CN103240122B - Preparation method of active carbon fiber loaded aminopyridine metal complex - Google Patents
Preparation method of active carbon fiber loaded aminopyridine metal complex Download PDFInfo
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Abstract
The invention discloses a preparation method of an active carbon fiber loaded aminopyridine metal complex. The preparation method comprises the following steps of: (1) dissolving aminopyridine and metal salt in an organic solvent respectively so as to prepare aminopyridine solution and metal salt solution; (2) adding the metal salt solution in the aminopyridine solution drop by drop so as to obtain aminopyridine metal complex solution; (3) processing pretreated active carbon fiber with thionyl chloride (SOCl2) so as to obtain active carbon fiber with acyl chlorides; and (4) adding the acyl chloride-based metal complex solution in the active carbon fiber with acyl chlorides for reaction, and preparing the active carbon fiber loaded aminopyridine metal complex through separation, washing and drying. According to the method, the simplicity is realized, the cost is low and the industrialized production is easy; and moreover, the used organic solvent can be recycled; and the preparation method is economical and environment-friendly.
Description
Technical field
The present invention relates to a kind of activated carbon fiber loaded aminopyridine iron catalyst and preparation method for treatment of dyeing wastewater.
Background technology
By Fe
2+/ Fe
3+and H
2o
2the Fenton reagent forming is a kind of high-level oxidation technology that is applied to wastewater treatment, and this is mainly owing to H
2o
2at Fe
2+/ Fe
3+existence under can produce a large amount of hydroxyl radical free radical with strong oxidizing property (oxidizing potential is 2.8V), they can with most organic pollutions reaction in waste water.But due to Fe
2+/ Fe
3+class reaction at pH, is greater than at 3 o'clock and can produces flocculent deposit, greatly reduce reaction efficiency, so generally can only be carried out in pH is less than 3 strong acid medium.Research shows that metal and organic coordination compound are carried out to effective coordination is expected to widen the Fenton reagent pH scope of application, the people such as Collins develop a kind of organic coordination compound catalyst (Fe-TAML) of iron, can within the scope of the pH broad to alkalescence from acidity, remove fast dyestuff and phenolic compound (Science, 2002,296:326-328).Yet the catalyst of homogeneous phase is because structural stability is poor, thereby can not continue to keep higher catalytic activity, and easily form secondary pollution, this has limited the further application of such catalyst.
In recent years, heterogeneous class Fenton technology because of have degradation efficiency high, reduce secondary pollution, the advantages such as pH value that can widen solution reaction are by extensive concern.In known technology, application number: 201210081648.7 " a kind of preparation methods of heterogeneous Fenton reagent oxidation catalyst of activated carbon supported ferrous iron " disclose Fe
2+load on active carbon and make heterogeneous Fenton catalyst, catalyst can be recycled, and has simplified processing technological flow, greatly reduces the cost of wastewater treatment, and catalyst preparation process is simple, and mild condition is easy to promote the use of.Application number: 201210489713.X " preparation method of a kind of year heterogeneous Fenton catalyst of iron bamboo charcoal " discloses and has utilized repeatedly cooking process that iron ion is firmly carried on bamboo charcoal, in wastewater treatment process, given full play to the strong oxidizing property of absorption property and the Fenton's reaction of bamboo charcoal, increased pH value scope, avoid producing secondary pollution, the pollutants removal rates such as phenol in waste water are reached more than 95%.Application number: 201310000494.9 " preparation methods of a kind of year heterogeneous Fenton catalyst of iron attapulgite " disclose utilize dipping and ion-exchange by iron ion be carried on attapulgite modified on, be prepared into heterogeneous Fenton catalyst, the strong oxidizing property of absorption property, ion-exchange performance and the Fenton's reaction of performance attapulgite, can process used water difficult to degradate expeditiously.The people such as Zhao directly load to iron ion and on ion exchange resin, obtain heterogeneous light and help Fenton catalyst, resin provides a special microenvironment for iron activated centre, effective rhodamine B degradation under neutrallty condition, the dyestuffs such as methyl blue, and Fe has been accelerated in adding of illumination
2+/ Fe
3+circulation, thereby improved the catalytic activity (Envir. Sci.Technol.2004,38:1569-1575) of catalyst.Although above heterogeneous class Fenton technology has certain advantage,, because iron is to be only adsorbed on carrier by ionic bond, all there is certain limitation in catalytic activity and stability.
