CN101818338B - Method for preparing nickel radical magnetic active carbon by non-palladium activation method - Google Patents
Method for preparing nickel radical magnetic active carbon by non-palladium activation method Download PDFInfo
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- CN101818338B CN101818338B CN2010101470773A CN201010147077A CN101818338B CN 101818338 B CN101818338 B CN 101818338B CN 2010101470773 A CN2010101470773 A CN 2010101470773A CN 201010147077 A CN201010147077 A CN 201010147077A CN 101818338 B CN101818338 B CN 101818338B
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Abstract
The invention discloses a method for preparing nickel radical magnetic active carbon, relating to a method for preparing magnetic active carbon. The invention solves the problem that the blockage of a screen and the loss of the active carbon are easily caused by using a filtering and separating method during the use of the prior powder active carbon. The method comprises the following steps of: 1, soaking the active carbon in a chitosan acetic acid solution, filtering, and then drying filtering slag; 2, activating surfaces; 3, adding the active carbon processed in the step 2 in the filtering liquid obtained in the step 2 to stir and plate, filtering, washing and drying to obtain the nickel radical magnetic active carbon. In the invention, the magnetic nickel can be introduced into the active carbon, the obtained nickel radical magnetic active carbon can be fully separated without filtering after use, thus, the invention not only solves the separation problem of the powder carbon, but also solves the problem of small adsorption capacity of the magnetic materials.
Description
Technical field
The present invention relates to a kind of method for preparing magnetic active carbon.
Background technology
Gac because of have highly developed pore texture, huge specific surface area, stable chemical property and good absorption property is widely used in metallurgy, medicine, food and environmental area.Powdered Activated Carbon also has fast, the cheap advantage of rate of adsorption, but there is the problem of separation difficulty in it in practical application, and the filtering separation method causes the loss of screen plugging or gac easily.Compare with traditional filtration method; It is a kind of advantages of simplicity and high efficiency separation method that magnetic separates; Materials such as detachable magnetic or magnetizable sorbent material, carrier, cell are widely used in fields such as biological chemistry, molecular biology, microbiology, cytobiology, analytical chemistry, environmental technology.
Summary of the invention
Technical problem to be solved by this invention is to adopt the filtering separation method to cause problem screen plugging or that gac runs off easily in the existing Powdered Activated Carbon use in order to solve, and a kind of method for preparing nickel radical magnetic active carbon is provided.
The method that the present invention prepares nickel radical magnetic active carbon is following: be that to be immersed in chitosan mass concentration be 5min～10min in 0.4%～0.6% the chitosan acetic acid soln to 200 orders～240 purpose gacs with fineness one; Filter, then filter residue is dried under 50 ℃～70 ℃ condition; Two, surface activation process: will passing through gac that step 1 handles, under the condition of room temperature, to be immersed in pH value be 10min～15min in 7～9 the chemical plating solution, and filtration joins 30 ℃～50 ℃, NaBH with filter residue then
4Concentration is the NaBH of 4g/L～8g/L
4Reduce 6min～10min in the alkali aqueous solution, filter; Three, will pass through that gac that step 2 handles joins that pH value is 6.0～8.5, temperature is stirring plating 30s～60s in 75 ℃～85 ℃ the filtrating of step 2 gained; Filter then, wash; Under 50 ℃～70 ℃ condition, dry again, promptly get nickel radical magnetic active carbon; Chemical plating solution described in the step 2 is made up of according to 1: 3 volume ratio nickel-plating liquid and deionized water; Said nickel-plating liquid is made up of single nickel salt, inferior sodium phosphate, sodium-acetate, lactic acid, ammonium chloride and thiocarbamide; Wherein the concentration of single nickel salt is 20g/L～50g/L; The concentration of inferior sodium phosphate is 20g/L～50g/L, and the concentration of sodium-acetate is 10g/L～45g/L, and concentration of lactic acid is 5g/L～35mL/L; The concentration of ammonium chloride is 10g/L～45g/L, and the concentration of thiocarbamide is 0g/L～0.006g/L.
