CN109850893A - A kind of preparation method and application of ox bone active carbon - Google Patents
A kind of preparation method and application of ox bone active carbon Download PDFInfo
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- CN109850893A CN109850893A CN201910076995.2A CN201910076995A CN109850893A CN 109850893 A CN109850893 A CN 109850893A CN 201910076995 A CN201910076995 A CN 201910076995A CN 109850893 A CN109850893 A CN 109850893A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 185
- 229910052799 carbon Inorganic materials 0.000 title claims abstract description 112
- 210000000988 bone and bone Anatomy 0.000 title claims abstract description 105
- 238000002360 preparation method Methods 0.000 title claims abstract description 57
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 92
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims abstract description 74
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims abstract description 72
- 239000012190 activator Substances 0.000 claims abstract description 54
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims abstract description 37
- 239000011592 zinc chloride Substances 0.000 claims abstract description 36
- 235000005074 zinc chloride Nutrition 0.000 claims abstract description 36
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 8
- 238000001994 activation Methods 0.000 claims description 48
- 230000004913 activation Effects 0.000 claims description 46
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 19
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 12
- 238000003763 carbonization Methods 0.000 claims description 11
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 10
- 238000005238 degreasing Methods 0.000 claims description 10
- 239000000126 substance Substances 0.000 claims description 9
- 238000007598 dipping method Methods 0.000 claims description 8
- 238000005554 pickling Methods 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000001035 drying Methods 0.000 claims description 7
- 238000009835 boiling Methods 0.000 claims description 6
- 230000008859 change Effects 0.000 claims description 6
- 239000012634 fragment Substances 0.000 claims description 6
- 238000000034 method Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 238000005470 impregnation Methods 0.000 claims description 5
- 239000002957 persistent organic pollutant Substances 0.000 claims description 5
- 239000000654 additive Substances 0.000 claims description 4
- 230000000996 additive effect Effects 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 235000013372 meat Nutrition 0.000 claims description 4
- 239000000843 powder Substances 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 239000013527 degreasing agent Substances 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 3
- 239000004519 grease Substances 0.000 claims description 3
- 230000009182 swimming Effects 0.000 claims description 3
- 238000010792 warming Methods 0.000 claims description 3
- 238000005255 carburizing Methods 0.000 claims description 2
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 238000004080 punching Methods 0.000 claims 1
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 abstract description 78
- 229960000907 methylthioninium chloride Drugs 0.000 abstract description 78
- 238000001179 sorption measurement Methods 0.000 abstract description 53
- 230000000694 effects Effects 0.000 abstract description 42
- 125000000524 functional group Chemical group 0.000 abstract description 15
- 238000010835 comparative analysis Methods 0.000 abstract description 2
- 238000010521 absorption reaction Methods 0.000 description 17
- 239000000243 solution Substances 0.000 description 15
- 238000004458 analytical method Methods 0.000 description 10
- 239000000523 sample Substances 0.000 description 10
- 230000001965 increasing effect Effects 0.000 description 9
- 238000002474 experimental method Methods 0.000 description 6
- 238000002336 sorption--desorption measurement Methods 0.000 description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 4
- 239000003610 charcoal Substances 0.000 description 4
- 239000011148 porous material Substances 0.000 description 4
- 239000011591 potassium Substances 0.000 description 4
- 229910052700 potassium Inorganic materials 0.000 description 4
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 3
- 241000209094 Oryza Species 0.000 description 3
- 235000007164 Oryza sativa Nutrition 0.000 description 3
- 230000003213 activating effect Effects 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 3
- 238000006297 dehydration reaction Methods 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 235000009566 rice Nutrition 0.000 description 3