Summary of the invention
The object of the invention is to overcome existing Fenton, there is the narrower defect of pH adaptability in class Fenton catalyst, provides that a kind of method is simple, cost is low, the preparation method of the activated carbon fiber loaded aminopyridine metal complex of easy suitability for industrialized production.Technical scheme of the present invention is as follows:
A preparation method for activated carbon fiber loaded aminopyridine metal complex, comprises the steps:
(1) aminopyridine and slaine are dissolved in respectively in organic solvent, are mixed with respectively aminopyridine and metal salt solution; (2) described metal salt solution is dropwise joined in aminopyridine solution, obtain aminopyridine metal complex solution; (3) adopt thionyl chloride (SOCl
2) pretreated activated carbon fiber is processed, obtain having the activated carbon fiber of acid chloride group; (4) in the activated carbon fiber of acid chloride group, add described aminopyridine metal complex solution to react, after separation, washing and being dried, make activated carbon fiber loaded aminopyridine complex compound.
Further, described aminopyridine is a kind of in 4-aminopyridine, 3-aminopyridine, PA, preferably 4-aminopyridine.
Further, the metal ion of described slaine can be a kind of in iron, cobalt, copper, manganese, zinc transition metal ions, preferably iron, cobalt metal ion, and molysite can be FeCl
2, FeCl
3, Fe (NO
3)
3, FeSO
4, Fe
2(SO
4)
3, Fe (ClO
4)
3in a kind of or their combination; Described cobalt salt can be CoCl
2, Co (NO
3)
2, CoSO
4, Co (Ac)
2in a kind of or their combination.
Further, described organic solvent is DMF, DMSO, DMAc, preferably DMF.
Further, described metal salt solution, by slaine is added in organic solvent, then stirs and makes for 10-30 minute at 20-50 ℃.
Further, described activated carbon fiber is polyacrylonitrile based activated carbon fiber, viscose base activated carbon fiber and asphalt activity carbon fiber, preferably polyacrylonitrile based activated carbon fiber.
Further, described pretreatment is activated carbon fiber to be flooded in concentrated nitric acid solution to 12-24 hour, then by deionized water, is washed till neutrality, at the baking oven inner drying 10-20 hour of 80-100 ℃, then in vacuum drying chamber, be dried 12-24 hour, baking temperature is 100-130 ℃; The nitric acid of described concentrated nitric acid solution: the volume ratio of water is 1:1-1:3.
Further, described aminopyridine metal complex solution is under magnetic stirring apparatus effect, by the mol ratio of slaine and aminopyridine, is 1:2-1:6, and described metal salt solution is added drop-wise to aminopyridine solution gradually, then stirs and obtains for 20-60 minute.
Further, the activated carbon fiber of described acid chloride group is to add SOCl in pretreated activated carbon fiber
2, at 80-95 ℃, process 5-8h, then be warming up to the 130-150 ℃ of SOCl that removal is unnecessary
2, cooling obtaining.
Further, described activated carbon fiber loaded aminopyridine metal complex is that aminopyridine metallic solution is joined in the activated carbon fiber of acid chloride group, after 50-70 ℃ of reaction 12-28h, respectively with DMF, deionized water, sodium bicarbonate solution washing, extremely neutral with deionized water washing again, at 80-100 ℃, be dried, be dried and can obtain after 12-14 hour.
Activated carbon fiber loaded aminopyridine metal complex is that the mode by acid amides covalent bond loads on aminopyridine metal complex on activated carbon fiber and makes.
Above activated carbon fiber loaded aminopyridine metal complex, the load capacity of aminopyridine metal complex is 0.5-10%.
Compared with prior art, beneficial effect of the present invention:
Aminopyridine metal complex is loaded on to the activated carbon fiber loaded aminopyridine metal complex catalyst preparing on activated carbon fiber, compare with independent aminopyridine metal complex, this catalyst has not only shown the better catalytic activity of dyestuff under oxidant hydrogen peroxide effect, and its stability also significantly improves in the process of degradation of dye.Therefore, activated carbon fiber loaded aminopyridine metal complex catalyst is when degradation of dye, metal ion in the waste water from dyestuff being degraded, do not detected, this illustrates that activated carbon fiber loaded aminopyridine metal complex can be repeatedly used, and non-secondary pollution.Simultaneously, actual dying is generally even alkaline in neutrality mostly, technology in the past often could be processed waste water under acidity, this just need to add extra acid-base reagent, this not only increases cost greatly, and the use of acid-base reagent extra work operating environment, endangered workman healthy.Activated carbon fiber loaded aminopyridine metal complex prepared by the present invention just can treatment of dyeing and printing at pH 3-11, add acid-base reagent, and under these pH conditions, catalyst of the present invention is all more stable, can repeatedly use without extra.
