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 2
- 239000012266 salt solution Substances 0.000 claims description 2
- 238000000034 method Methods 0.000 abstract description 14
- 238000004043 dyeing Methods 0.000 abstract description 9
- 238000001035 drying Methods 0.000 abstract description 4
- 238000007639 printing Methods 0.000 abstract description 2
- SMWDFEZZVXVKRB-UHFFFAOYSA-N Quinoline Chemical compound N1=CC=CC2=CC=CC=C21 SMWDFEZZVXVKRB-UHFFFAOYSA-N 0.000 abstract 4
- 150000004325 8-hydroxyquinolines Chemical class 0.000 abstract 2
- 150000003839 salts Chemical class 0.000 abstract 2
- 230000007547 defect Effects 0.000 abstract 1
- 238000001179 sorption measurement Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 11
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 10
- 229940044631 ferric chloride hexahydrate Drugs 0.000 description 10
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 description 10
- 238000004065 wastewater treatment Methods 0.000 description 10
- 238000005303 weighing Methods 0.000 description 10
- 238000012545 processing Methods 0.000 description 6
- 238000003756 stirring Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 239000003054 catalyst Substances 0.000 description 4
- 238000011282 treatment Methods 0.000 description 4
- LGDFHDKSYGVKDC-UHFFFAOYSA-N 8-hydroxyquinoline-5-sulfonic acid Chemical compound C1=CN=C2C(O)=CC=C(S(O)(=O)=O)C2=C1 LGDFHDKSYGVKDC-UHFFFAOYSA-N 0.000 description 2
- 239000012028 Fenton's reagent Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000015556 catabolic process Effects 0.000 description 2
- 238000006731 degradation reaction Methods 0.000 description 2
- 235000019441 ethanol Nutrition 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 2
- 229940043267 rhodamine b Drugs 0.000 description 2
- 239000004753 textile Substances 0.000 description 2
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 description 1
- WSIGGURFGMNQNZ-UHFFFAOYSA-N N'-(3-bromo-4-fluorophenyl)-N-hydroxy-4-[2-(sulfamoylamino)ethylsulfanyl]-1,2,5-oxadiazole-3-carboximidamide Chemical compound BrC=1C=C(C=CC=1F)N\C(=N/O)\C1=NON=C1SCCNS(N)(=O)=O WSIGGURFGMNQNZ-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 238000009303 advanced oxidation process reaction Methods 0.000 description 1
- 150000007942 carboxylates Chemical class 0.000 description 1
- 239000008139 complexing agent Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000010919 dye waste Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 229910052731 fluorine Inorganic materials 0.000 description 1
- 239000011737 fluorine Substances 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- STZCRXQWRGQSJD-GEEYTBSJSA-M methyl orange Chemical compound [Na+].C1=CC(N(C)C)=CC=C1\N=N\C1=CC=C(S([O-])(=O)=O)C=C1 STZCRXQWRGQSJD-GEEYTBSJSA-M 0.000 description 1
- 229940012189 methyl orange Drugs 0.000 description 1
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 description 1
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000003672 processing method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
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- Water Treatment By Sorption (AREA)
Abstract
The invention discloses a preparation method and application of a modified active carbon fiber based on 8-hydroxyquinoline ferrum. The preparation method of the supported active carbon fiber comprises the following steps of: (1) respectively dissolving ferric salt and 8-hydroxyquinoline compounds into an organic solvent, and mixing the ferric salt and the 8-hydroxyquinoline compounds according to a certain proportion to prepare a quinoline ferrum complex solution; (2) supporting a quinoline ferrum complex on an active carbon fiber by using an adsorption method or covalent bond grafting method; and (3) finally, taking out the active carbon fiber, washing the surface of the active carbon fiber by using water, and placing the active carbon fiber into a drying oven to dry to obtain the modified active carbon fiber. The modified active carbon fiber is simple in preparation, lower in requirement for reaction environments, capable of efficiently treating printing and dyeing wastewater through catalyzing hydrogen peroxide under the condition that the pH is 2-11, being repeatedly used many times and making up the defects of secondary pollution, narrow pH application range and the like of the traditional Fenton, and higher in implementation value and socioeconomic benefit.
Description
Technical field
The present invention relates to a kind ofly for the techniques of Dyeing Wastewater Treatment field, be specifically related to preparation method and the application of activated carbon fiber loaded oxine iron catalyst.