- 241000894007 species Species 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- 241000283690 Bos taurus Species 0.000 description 2
- 230000002378 acidificating effect Effects 0.000 description 2
- 229940036811 bone meal Drugs 0.000 description 2
- 239000002374 bone meal Substances 0.000 description 2
- 235000013399 edible fruits Nutrition 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011259 mixed solution Substances 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000002689 soil Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000002344 surface layer Substances 0.000 description 2
- 229910052725 zinc Inorganic materials 0.000 description 2
- 239000011701 zinc Substances 0.000 description 2
- RLLPVAHGXHCWKJ-IEBWSBKVSA-N (3-phenoxyphenyl)methyl (1s,3s)-3-(2,2-dichloroethenyl)-2,2-dimethylcyclopropane-1-carboxylate Chemical compound CC1(C)[C@H](C=C(Cl)Cl)[C@@H]1C(=O)OCC1=CC=CC(OC=2C=CC=CC=2)=C1 RLLPVAHGXHCWKJ-IEBWSBKVSA-N 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 238000004566 IR spectroscopy Methods 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000007792 addition Methods 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 238000002159 adsorption--desorption isotherm Methods 0.000 description 1
- 239000012675 alcoholic extract Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 235000015278 beef Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 150000001875 compounds Chemical group 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000011067 equilibration Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000011261 inert gas Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 210000000936 intestine Anatomy 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000012263 liquid product Substances 0.000 description 1
- 244000144972 livestock Species 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- MCPLVIGCWWTHFH-UHFFFAOYSA-L methyl blue Chemical compound [Na+].[Na+].C1=CC(S(=O)(=O)[O-])=CC=C1NC1=CC=C(C(=C2C=CC(C=C2)=[NH+]C=2C=CC(=CC=2)S([O-])(=O)=O)C=2C=CC(NC=3C=CC(=CC=3)S([O-])(=O)=O)=CC=2)C=C1 MCPLVIGCWWTHFH-UHFFFAOYSA-L 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 235000013594 poultry meat Nutrition 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
Landscapes
- Carbon And Carbon Compounds (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
A kind of preparation method and application of ox bone active carbon is related to domestic refuse comprehensive utilization and Adsorption of Organic agent preparation technical field.The present invention is utilized respectively zinc chloride, potassium hydroxide, phosphoric acid as activator and is activated ox bone carbide to prepare ox bone active carbon.It has been found through experimentation that: under the conditions of 400 DEG C, carbonize 2h, activator is made with zinc chloride, the ox bone active carbon that 90min preparation is activated at 400 DEG C is best to the adsorption effect of methylene blue, the active carbon that 0.3g is prepared with zinc chloride is added in the methylene blue solution of 100mL, 100mg/L, its adsorption rate removal rate after 4.5h reaches 100%, additionally by its surface functional group measure comparative analysis it can be concluded that, ox bone activated carbon adsorption methylene blue is not only related with its hole, also related with the functional group on its surface.
Description
Technical field
The present invention relates to domestic refuse comprehensive utilization and Adsorption of Organic agent preparation technical fields, are specifically related to
A kind of preparation method and application of ox bone active carbon.
Background technique
China is populous nation, and annual edible and consumption meat is extremely more, according to related data, what China in 2015 consumed
Pig, there are about 9x10 for beef or mutton class7Ton, wherein there are about 85x10 for the bone class after edible4Ton accounts for about the 1/4 of the whole world.It is generated each
Kind bone class is also extremely more, how rationally to utilize these ox bone recyclings after edible, being one is worth our explore and studies
Problem.At present, China's bone utilization of resources this aspect also there have been no large-scale development, how recycle bone class,
The problem of by-product value of raising livestock and poultry meat, the loss to reduce environmental pollution with resource is our a worth exploration.
There is the processing and utilization that generally can be divided into food-grade to bone class progress resource utilization at present, such as Zhang Ting, Yin et al.
Application of the micro- bone meal mentioned in Western-style intestines based article and in terms of bone mud, bone involved in Wang Wei, Zhang Zhiyu et al.