The inventive method is simple, cost is low, and easily suitability for industrialized production, and the organic solvent using can reclaim, and is the processing method of a kind of economy, green.Activated carbon fiber loaded aminopyridine metal complex to catalyze activity of the present invention is high, reusability good, and just can high-activity treatment of textile dye waste in the pH condition that does not change actual dying.Therefore, activated carbon fiber loaded aminopyridine metal complex catalyst of the present invention not only can be used as the preconditioning technique of dyeing waste water, also can be used as the advanced treating technology for the treatment of of dyeing wastewater, also can be used as the regeneration techniques of activated carbon fiber.Activated carbon fiber loaded aminopyridine metal complex of the present invention not only can be applicable to the processing of dyeing waste water, but also can be applicable to the wastewater treatment in the fields such as papermaking, pharmacy, chemical industry.
Accompanying drawing explanation
Fig. 1 is activated carbon fiber loaded aminopyridine iron clearance block diagram to azogeramine under different pH values of embodiment 1 preparation;
Fig. 2 is that the activated carbon fiber loaded aminopyridine iron of embodiment 1 preparation and aminopyridine iron are the effect contrast figure of pH 7 degradation of dye.
The specific embodiment
Below in conjunction with accompanying drawing, the invention will be further described.
Embodiment 1
By 4-aminopyridine and FeCl
3be dissolved in respectively in DMF solution, be mixed with respectively 4-aminopyridine and FeCl
3solution, under the effect of magnetic stirring apparatus, by FeCl
3solution is added drop-wise in 4-aminopyridine solution gradually, FeCl
3with the mol ratio of 4-aminopyridine be 1:4, at 30 ℃, react and within 30 minutes, obtain 4-aminopyridine ferrous solution.
Polyacrylonitrile based activated carbon fiber floods 15 hours in the red fuming nitric acid (RFNA) aqueous solution (nitric acid: the volume ratio of water is 1:3), then by deionized water, be washed till neutrality, the baking oven inner dryings of 90 ℃ 12 hours, then in the vacuum drying oven of 130 ℃ of temperature, be dried 14 hours, obtain the polyacrylonitrile based activated carbon fiber through nitric acid pretreatment.In pretreated polyacrylonitrile based activated carbon fiber, add excessive SOCl
2, at 90 ℃, react 6h, and then be warming up to 130 ℃ of remaining SOCl of removal
2, the cooling chloride polyacrylonitrile based activated carbon fiber that obtains.
4-aminopyridine ferrous solution is joined in chloride polyacrylonitrile based activated carbon fiber, at 60 ℃, react 24 hours, respectively with DMF, deionized water, sodium bicarbonate solution washing, extremely neutral with deionized water washing again, oven dry can obtain the activated carbon fiber loaded 4-aminopyridine iron catalyst of polyacrylonitrile-radical.
Embodiment 2
By PA and FeCl
3be dissolved in respectively in DMF solution, be mixed with respectively PA and FeCl
3solution, under the effect of magnetic stirring apparatus, by FeCl
3solution is added drop-wise in PA solution gradually, FeCl
3with the mol ratio of PA be 1:4, at 30 ℃, react and within 30 minutes, obtain PA ferrous solution.
Polyacrylonitrile based activated carbon fiber floods 15 hours in the red fuming nitric acid (RFNA) aqueous solution (nitric acid: the volume ratio of water is 1:3), then by deionized water, be washed till neutrality, the baking oven inner dryings of 90 ℃ 12 hours, then in the vacuum drying oven of 130 ℃ of temperature, be dried 14 hours, obtain the polyacrylonitrile based activated carbon fiber through nitric acid pretreatment.In pretreated polyacrylonitrile based activated carbon fiber, add excessive SOCl
2, at 90 ℃, react 6h, and then be warming up to 130 ℃ of remaining SOCl of removal
2, the cooling chloride polyacrylonitrile based activated carbon fiber that obtains.
PA ferrous solution is joined in chloride polyacrylonitrile based activated carbon fiber, at 60 ℃, react 24 hours, respectively with DMF, deionized water, sodium bicarbonate solution washing, extremely neutral with deionized water washing again, oven dry can obtain the activated carbon fiber loaded PA iron catalyst of polyacrylonitrile-radical.