Reaction equation is following in the step 2:
2H
2O+BH
4 -+2Ni
2+→2Ni↓+2H
2↑+BO
2 -+4H
+(1)
Reaction equation is following in the step 3:
2H
2PO
2 -+Ni
2++2H
2O→2H
2PO
3 -+H
2↑+2H
++Ni↓(2)
Present method can be introduced gac with the metallic nickel of magnetic; The nickel radical magnetic active carbon that obtains need not filter and can nickel radical magnetic active carbon be separated fully after using; Not only the separation problem of powder charcoal can be solved but also the little problem of magnetic loading capacity can be solved; The procedure that the present invention adopts electroless plating method simply, rapidly and efficiently, need not to contain palladium compound, be a kind of environmentally friendly, preparation method that the applications well prospect is arranged.
Description of drawings
Fig. 1 is the influence curve figure of the volume ratio of nickel-plating liquid and deionized water in the embodiment nine to gained nickel radical magnetic active carbon iodine number; The iodine number curve of plating 60s gained nickel radical magnetic active carbon in
expression step 3 among the figure, the iodine number curve of plating 30s gained nickel radical magnetic active carbon in
expression step 3 among the figure; Fig. 2 be in the embodiment nine the chemical plating solution volume to the influence curve figure of gained nickel radical magnetic active carbon iodine number; The iodine number curve of plating 30s gained nickel radical magnetic active carbon in
step 3 among the figure, the iodine number curve of plating 60s gained nickel radical magnetic active carbon in
expression step 3; Fig. 3 is the Socryl Blue BRL adsorption curve of used gac in the embodiment nine; Fig. 4 is the degree of metalization graphic representation of plating 60s gained nickel radical magnetic active carbon in the step 3 in the embodiment nine; Fig. 5 is the pore volume curve of the nickel radical magnetic active carbon in the embodiment nine; After
representes the 4ml nickel-plating liquid and deionized water mixes according to 1: 3 volume ratio among the figure; The pore volume curve of gained nickel radical magnetic active carbon; After
representes the 20ml nickel-plating liquid and deionized water mixes according to 1: 3 volume ratio; The pore volume curve of gained nickel radical magnetic active carbon, the pore volume curve of
expression former state gac; Fig. 6 is that the gained nickel radical magnetic active carbon amplifies 1000 times stereoscan photograph in the embodiment nine; Fig. 7 is that the gained nickel radical magnetic active carbon amplifies 3000 times stereoscan photograph in the embodiment nine; Fig. 8 is that the gained nickel radical magnetic active carbon amplifies 5000 times stereoscan photograph in the embodiment nine; Fig. 9 is that the gained nickel radical magnetic active carbon amplifies 10000 times stereoscan photograph in the embodiment nine; Figure 10 is the magnetic hysteresis loop of gained nickel radical magnetic active carbon in the embodiment nine.
Embodiment
Technical scheme of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: the method that non-palladium activation method prepares nickel radical magnetic active carbon in this embodiment is following: be that to be immersed in chitosan mass concentration be 5min～10min in 0.4%～0.6% the chitosan acetic acid soln to 200 orders～240 purpose gacs with fineness one; Filter, then filter residue is dried under 50 ℃～70 ℃ condition; Two, surface activation process: will passing through gac that step 1 handles, under the condition of room temperature, to be immersed in pH value be 10min～15min in 7～9 the chemical plating solution, and filtration joins 30 ℃～50 ℃, NaBH with filter residue then
4Concentration is the NaBH of 4g/L～8g/L
4Reduce 6min～10min in the alkali aqueous solution, filter; Three, will pass through that gac that step 2 handles joins that pH value is 6.0～8.5, temperature is stirring plating 30s～60s in 75 ℃～85 ℃ the filtrating of step 2 gained; Filter then, wash; Under 50 ℃～70 ℃ condition, dry again, promptly get nickel radical magnetic active carbon; Chemical plating solution described in the step 2 is made up of according to 1: 3 volume ratio nickel-plating liquid and deionized water.
NaBH described in this embodiment
4Alkali aqueous solution is by NaBH
4The NaOH aqueous solution that is dissolved in concentration and is 1g/L～5g/L makes.
Embodiment two: this embodiment and embodiment one are different is that the mass concentration of chitosan in the acetic acid soln of chitosan described in the step 1 is 0.5%.Other is identical with embodiment one.
Embodiment three: what this embodiment was different with one of embodiment one or two is in the step 1 filter residue to be dried under 60 ℃ condition.Other is identical with one of embodiment one or two.