Background technology
According to statistics, the annual waste water that produces of China's textile industry is up to more than 20 hundred million tons, and wherein dyeing waste water accounts for 80%.Therefore, how better more efficiently treatment of dyeing and printing is a major issue being badly in need of at present solution.In method of wastewater treatment, the Fenton method is to use more extensively and comparatively effective a kind of method.
The Fenton method is a kind of advanced oxidation processes, hydroxyl radical free radical (the oxidizing potential 2.8V that its reaction produces, the oxidizing potential 2.87V that is only second to fluorine), has very strong oxidisability, dye molecule and other poisonous and hazardous organic pollutions in can the oxidation dyeing waste water, thus reach the purpose for the treatment of and purification dyeing waste water.Yet traditional F enton method exists many limitation: the pH interval of (1) reaction is too narrow, must at 2-4 than just carrying out under the strong acidic environment, therefore for neutral or alkaline dyeing waste water, almost not have effect; (2) Fe that uses
2+And Fe
3+Easily form mud, cause secondary pollution.
Class Fenton technology is a kind of high-level oxidation technology that grows up on traditional Fenton reagent basis, in broad terms, except Fenton reagent, other adopts hydrogen peroxide to produce hydroxyl radical free radical isoreactivity base and processes the technology of organic pollution and all be called class Fenton technology, such as the fragrant class of electric class pause technology, light class Fenton technology, heterogeneous class Fenton technology etc.In recent years, heterogeneous class Fenton technology because of have degradation efficiency high, reduce secondary pollution, can widen the advantages such as pH value of solution reaction by extensive concern.In the known technology, application number is: 201110009690.3 " preparation of magnetic heterogeneous light Fenton and the methods of degradable organic pollutant thereof " are disclosed to be the heterogeneous smooth Fenton catalyst of processing for rhodamine B, ferric trichloride and nickelous sulfate are mixed with mixed solution, then mixed solution is heated, separates, washs, dries, obtain magnetic heterogeneous light Fenton catalyst n iFe
2O
4Application number: 201010146094.5 is electro-Fenton reaction method for the processing of dyeing waste water for " based on the method for wastewater treatment of electro-Fenton reaction " is disclosed.Application number: " method of microwave cooperating magnetic class Fenton catalyst treatment waste water from dyestuff " is disclosed to be to be the microwave heating appts synergic nano MgFe of 800W with power
2O
4Dye wastewater treatment using.
Yet the required device more complicated of above-mentioned preparation method and processing method, and energy consumption is higher, is not suitable for a large amount of wastewater treatments.
Summary of the invention
In order to solve the above-mentioned technical problem that exists in the prior art, the invention provides a kind of efficiently preparation method and application of the activated carbon fiber of dye wastewater treatment using.Concrete technical scheme is as follows:
A kind of preparation method based on oxine iron modified activated carbon fiber comprises the steps:
Step (1) is dissolved in respectively organic solvent with molysite and oxine compounds, and the pH of control oxine compounds solution is 3-6, then iron salt solutions dropwise is added drop-wise in molar ratio 1:1-1:6 mixing in the oxine compounds solution, obtains quinoline iron complex solution;
The quinoline iron complex solution that step (2) is got step (1) gained mixes by 1-30g/L with activated carbon fiber, left standstill 1-12 hour after ultrasonic 1-2 hour, then with alcohol and clear water washing, put it into again and dry the activated carbon fiber that can obtain based on the modification of oxine iron in the baking oven after taking out.
Further, adopt step (3) to replace step 2, wherein step (3) is as follows: get activated carbon fiber and mix with organic solvent in the 1-30g/L ratio, add thionyl chloride, with the ratio of activated carbon fiber be 1-10mL/g, 80-100 ℃ of control temperature, reaction 12-24h, then get the described quinoline iron complex of step (1) solution and mix in the ratio of 1-20g/L, 50-70 ℃ of control temperature, reaction 12-24h; Then take out washing, place 50-70 ℃ baking oven 2-4h, place again 100-120 ℃ vacuum drying oven to dry, can obtain the activated carbon fiber based on the modification of oxine iron.
Further, described molysite is FeCl
3, FeCl
2, Fe (NO
3)
3, Fe (NO
3)
2, Fe
2(SO
4)
3, FeSO
4, Fe (ClO
4)
3In a kind of or their combination.
Further, described oxine compounds is oxine, HQS, 5-amino-8-hydroxyquinoline, oxine-5-carboxylic acid, a kind of in 5-chlorine (bromine, iodine)-oxine or their combination.
Further, described organic solvent is ethanol, DMF, oxolane or acetone.