Embodiment 3
By 4-aminopyridine and CoCl
2be dissolved in respectively in DMF solution, be mixed with respectively 4-aminopyridine and CoCl
2solution, under the effect of magnetic stirring apparatus, by CoCl
2solution is added drop-wise in 4-aminopyridine solution gradually, CoCl
2with the mol ratio of 4-aminopyridine be 1:4, at 30 ℃, react and within 30 minutes, obtain 4-aminopyridine cobalt liquor.
Polyacrylonitrile based activated carbon fiber floods 15 hours in the red fuming nitric acid (RFNA) aqueous solution (nitric acid: the volume ratio of water is 1:3), then by deionized water, be washed till neutrality, the baking oven inner dryings of 90 ℃ 12 hours, then in the vacuum drying oven of 130 ℃ of temperature, be dried 14 hours, obtain the polyacrylonitrile based activated carbon fiber through nitric acid pretreatment.In pretreated polyacrylonitrile based activated carbon fiber, add excessive SOCl
2, at 90 ℃, react 6h, and then be warming up to 130 ℃ of SOCl that removal is unnecessary
2, the cooling chloride polyacrylonitrile based activated carbon fiber that obtains.
4-aminopyridine cobalt liquor is joined in chloride polyacrylonitrile based activated carbon fiber, at 60 ℃, react 24 hours, respectively with DMF, deionized water, sodium bicarbonate solution washing, extremely neutral with deionized water washing again, oven dry can obtain the activated carbon fiber loaded 4-aminopyridine Co catalysts of polyacrylonitrile-radical.
Embodiment 4
By PA and CoCl
2be dissolved in respectively in DMF solution, be mixed with respectively PA and FeCl
3solution, under the effect of magnetic stirring apparatus, by CoCl
2solution is added drop-wise in PA solution gradually, CoCl
2with the mol ratio of PA be 1:4, at 30 ℃, react and within 30 minutes, obtain PA cobalt liquor.
Polyacrylonitrile based activated carbon fiber floods 15 hours in the red fuming nitric acid (RFNA) aqueous solution (nitric acid: the volume ratio of water is 1:3), then by deionized water, be washed till neutrality, the baking oven inner dryings of 90 ℃ 12 hours, then in the vacuum drying oven of 130 ℃ of temperature, be dried 14 hours, obtain the polyacrylonitrile based activated carbon fiber through nitric acid pretreatment.In pretreated polyacrylonitrile based activated carbon fiber, add excessive SOCl
2, at 90 ℃, react 6h, and then be warming up to 130 ℃ of remaining SOCl of removal
2, the cooling chloride polyacrylonitrile based activated carbon fiber that obtains.
PA cobalt liquor is joined in chloride polyacrylonitrile based activated carbon fiber, at 60 ℃, react 24 hours, respectively with DMF, deionized water, sodium bicarbonate solution washing, extremely neutral with deionized water washing again, oven dry can obtain the activated carbon fiber loaded PA Co catalysts of polyacrylonitrile-radical.
Embodiment 5
By 4-aminopyridine and FeCl
3be dissolved in respectively in DMSO solution, be mixed with respectively 4-aminopyridine and FeCl
3solution, under the effect of magnetic stirring apparatus, by FeCl
3solution is added drop-wise in 4-aminopyridine solution gradually, FeCl
3with the mol ratio of 4-aminopyridine be 1:4, at 30 ℃, react and within 30 minutes, obtain 4-aminopyridine ferrous solution.
Polyacrylonitrile based activated carbon fiber floods 15 hours in the red fuming nitric acid (RFNA) aqueous solution (nitric acid: the volume ratio of water is 1:3), then by deionized water, be washed till neutrality, the baking oven inner dryings of 90 ℃ 12 hours, then in the vacuum drying oven of 130 ℃ of temperature, be dried 14 hours, obtain the polyacrylonitrile based activated carbon fiber through nitric acid pretreatment.In pretreated polyacrylonitrile based activated carbon fiber, add excessive SOCl
2, at 90 ℃, react 6h, and then be warming up to 130 ℃ of remaining SOCl of removal
2, the cooling chloride polyacrylonitrile based activated carbon fiber that obtains.
4-aminopyridine ferrous solution is joined in chloride polyacrylonitrile based activated carbon fiber, at 60 ℃, react 24 hours, respectively with DMF, deionized water, sodium bicarbonate solution washing, extremely neutral with deionized water washing again, oven dry can obtain the activated carbon fiber loaded 4-aminopyridine iron catalyst of polyacrylonitrile-radical.