Application such as extraction of oil etc.；Another is exactly to prepare bone black or bone active charcoal, to the organic matter or a huge sum of money in water quality or soil
Category is adsorbed.Huang Yizong and Hu Ying et al. active carbon and the soil sample culture rice containing heavy metal pollution, observe seedling stage water
Rice adsorbs the influence of heavy metal, studies have shown that application bone black is bigger on the influence of Rice Seedlings root border cells Fe, Zn content, it is right
Other elements content there is no influence.J.C.Moreno-Piraj á n and R.G ó mez-Cruz et al. research is living with ox bone
Property charcoal absorption ion of copper and lead mixed solution, study it in mixed solution, the mutual absorption competition relationship of different ions
Additionally by the absorption property of the bone black carbonized respectively in comparison inert gas and air, aperture can be different, and its surface
Electronegativity and the size of adion also will affect the adsorptivity of bone black.
Aspect there are two ox bone active carbon is main to the ability of Adsorption of Organic, first is that surface characteristics of macrostructure,
The specific surface area, pore volume and pore structure of such as ox bone active carbon, the other is the chemical property of ox bone activated carbon surface,
Such as functional group, acid-base property and electrochemical properties.Utilize the organic pollutant major advantage in ox bone activated carbon adsorption waste water
Have: (1) organic pollutant of some low concentrations can be adsorbed, (2) can reuse, and (3) secondary pollution is small, and (4) are available
Adsorbent species are more.Active carbon is prepared using ox bone in the present invention, while probing into ox bone and prepare the optimum condition of active carbon,
Its adsorption effect to methylene blue is studied, to probe into its removal ability to organic pollutant.
Summary of the invention
For the technical problems in the prior art, it the present invention provides a kind of preparation method of ox bone active carbon, obtains
The ox bone active carbon obtained can be applied to the absorption of methylene blue, and then realize the adsorption treatment to organic pollutant.
To achieve the goals above, the technical scheme adopted by the invention is as follows: a kind of preparation method of ox bone active carbon,
It is characterized in that, steps are as follows:
1. ox bone pre-processes
The substances such as remaining meat on ox bone are removed with scalpel, ox bone is sawed-off at fritter, remove internal marrow, stream
Water is rinsed well, after be placed in baking oven it is dry；
2. the coarse crushing of ox bone
Pretreated ox bone is hammered into shape repeatedly and is pounded to fragment；
3. the degreasing of ox bone
Suitable water is added in ox bone fragment after coarse crushing, and boiling carries out degreasing repeatedly, until swimming in water without grease
Face surface layer, the ox bone after degreasing are dried after cleaning up；
4. ox bone is finely divided
It is finely divided to the ox bone progress after degreaser drying, cross 40-100 mesh；
5. charing prepares ox bone charcoal
Ox bone powder is put into vacuum tube furnace, heating charing, then cooling is ox bone charcoal；
6. the activation of ox bone charcoal
Impregnation is carried out to ox bone charcoal using activator, is successively dried after dipping, is high in vacuum tube furnace
Temperature activation；
7. pickling, washing
Pickling is carried out with the ox bone active carbon that hydrochloric acid completes preparation, then washes, is dry.
Optimal technical scheme as preparation method of the invention:
5. middle carburizing temperature is 400 DEG C, carbonization time 2h to above-mentioned steps, and heating rate is 10 DEG C/min, and charing terminates
Natural cooling afterwards.
Above-mentioned steps 6. in activator be zinc chloride, potassium hydroxide or phosphoric acid, dip time 12h.
Above-mentioned steps 6. employed in liquor zinci chloridi mass fraction be 40%, potassium hydroxide solution concentration be 1g/
L, the mass fraction of phosphoric acid are 70%；Liquor zinci chloridi, potassium hydroxide solution additive amount be that every 1mg ox bone charcoal adds 2mL
Activator, the additive amount of phosphoric acid are the activator that every 1mg ox bone charcoal adds 3mL.
6. above-mentioned steps after middle dipping, are dipped into object and are placed in baking oven at 105 DEG C dry 12h.
Above-mentioned steps 6. in will be placed again into vacuum tube furnace after drying by the ox bone charcoal of dipping, be passed through nitrogen,
400 DEG C are warming up to the speed of 10 DEG C/min, and constant temperature 90min is activated, and sample is taken when it is naturally cooling to 80 DEG C
Out.