Further, described activated carbon fiber is viscose base activated carbon fiber, polyacrylonitrile based activated carbon fiber, asphalt activity carbon fiber or phenolic resin based activated carbon fiber.
The present invention also provides a kind of application of the activated carbon fiber based on the modification of oxine iron, be used for the degraded of the organic pollutions such as dyestuff, comprise the steps: to containing the reactive dye that concentration is 0.01-0.5g/L, acid dyes or neutral dye, activated carbon fiber and hydrogen peroxide after pH is to add load in the waste water from dyestuff of 2-11 are 20-90 in temperature
oThe stirred in water bath 5-30min of C, wherein the addition of activated carbon fiber is 0.5-10g/L, the addition of hydrogen peroxide is 10-100mmol/L.
The present invention has not only overcome traditional F enton secondary pollution, and the hydrogen peroxide utilization rate is low, and applicable scope is little to wait deficiency, and has the characteristic of high-activity treatment of textile dye waste.
Activated carbon fiber among the present invention has larger specific area, is a kind of good carrier, and its surperficial functional group has again various chemical property; The oxine compounds is good complexing agent, can form stable complex with metal ion, and the complex that forms has certain catalytic activity.The present invention utilizes above-mentioned characteristic that oxine compounds and the reacted part of iron are loaded on the activated carbon fiber, and the activated carbon fiber after the modification has efficient catalytic activity.Therefore compared with prior art, advantage of the present invention has: (1) efficient catalytic hydrogen peroxide degradation dyeing waste water; (2) realized the recycling of activated carbon fiber, and the secondary pollution that does not have iron ion to cause, the environmental protection theory met; (3) required reaction condition is gentle, do not need other extraneous factors such as light, ultrasonic wave auxiliary, and pH has catalytic activity in the wider interval of 2-11.
The specific embodiment
Application based on oxine iron modified activated carbon fiber, the process of processing waste water is as follows: be used for the degraded of the organic pollutions such as dyestuff, to containing reactive dye that concentration is 0.01-0.5g/L, acid dyes, neutral dye etc., pH is activated carbon fiber and the hydrogen peroxide that adds in the waste water from dyestuff of 3-11 after the load, is 20-90 in temperature
OC and above stirred in water bath 5-30min, wherein the addition of activated carbon fiber is 0.5-10g/L, the addition of hydrogen peroxide is 10-100mmol/L.
Benq is in the preparation of oxine iron modified activated carbon fiber below by several embodiment:
Embodiment 1
Take by weighing oxine 2.177g and be dissolved in the 200ml absolute ethyl alcohol, be stirred to fully dissolving, and control pH scope 3-6; Take by weighing ferric chloride hexahydrate 1.35g, add the 100ml anhydrous alcohol solution, then while stirring ferric chloride hexahydrate solution slowly is added drop-wise in the ethanolic solution of oxine, namely get the oxine ferrous solution.Then the 5g activated carbon fiber is joined in the oxine ferrous solution, ultrasonic processing 1 hour was left standstill 2 hours, took out activated carbon fiber, and washing and drying namely gets the activated carbon fiber with efficient dye wastewater treatment using characteristic.
Test factually demonstration, at the X-3B of 25ml 0.05g/L reactive red, pH is in 7 the waste water from dyestuff, adds the 0.15g activated carbon fiber, splashes into the 0.1mL hydrogen peroxide again, in 50 ℃ water-bath, vibrates 10 minutes, and the dyestuff clearance is 99.7%.
Embodiment 2
Take by weighing oxine-5 sulfonic acid 3.36g and be dissolved in the 200ml absolute ethyl alcohol, be stirred to fully dissolving, and control pH scope 3-6; Take by weighing ferric chloride hexahydrate 1.35g, add the 100ml anhydrous alcohol solution, then while stirring ferric chloride hexahydrate solution slowly is added drop-wise in the ethanolic solution of HQS, namely get the HQS ferrous solution.Then the 5g activated carbon fiber is joined in the oxine 5-sulfonic acid ferrous solution, ultrasonic processing 1 hour was left standstill 2 hours, took out activated carbon fiber, and washing and drying namely gets the activated carbon fiber with high dye wastewater treatment using characteristic.
Test factually demonstration, in the Acid of 25ml 0.05g/L 1 acid red, pH are 7 waste water from dyestuff, add the 0.15g activated carbon fiber, splash into again the 0.1mL hydrogen peroxide, 40
oIn the water-bath of C, vibrated 10 minutes, the dyestuff clearance is 98.4%.