Embodiment 6
By 4-aminopyridine and FeCl
3be dissolved in respectively in DMF solution, be mixed with respectively 4-aminopyridine and FeCl
3solution, under the effect of magnetic stirring apparatus, by FeCl
3solution is added drop-wise in 4-aminopyridine solution gradually, FeCl
3with the mol ratio of 4-aminopyridine be 1:4.5, at 30 ℃, react and within 30 minutes, obtain 4-aminopyridine ferrous solution.
Polyacrylonitrile based activated carbon fiber floods 15 hours in the red fuming nitric acid (RFNA) aqueous solution (nitric acid: the volume ratio of water is 1:3), then by deionized water, be washed till neutrality, the baking oven inner dryings of 90 ℃ 12 hours, then in the vacuum drying oven of 130 ℃ of temperature, be dried 14 hours, obtain the polyacrylonitrile based activated carbon fiber through nitric acid pretreatment.In pretreated polyacrylonitrile based activated carbon fiber, add excessive SOCl
2, at 90 ℃, react 6h, and then be warming up to 130 ℃ of remaining SOCl of removal
2, the cooling chloride polyacrylonitrile based activated carbon fiber that obtains.
4-aminopyridine ferrous solution is joined in chloride polyacrylonitrile based activated carbon fiber, at 60 ℃, react 24 hours, respectively with DMF, deionized water, sodium bicarbonate solution washing, extremely neutral with deionized water washing again, oven dry can obtain the activated carbon fiber loaded 4-aminopyridine iron catalyst of polyacrylonitrile-radical.
Embodiment 7
By PA and CoCl
2be dissolved in respectively in DMF solution, be mixed with respectively PA and FeCl
3solution, under the effect of magnetic stirring apparatus, by CoCl
2solution is added drop-wise in PA solution gradually, CoCl
2with the mol ratio of PA be 1:4.5, at 30 ℃, react and within 30 minutes, obtain PA cobalt liquor.
Polyacrylonitrile based activated carbon fiber floods 15 hours in the red fuming nitric acid (RFNA) aqueous solution (nitric acid: the volume ratio of water is 1:3), then by deionized water, be washed till neutrality, the baking oven inner dryings of 90 ℃ 12 hours, then in the vacuum drying oven of 130 ℃ of temperature, be dried 14 hours, obtain the polyacrylonitrile based activated carbon fiber through nitric acid pretreatment.In pretreated polyacrylonitrile based activated carbon fiber, add excessive SOCl
2, at 90 ℃, react 6h, and then be warming up to 130 ℃ of remaining SOCl of removal
2, the cooling chloride polyacrylonitrile based activated carbon fiber that obtains.
PA cobalt liquor is joined in chloride polyacrylonitrile based activated carbon fiber, at 60 ℃, react 24 hours, respectively with DMF, deionized water, sodium bicarbonate solution washing, extremely neutral with deionized water washing again, oven dry can obtain the activated carbon fiber loaded PA Co catalysts of polyacrylonitrile-radical.
Embodiment 8
By 4-aminopyridine and FeCl
3be dissolved in respectively in DMF solution, be mixed with respectively 4-aminopyridine and FeCl
3solution, under the effect of magnetic stirring apparatus, by FeCl
3solution is added drop-wise in 4-aminopyridine solution gradually, FeCl
3with the mol ratio of 4-aminopyridine be 1:4, at 30 ℃, react and within 30 minutes, obtain 4-aminopyridine ferrous solution.
Viscose base activated carbon fiber floods 15 hours in the red fuming nitric acid (RFNA) aqueous solution (nitric acid: the volume ratio of water is 1:3), then by deionized water, be washed till neutrality, the baking oven inner dryings of 90 ℃ 12 hours, then in the vacuum drying oven of 130 ℃ of temperature, be dried 14 hours, obtain the viscose base activated carbon fiber through nitric acid pretreatment.In pretreated viscose base activated carbon fiber, add excessive SOCl
2, at 90 ℃, react 6h, and then be warming up to 130 ℃ of remaining SOCl of removal
2, the cooling chloride viscose base activated carbon fiber that obtains.
4-aminopyridine ferrous solution is joined in chloride viscose base activated carbon fiber, at 60 ℃, react 24 hours, respectively with DMF, deionized water, sodium bicarbonate solution washing, then with deionized water washing, to neutral, oven dry can obtain viscose base activated carbon fiber load 4-aminopyridine iron catalyst.