Embodiment four: what this embodiment was different with one of embodiment one to three is that said nickel-plating liquid is made up of single nickel salt, inferior sodium phosphate, sodium-acetate, lactic acid, ammonium chloride and thiocarbamide; Wherein the concentration of single nickel salt is 20g/L～50g/L; The concentration of inferior sodium phosphate is 20g/L～50g/L, and the concentration of sodium-acetate is 10g/L～45g/L, and concentration of lactic acid is 5g/L～35mL/L; The concentration of ammonium chloride is 10g/L～45g/L, and the concentration of thiocarbamide is 0g/L～0.006g/L.Other is identical with one of embodiment one to three.
Embodiment five: this embodiment is different with one of embodiment one to four is in the step 2 filter residue to be joined 40 ℃ NaBH
4Reduce in the alkali aqueous solution.Other is identical with one of embodiment one to four.
Embodiment six: that this embodiment is different with one of embodiment one to five is the said NaBH of step 2
4NaBH in the alkali aqueous solution
4Concentration be 5g/L.Other is identical with one of embodiment one to five.
Embodiment seven: that this embodiment is different with one of embodiment one to six is the said NaBH of step 2
4NaBH in the alkali aqueous solution
4Concentration be 6g/L.Other is identical with one of embodiment one to six.
Embodiment eight: this embodiment is different with one of embodiment one to seven be will pass through in the step 3 that gac that step 2 handles joins that pH value is 8, temperature is stirring plating 50s in 80 ℃ the filtrating of step 2 gained.Other is identical with one of embodiment one to seven.
Embodiment nine: the method that non-palladium activation method prepares nickel radical magnetic active carbon in this embodiment is following: be that to be immersed in chitosan mass concentration be 10min in 0.5% the chitosan acetic acid soln to 230 purpose gacs with the 5g fineness one; Filter, then filter residue is dried under 60 ℃ condition; Two, surface activation process: will passing through gac that step 1 handles, under the condition of room temperature, to be immersed in pH value be 10min in 8 the chemical plating solution, and filtration joins 40 ℃, NaBH with filter residue then
4Concentration is the NaBH of 5g/L
4Reduce 8min in the alkali aqueous solution, filter; Three, will passing through gac that step 2 handles, to join temperature be to stir plating 30s～60s in 80 ℃ the filtrating of step 2 gained, filters then, washs, and under 60 ℃ condition, dries again, promptly gets nickel radical magnetic active carbon; Chemical plating solution described in the step 2 is made up of according to 1: 3 volume ratio nickel-plating liquid and deionized water; Said nickel-plating liquid is made up of single nickel salt, inferior sodium phosphate, sodium-acetate, lactic acid, ammonium chloride and thiocarbamide; Wherein the concentration of single nickel salt is 40g/L; The concentration of inferior sodium phosphate is 40g/L, and the concentration of sodium-acetate is 25g/L, and concentration of lactic acid is 25mL/L; The concentration of ammonium chloride is 25g/L, and the concentration of thiocarbamide is 0.003g/L.
Can know that by Fig. 1 the gained nickel radical magnetic active carbon can reach 1116.50mg/g when in the high temperature plating bath, reacting 30s; Can reach 1078.21mg/g during reaction 60s; The iodine number of used former state gac is 1035.10mg/g, and hence one can see that, and gac raises through iodine number behind the chemical nickel plating.
The whole iodine number that can be known plating 60s gained nickel radical magnetic active carbon in the step 3 by Fig. 2 is higher than the whole iodine number of plating 30s gained nickel radical magnetic active carbon.The plating bath volume does not influence as long as a certain amount of gac is reached enough within the specific limits.
Table 1
Table 2
| Sample quality g | 0.1005 | 0.1003 | 0.1006 | 0.1011 | 0.1002 | 0.1009 | 0.1006 | 0.1009 | 0.1010 | 0.1008 |
| Adsorptive value mg/g | 148.74 | 147.95 | 147.44 | 145.46 | 145.54 | 146.00 | 146.53 | 146.15 | 143.76 | 140.53 |
Can know that from table 1 (the Socryl Blue BRL adsorptive value of used gac this embodiment), Fig. 3 and table 2 (the Socryl Blue BRL adsorptive value of gained nickel radical magnetic active carbon in this embodiment) gained nickel radical magnetic active carbon and used gac are approaching to the absorption of Socryl Blue BRL.