Embodiment 3
Take by weighing oxine 2.177g and be dissolved in the 200ml absolute ethyl alcohol, be stirred to fully dissolving, and control pH scope 3-6; Take by weighing ferric chloride hexahydrate 1.35g, add the 100ml anhydrous alcohol solution, then while stirring ferric chloride hexahydrate solution slowly is added drop-wise in the ethanolic solution of oxine, namely get the oxine ferrous solution.Then the 5g activated carbon fiber is joined in the oxine ferrous solution, ultrasonic processing 1 hour was left standstill 2 hours, took out activated carbon fiber, and washing and drying namely gets the activated carbon fiber with high dye wastewater treatment using characteristic.
Test factually demonstration, in rhodamine B, the pH of 25ml 0.05g/L are 7 waste water from dyestuff, add the 0.3g activated carbon fiber, splash into the 0.15mL hydrogen peroxide again, in 50 ℃ water-bath, vibrated 15 minutes, the dyestuff clearance is 99.1%.
Embodiment 4
Take by weighing the amino oxine 2.40g of 5-and be dissolved among the 200ml DMF, be stirred to fully dissolving, and control pH scope 3-6; Take by weighing ferric chloride hexahydrate 1.35g, add 100ml DMF dissolving, then while stirring ferric chloride hexahydrate solution slowly is added drop-wise in the DMF solution of 5-amino-8-hydroxyquinoline, namely get 5-amino-8-hydroxyquinoline ferrous solution, getting the 5g activated carbon fiber mixes with the 500mL dry DMF, 90 ℃ of control temperature add the 20ml thionyl chloride again in this solution, the control temperature 60 C, reaction 12h, add again amino-8 oxyquinoline ferrous solutions of the above-mentioned 5-for preparing, 80 ℃ of control temperature, reaction 12h; Take out activated carbon fiber, wash 2h in the baking oven that is placed on 60 ℃, place again 120 ℃ vacuum drying oven to dry, can obtain the activated carbon fiber based on the modification of oxine iron.
Test factually demonstration, in the methyl orange of 25ml 0.05g/L, pH is in 7 the waste water from dyestuff, adds this activated carbon fiber of 0.30g, splashes into the 0.15mL hydrogen peroxide, 50 again
oIn the water-bath of C, vibrated 10 minutes, the dyestuff clearance is 99.9%.
Embodiment 5
Take by weighing the amino oxine 2.40g of 5-and be dissolved among the 250ml DMF, be stirred to fully dissolving, and control pH scope 3-6; Take by weighing ferric chloride hexahydrate 2.70g, add 250ml DMF dissolving, then while stirring ferric chloride hexahydrate solution slowly is added drop-wise in the DMF solution of 5-amino-8-hydroxyquinoline, namely get 5-amino-8-hydroxyquinoline ferrous solution, getting the 5g activated carbon fiber mixes with the 500mL dry DMF, 90 ℃ of control temperature add the 20ml thionyl chloride again in this solution, the control temperature 60 C, reaction 24h, add again amino-8 oxyquinoline ferrous solutions of the above-mentioned 5-for preparing, 80 ℃ of control temperature, reaction 24h; Take out activated carbon fiber, wash 2h in the baking oven that is placed on 60 ℃, place again 120 ℃ vacuum drying oven to dry, namely get the activated carbon fiber with efficient dye wastewater treatment using characteristic.
Test factually demonstration, at the Reactive Red K-2BP of 100ml 0.05g/L, pH is in 9 the waste water from dyestuff, adds this activated carbon fiber of 0.30g, splashes into the 0.2mL hydrogen peroxide, 50 again
oIn the water-bath of C, vibrated 10 minutes, the dyestuff clearance is 99.9%.
To those skilled in the art; under this patent design and specific embodiment enlightenment; the distortion that can directly derive or associate from this patent disclosure and general knowledge; or the substituting of known technology commonly used in the prior art; and the mutual various combination between feature; for example according to different waste water and pollutant levels; determine different amounts; and different molysite, mantoquita; the unsubstantiality of carboxylate etc. is changed, and can be employed equally, can both realize and the essentially identical function of above-described embodiment and effect; give an example no longer one by one, all belong to the protection domain of this patent.
Claims (7)
1. the preparation method based on oxine iron modified activated carbon fiber comprises the steps:
Step (1) is dissolved in respectively organic solvent with molysite and oxine compounds, and the pH of control oxine compounds solution is 3-6, then iron salt solutions dropwise is added drop-wise in molar ratio 1:1-1:6 mixing in the oxine compounds solution, obtains quinoline iron complex solution;
The quinoline iron complex solution that step (2) is got step (1) gained mixes by 1-30g/L with activated carbon fiber, left standstill 1-12 hour after ultrasonic 1-2 hour, then with alcohol and clear water washing, put it into again and dry the activated carbon fiber that can obtain based on the modification of oxine iron in the baking oven after taking out.