Above-mentioned steps 7. in be added in ox bone active carbon in suitable 0.1mol/L hydrochloric acid solution, be heated to boiling
20min。
Above-mentioned steps 7. in after pickling with 70-80 DEG C of pure water repeated flushing to pH in 6-7, then will be after sample filtering
It is put into baking oven, is dried under the conditions of 105 DEG C to constant weight.
Compared with prior art, beneficial effects of the present invention are shown:
1), the present invention in carbonization temperature is 400 DEG C, carbonization time 2h, and activation temperature is used three under conditions of 400 DEG C
In the active carbon of the different activators preparations of kind, the Z-BC-3 specific surface area of zinc chloride activation preparation is up to
105.186m2The K-BC-3 of/g, followed by activation of potassium hydroxide preparation does active carbon specific surface area prepared by activator and is
72.586m2It is 57.338m that/g, which is finally the H-BC-3 specific surface area of phosphoric acid activation preparation,2/g.Additionally by suitable
The experiment of 100mg/L methylene blue adsorption number is as can be seen that 40 mesh are in the ox bone active carbon of 40 mesh, 60 mesh and 100 mesh in this experiment
Best mesh number.Under the conditions of same dosage, Z-BC-3 is best to the adsorption effect of methylene blue, and K-BC-3 takes second place, and H-BC-3 is most
Difference.In addition in the case where different dosages, adsorb 100mL, 100mg/L methylene blue solution, Z-BC-3 add into
Removal rate just has reached 100% after 0.3g, and K-BC-3 exists into 0.5g most removal rate in 91% or so, H-BC-3 adding
It adds 0.5g and also there was only 65% or so to the removal rate of methylene blue.
2), by FT-IR analysis it can be concluded that, different activators can generate different functions when activating ox bone charcoal really
Group, and different activators can all play dehydration when preparing active carbon, in addition phosphoric acid, which makees activator, will lead to acidity
Functional group greatly increases, and potassium hydroxide, which makees activator, can then generate a large amount of basic functionality.
3), by the absorption to methylene blue, and comprehensive BET, FT-IR analysis is it can be found that activated carbon adsorption methylene
Blue mechanism is physical absorption and chemical reaction two ways collective effect, and adsorption effect is good, and removal efficiency is high.
Detailed description of the invention
Fig. 1 is the process flow chart of the preparation method of ox bone active carbon of the invention；
Fig. 2 is that not activated ox bone charcoal is prepared under different carbonization temperatures to the removal rate curve of methylene blue；
Fig. 3 is removal rate curve of the active carbon to methylene blue of different activator preparations；
Fig. 4 is removal rate curve of the active carbon to methylene blue of different activator preparations；
Fig. 5 is the removal rate curve that the zinc chloride activation of different dosages prepares Z-BC-3 to methylene blue；
Fig. 6 is removal rate curve of the K-BC-3 to methylene blue of the activation of potassium hydroxide preparation of different dosages；
Fig. 7 is removal rate curve of the H-BC-3 to methylene blue of the phosphoric acid activation preparation of different dosages；
Fig. 8 is the removal rate curve that different activator differences add carbon content active to methylene blue；
Fig. 9 is removal rate curve of the different dosage different meshes active carbons to methylene blue；
Figure 10 is non-activated ox bone charcoal BC-2 (a), the active carbon K-BC-3 (b) prepared by potassium hydroxide, uses phosphoric acid
Adsorption-desorption etc. in the BET of prepared active carbon H-BC-3 (c) and the active carbon Z-BC-3 (d) prepared by zinc chloride
Warm curve；
Figure 11 is non-activated ox bone charcoal BC-2 (A), the active carbon Z-BC-3 (B) prepared by zinc chloride, uses hydroxide
The SEM spectrum of active carbon K-BC-3 (C) prepared by potassium and the active carbon H-BC-3 (D) prepared by phosphoric acid；
Figure 12 is non-activated ox bone charcoal BC-2 (A), the active carbon H-BC-3 (B) prepared by phosphoric acid, uses potassium hydroxide
The infrared spectrogram of prepared active carbon K-BC-3 (C) and the active carbon Z-BC-3 (D) prepared by zinc chloride；
Figure 13 is the absorption front and back infrared spectrogram that active carbon is prepared using zinc chloride activation；
Figure 14 is the absorption front and back infrared spectrogram that active carbon is prepared using phosphoric acid activation；
Figure 15 is the absorption front and back infrared spectrogram that active carbon is prepared using activation of potassium hydroxide.