Several concrete case study on implementation of above combination; the present invention is further understood in exemplary explanation and help; but case study on implementation detail is only used to illustrate the present invention; do not represent that the present invention conceives lower whole technical scheme; therefore should not be construed as limited overall technical solution; some are In the view of technical staff; the unsubstantiality that does not depart from the present invention's design increases and changes; for example, to there is simple the change or replacement of technical characterictic of same or similar technique effect, all belong to protection domain of the present invention.
Claims (10)
1. a preparation method for activated carbon fiber loaded aminopyridine metal complex, comprises the steps:
(1) aminopyridine and slaine are dissolved in respectively in organic solvent, are mixed with respectively aminopyridine and metal salt solution; (2) described metal salt solution is dropwise joined in aminopyridine solution, obtain aminopyridine metal complex solution; (3) adopt thionyl chloride (SOCl
2) pretreated activated carbon fiber is processed, obtain having the activated carbon fiber of acid chloride group; (4) in the activated carbon fiber of acid chloride group, add described aminopyridine metal complex solution to react, after separation, washing and being dried, make activated carbon fiber loaded aminopyridine complex compound; The metal ion of described slaine can be a kind of in iron, cobalt, copper, manganese, zinc transition metal ions.
2. the preparation method of activated carbon fiber loaded aminopyridine metal complex as claimed in claim 1, is characterized in that: described aminopyridine is a kind of in 4-aminopyridine, 3-aminopyridine, PA.
3. the preparation method of activated carbon fiber loaded aminopyridine metal complex as claimed in claim 1, is characterized in that: the metal ion of described slaine is iron or cobalt metal ion, and molysite can be FeCl
2, FeCl
3, Fe (NO
3)
3, FeSO
4, Fe
2(SO
4)
3, Fe (ClO
4)
3in a kind of or their combination; Cobalt salt can be CoCl
2, Co (NO
3)
2, CoSO
4, Co (Ac)
2in a kind of or their combination.
4. the preparation method of activated carbon fiber loaded aminopyridine metal complex as claimed in claim 1, is characterized in that: described organic solvent is DMF, DMSO, DMAc.
5. the preparation method of activated carbon fiber loaded aminopyridine metal complex as claimed in claim 1, is characterized in that: described metal salt solution, by slaine is added in organic solvent, then stirs and makes for 10-30 minute at 20-50 ℃.
6. the preparation method of activated carbon fiber loaded aminopyridine metal complex as claimed in claim 1, is characterized in that: described activated carbon fiber is polyacrylonitrile based activated carbon fiber, viscose base activated carbon fiber and asphalt activity carbon fiber.
7. the preparation method of activated carbon fiber loaded aminopyridine metal complex as claimed in claim 1, it is characterized in that: described pretreatment is activated carbon fiber to be flooded in concentrated nitric acid solution to 12-24 hour, then by deionized water, be washed till neutrality, baking oven inner drying 10-20 hour at 80-100 ℃, then in vacuum drying chamber, be dried 12-24 hour, baking temperature is 100-130 ℃; The nitric acid of described concentrated nitric acid solution: the volume ratio of water is 1:1-1:3.
8. the preparation method of activated carbon fiber loaded aminopyridine metal complex as claimed in claim 1, it is characterized in that: described aminopyridine metal complex solution is under magnetic stirring apparatus effect, by the mol ratio of slaine and aminopyridine, be 1:2-1:6, described metal salt solution is added drop-wise to aminopyridine solution gradually, then stirs and obtain for 20-60 minute.
9. the preparation method of activated carbon fiber loaded aminopyridine metal complex as claimed in claim 1, is characterized in that: the activated carbon fiber of described acid chloride group is to add SOCl in pretreated activated carbon fiber
2, at 80-95 ℃, process 5-8h, then be warming up to the 130-150 ℃ of SOCl that removal is unnecessary
2, cooling obtaining.
10. the preparation method of activated carbon fiber loaded aminopyridine metal complex as claimed in claim 1, it is characterized in that: described activated carbon fiber loaded aminopyridine metal complex is that aminopyridine metallic solution is joined in the activated carbon fiber of acid chloride group, after 50-70 ℃ of reaction 12-28h, respectively with DMF, deionized water, sodium bicarbonate solution washing, extremely neutral with deionized water washing again, at 80-100 ℃, be dried, be dried and can obtain after 12-14 hour.
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