By Fig. 4 find out in the step 3 plating time be between during 60s, gained nickel radical magnetic active carbon degree of metalization is with the increase of chemical plating solution amount and increases progressively trend.
Table 3
| Sample | Degree of metalization % | Specific surface area m 2/g | Pore volume V pore(mL/g) |
| AC | 0 | 942.86 | 0.462 |
| AC-1 | 3.35 | 879.00 | 0.424 |
| AC-2 | 16.37 | 859.12 | 0.417 |
AC representative expression former state gac in the table 3; After AC-1 represents the 4ml nickel-plating liquid and deionized water mixes according to 1: 3 volume ratio, the nickel radical magnetic active carbon of gained; After AC-2 represents the 20ml nickel-plating liquid and deionized water mixes according to 1: 3 volume ratio, the nickel radical magnetic active carbon of gained.
Can know that by table 3 and Fig. 5 the specific surface area before and after the gac nickel plating changes not quite, the quantity of mesopore micropore reduces to some extent, but relative proportion is almost constant.Though can analyze thus to the adsorptive power after the gac nickel plating descends to some extent, the degree that descends seldom.
But the overlay coating by Fig. 6-Fig. 9 knowledge capital embodiment gained nickel radical magnetic active carbon is fine and close; The metal sense is arranged; The original duct of gac is still high-visible, explains at the thickness of activated carbon surface metal plated coating forr a short time than the diameter of hole, can not cover the pore texture of gac.
Table 4
| Element | C | N | O | Na | P | S | Cl | Ni |
[0038]
| Weight % | 26.07 | 02.97 | 04.31 | 01.64 | 01.75 | 00.42 | 00.43 | 62.42 |
| Atomicity % | 56.12 | 05.47 | 06.96 | 01.85 | 01.46 | 00.34 | 00.31 | 27.49 |
Can be known by table 4 and to utilize energy spectrometer to measure gained nickel radical magnetic active carbon overlay coating composition and content, analytical results can obtain containing in the overlay coating Ni, P element, and the massfraction of nickel is 97.73%, and the content of phosphorus is 2.27%, is low-phosphorous coating.All the other elements are mainly from gac and treatment with chitosan.
Can know that from Figure 10 the magnetic performance that the gained nickel radical magnetic active carbon is unique: saturation magnetization (Ms) is 0.56927emu/g, and residual magnetization (Mr) is 76.140 * 10
-3Emu/g, coercive force (Hc) is 26.169G.In addition, magnetic property can characterize through remanence ratic (Mr/MS), the Mr/Ms=0.134 of gained nickel radical magnetic active carbon, and this low remanence ratic (＜0.25) shows that the nickel radical magnetic active carbon of gained demonstrates superparamagnetism.
Can know that by above result the gained nickel radical magnetic active carbon has perfection relatively, homogeneous, good shapes and porous shell structure, and iodine and Socryl Blue BRL are had higher adsorptive power.
Embodiment ten: the method that non-palladium activation method prepares nickel radical magnetic active carbon in this embodiment is following: be that to be immersed in chitosan mass concentration be 5min in 0.4% the chitosan acetic acid soln to 200 purpose gacs with fineness one; Filter, then filter residue is dried under 50 ℃ condition; Two, surface activation process: will passing through gac that step 1 handles, under the condition of room temperature, to be immersed in pH value be 10min in 7 the chemical plating solution, and filtration joins 30 ℃, NaBH with filter residue then
4Concentration is the NaBH of 4g/L
4Reduce 6min in the alkali aqueous solution, filter; Three, will pass through that gac that step 2 handles joins that pH value is 6.0, temperature is stirring plating 30s in 75 ℃ the filtrating of step 2 gained, filters then, washs, and under 50 ℃ condition, dries again, promptly gets nickel radical magnetic active carbon; Chemical plating solution described in the step 2 is made up of according to 1: 3 volume ratio nickel-plating liquid and deionized water.
Embodiment 11: the method that non-palladium activation method prepares nickel radical magnetic active carbon in this embodiment is following: be that to be immersed in chitosan mass concentration be 10min in 0.6% the chitosan acetic acid soln to 240 purpose gacs with fineness one; Filter, then filter residue is dried under 70 ℃ condition; Two, surface activation process: will passing through gac that step 1 handles, under the condition of room temperature, to be immersed in pH value be 15min in 9 the chemical plating solution, and filtration joins 50 ℃, NaBH with filter residue then
4Concentration is the NaBH of 8g/L
4Reduce 10min in the alkali aqueous solution, filter; Three, will pass through that gac that step 2 handles joins that pH value is 8.5, temperature is stirring plating 60s in 85 ℃ the filtrating of step 2 gained, filters then, washs, and under 70 ℃ condition, dries again, promptly gets nickel radical magnetic active carbon; Chemical plating solution described in the step 2 is made up of according to 1: 3 volume ratio nickel-plating liquid and deionized water.