Specific embodiment
It is made further with preparation method and application of the attached drawing to ox bone active carbon of the invention with reference to embodiments
It is described in detail.
Embodiment 1
Refering to Figure 1, a kind of preparation method of ox bone active carbon, steps are as follows:
1. ox bone pre-processes
The substances such as remaining meat on ox bone are removed with scalpel, it is with hacksaw that ox bone is sawed-off at the ox bone block for being about 5cm,
Remove internal marrow, flowing water is rinsed well, after be placed on 105 DEG C of temperature of setting, freeze-day with constant temperature 12h in baking oven.
2. the coarse crushing of ox bone
Pretreated ox bone hammer hammers the ox bone fragment pounded to particle diameter about 0.5cm-1cm size into shape repeatedly.
3. the degreasing of ox bone
Ox bone fragment after coarse crushing is installed with triangular flask, and suitable water is added, and wrapping is placed on high-pressure steam sterilizing pan
Inside boiling repeatedly carries out degreasing, until swimming in water surface surface layer without grease.Ox bone after degreasing, which cleans up, is placed on baking
105 DEG C in case, packs, be placed in spare in drier after dry 12h.
4. ox bone is finely divided
Ox bone after degreaser drying is crushed using high speed Universal pulverizer, it is allowed to cross 40,60 and 100 meshes respectively, is collected,
Pack, it is labelled, it is placed in spare in drier.
5. charing prepares ox bone charcoal
The ox bone 50g for weighing three kinds of different meshes respectively, is put into vacuum tube furnace, experimental provision is adjusted, in nitrogen
Under protection, temperature program is set as 10 DEG C/min, is warming up to 400 or 800 DEG C, and constant temperature carbonizes 2h, certainly to electron tubes type furnace temperature
80 DEG C or so rear taking-up samples, as ox bone charcoal so are cooled to, pack is stored in respectively after the ox bone charcoal of different meshes is weighed
It is spare in drier.
6. the activation of ox bone charcoal
Zinc chloride, potassium hydroxide and phosphoric acid is respectively adopted, impregnation is carried out to the ox bone charcoal of different meshes, in which:
Impregnation condition of the zinc chloride to ox bone are as follows: liquor zinci chloridi mass fraction is 40%, and impregnating ratio is that 2:1 is [molten
Liquid product (mL): ox bone charcoal quality (mg)].
Impregnation condition of the potassium hydroxide to ox bone charcoal are as follows: potassium hydroxide solution concentration is 1g/L, impregnating ratio 2:1
[liquor capacity (mL): ox bone charcoal quality (mg)].
The treatment conditions that phosphoric acid impregnates ox bone charcoal are as follows: the impregnating ratio of 70% phosphoric acid is 3:1 [liquor capacity (mL): ox bone
Charcoal quality (mg)].
Dip time is 12h, after dipping, is dipped into object and is placed in 105 DEG C of dry 12h in baking oven.After drying
It is placed again into vacuum tube furnace by the different meshes ox bone charcoal of dipping, is passed through nitrogen, is risen respectively with the speed of 10 DEG C/min
To 400,800,850 DEG C, constant temperature 90min is activated temperature, takes out sample when it is naturally cooling to 80 DEG C or so.Weighing
After pack it is spare.
7. pickling is washed
Pickling is carried out with the ox bone active carbon that the hydrochloric acid of 0.1mol/L completes preparation.Specific step is as follows: living in ox bone
It is added in suitable 0.1mol/L hydrochloric acid solution, is heated to after boiling 20min, with 70-80 DEG C of pure water repeated flushing in property charcoal
Until pH is in 6-7 or so.Baking oven will be put into after sample filtering again, is dried under the conditions of 105 DEG C to constant weight, pack is put into drying
It is spare in device.