2. the preparation method based on oxine iron modified activated carbon fiber as claimed in claim 1, it is characterized in that: adopt step (3) to replace step 2, wherein step (3) is as follows: get activated carbon fiber and mix with organic solvent in the 1-30g/L ratio, add thionyl chloride, with the ratio of activated carbon fiber be 1-10mL/g, 80-100 ℃ of control temperature, reaction 12-24h, then getting the described quinoline iron complex of step (1) solution mixes in the ratio of 1-20g/L, 50-70 ℃ of control temperature, reaction 12-24h; Then take out washing, place 50-70 ℃ baking oven 2-4h, place again 100-120 ℃ vacuum drying oven to dry, can obtain the activated carbon fiber based on the modification of oxine iron.
3. the preparation method based on oxine iron modified activated carbon fiber as claimed in claim 1 or 2, it is characterized in that: described molysite is FeCl
3, FeCl
2, Fe (NO
3)
3, Fe (NO
3)
2, Fe
2(SO
4)
3, FeSO
4, Fe (ClO
4)
3In a kind of or their combination.
4. the preparation method based on oxine iron modified activated carbon fiber as claimed in claim 1 or 2, it is characterized in that: described oxine compounds is oxine, HQS, the 5-amino-8-hydroxyquinoline, oxine-5-carboxylic acid, a kind of in 5-chlorine (bromine, iodine)-oxine or their combination.
5. the preparation method based on oxine iron modified activated carbon fiber as claimed in claim 1 or 2, it is characterized in that: described organic solvent is ethanol, DMF, oxolane or acetone.
6. the preparation method of the activated carbon fiber of high catalytic activity as claimed in claim 1 or 2, it is characterized in that: described activated carbon fiber is viscose base activated carbon fiber, polyacrylonitrile based activated carbon fiber, asphalt activity carbon fiber or phenolic resin based activated carbon fiber.
7. the application of the activated carbon fiber based on the modification of oxine iron as claimed in claim 1 or 2, be used for the degraded of the organic pollutions such as dyestuff, comprise the steps: to containing the reactive dye that concentration is 0.01-0.5g/L, acid dyes or neutral dye, activated carbon fiber and hydrogen peroxide after pH is to add load in the waste water from dyestuff of 2-11 are 20-90 in temperature
oThe stirred in water bath 5-30 min of C, wherein the addition of activated carbon fiber is 0.5-10 g/L, the addition of hydrogen peroxide is 10-100 mmol/L.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310234834.4A CN103301884B (en) | 2013-06-14 | 2013-06-14 | Preparation method and application of modified active carbon fiber based on 8-hydroxyquinoline ferrum |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
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| CN104830313A (en) * | 2015-04-21 | 2015-08-12 | 吉林化工学院 | Preparation method of {[Co(5-amino-8-hydroxyquinoline)2].H2O}n complex with blue light property |
| CN108080028A (en) * | 2017-12-22 | 2018-05-29 | 安徽工业大学 | The preparation method of 8-hydroxyquinoline iron class organic dyestuff Photodegradation catalyst |
| CN116060131A (en) * | 2022-10-27 | 2023-05-05 | 浙江工商大学 | Ionic metal chelate catalyst and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104830313A (en) * | 2015-04-21 | 2015-08-12 | 吉林化工学院 | Preparation method of {[Co(5-amino-8-hydroxyquinoline)2].H2O}n complex with blue light property |
| CN104830313B (en) * | 2015-04-21 | 2017-01-11 | 吉林化工学院 | Preparation method of {[Co(5-amino-8-hydroxyquinoline)2].H2O}n complex with blue light property |
| CN108080028A (en) * | 2017-12-22 | 2018-05-29 | 安徽工业大学 | The preparation method of 8-hydroxyquinoline iron class organic dyestuff Photodegradation catalyst |
| CN108080028B (en) * | 2017-12-22 | 2020-11-03 | 安徽工业大学 | Preparation method of 8-hydroxyquinoline iron organic dye photodegradation catalyst |
| CN116060131A (en) * | 2022-10-27 | 2023-05-05 | 浙江工商大学 | Ionic metal chelate catalyst and preparation method and application thereof |
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