Claims (7)
1. method for preparing nickel radical magnetic active carbon; The method that it is characterized in that preparing nickel radical magnetic active carbon is following: be that to be immersed in chitosan mass concentration be 5min～10min in 0.4%～0.6% the chitosan acetic acid soln to 200 orders～240 purpose gacs with fineness one; Filter, then filter residue is dried under 50 ℃～70 ℃ condition; Two, surface activation process: will passing through gac that step 1 handles, under the condition of room temperature, to be immersed in pH value be 10min～15min in 7～9 the chemical plating solution, and filtration joins 30 ℃～50 ℃, NaBH with filter residue then
4Concentration is the NaBH of 4g/L～8g/L
4Reduce 6min～10min in the alkali aqueous solution, filter; Three, will pass through that gac that step 2 handles joins that pH value is 6.0～8.5, temperature is stirring plating 30s～60s in 75 ℃～85 ℃ the filtrating of step 2 gained; Filter then, wash; Under 50 ℃～70 ℃ condition, dry again, promptly get nickel radical magnetic active carbon; Chemical plating solution described in the step 2 is made up of according to 1: 3 volume ratio nickel-plating liquid and deionized water; Said nickel-plating liquid is made up of single nickel salt, inferior sodium phosphate, sodium-acetate, lactic acid, ammonium chloride and thiocarbamide; Wherein the concentration of single nickel salt is 20g/L～50g/L; The concentration of inferior sodium phosphate is 20g/L～50g/L, and the concentration of sodium-acetate is 10g/L～45g/L, and concentration of lactic acid is 5g/L～35mL/L; The concentration of ammonium chloride is 10g/L～45g/L, and the concentration of thiocarbamide is 0g/L～0.006g/L.
2. a kind of method for preparing nickel radical magnetic active carbon according to claim 1, the mass concentration that it is characterized in that chitosan in the acetic acid soln of chitosan described in the step 1 is 0.5%.
3. a kind of method for preparing nickel radical magnetic active carbon according to claim 1 and 2 is characterized in that in the step 1 filter residue being dried under 60 ℃ condition.
4. a kind of method for preparing nickel radical magnetic active carbon according to claim 1 and 2 is characterized in that in the step 2 filter residue joined 40 ℃ NaBH
4Reduce in the alkali aqueous solution.
5. a kind of method for preparing nickel radical magnetic active carbon according to claim 4 is characterized in that the said NaBH of step 2
4NaBH in the alkali aqueous solution
4Concentration be 5g/L.
6. a kind of method for preparing nickel radical magnetic active carbon according to claim 4 is characterized in that the said NaBH of step 2
4NaBH in the alkali aqueous solution
4Concentration be 6g/L.
7. according to claim 1,2,5 or 6 described a kind of methods that prepare nickel radical magnetic active carbon, it is characterized in that to pass through in the step 3 that gac that step 2 handles joins that pH value is 8, temperature is stirring plating 50s in 80 ℃ the filtrating of step 2 gained.
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| CN103114437B (en) * | 2013-02-01 | 2014-11-05 | 东华大学 | Method for chemically plating nickel at textile surface without using palladium |
| CN105803433B (en) * | 2016-04-20 | 2019-07-30 | 青岛科技大学 | A kind of alumina ceramic face no-palladium activating nickel chemical plating technology |
| CN108620088A (en) * | 2018-05-21 | 2018-10-09 | 北京鑫佰利科技发展有限公司 | A kind of preparation method of water process high grade oxidation catalytic agent |
| CN110918052A (en) * | 2019-10-28 | 2020-03-27 | 安徽省通源环境节能股份有限公司 | Preparation process of magnetic livestock bone carbonized particle adsorbent |
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| CN1234451C (en) * | 2002-11-13 | 2006-01-04 | 中国科学院生态环境研究中心 | Preparing Method for magnetic active carbon used for water treatment |
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