Experiment condition and the preparation product number that ox bone active carbon is prepared under above-mentioned different condition are as shown in table 1.
1 different condition of table prepares ox bone active carbon
One, active carbon yield counts
By above-mentioned experiment, the yield of prepared active carbon is calculated.When counting 400 DEG C of carbonization temperature, charing
Between 2h, the yield of three kinds of active carbons is prepared at 400 DEG C of activation temperature.Calculated result is as shown in table 2.
Calculation formula are as follows: W=m/m0* 100%
Wherein: m is quality of activated carbon, g；m0For raw material quality, g.
Active carbon yield under 2 three kinds of preparation conditions of table
| Activator | Active carbon title | Yield |
| Zinc chloride | Z-BC-3 | 46.75% |
| Potassium hydroxide | K-BC-3 | 34.54% |
| Phosphoric acid | H-BC-3 | 62.89% |
From table 2 it can be seen that preparing resulting active carbon H-BC-3 yield highest with phosphoric acid, zinc chloride prepares obtained
Active carbon Z-BC-3 yield is moderate, and to prepare obtained active carbon K-BC-3 yield minimum for potassium hydroxide, illustrates identical
Under preparation condition, the bone black yield of different activator activation preparations is not identical, the reason is that different activators are in bone black
The influence degree and action site of portion's structure are simultaneously different.
Two, influence of the carbonization temperature to ox bone charcoal adsorption effect
3 parts of 100mL concentration be 100mg/L methylene blue solution in be separately added into 0.5g BC-2, BC-1 ox bone charcoal and
Pretreated bovine bone powder is crossed, is mixed, every 12h measurement bone black to the removal rate of methylene blue, is drawn, as a result such as Fig. 2 institute
Show.
Fig. 2 is that not activated ox bone charcoal is prepared under different carbonization temperatures to the removal rate curve of methylene blue.In Fig. 2, ox
Bone meal be it is edible after ox bone through the smashed bovine bone powder being prepared of degreasing, BC-1 and BC-2 are in different charings respectively
Temperature and carbonization time (BC-1:800 DEG C, 8h；BC-2:400 DEG C, 2h) under the not activated ox bone charcoal that is prepared into, three kinds of objects
The adsorption effect of confrontation methylene blue is as shown in Figure 2.By comparative analysis as can be seen that without charing and different charing temperature
The lower ox bone charcoal prepared of degree, the physical characteristic and adsorption effect showed be not identical.BC-2 to after 48h to methylene
Blue removal rate nearly 40%, and adsorption effect is substantially absent to methylene blue in ox bone and BC-1, BC-1 removes methylene blue
Rate is about 7.5% or so.Reason is: carbonization temperature is excessively high to cause organic principle volatilization loss in ox bone only to remain ash content, internal
Gap collapses, and loses the adsorptivity to organic substance, and BC-1 product form is presented canescence and also demonstrates this point, ash content
Suction-operated there's almost no to organic substance, and 400 DEG C, has apparent removal effect to methylene blue after the BC-2 of 2h preparation
Fruit.Illustrate that carbonization temperature is prepared with apparent influence to ox bone charcoal.
Three, influence of the activation temperature to ox bone charcoal adsorption effect
The above-mentioned several ox bone active carbons of 0.5g are added in the methylene blue solution that 100mL concentration is 100mg/L, measure it
To the removal rate of methylene blue, draw, as a result as shown in Figure 3.
Fig. 3 is removal rate curve of the active carbon to methylene blue of different activator preparations, as seen in Figure 3,
In the 4.5h measured, K-BC-2 and Z-BC-2 are not much variation to the removal rate of methylene blue substantially, 7% or so,
And H-BC-2/3 has reached 52% to the removal rate of methylene blue and not yet reaches adsorption equilibrium, Z-BC-3 is in 4.5h
Afterwards to the removal rate of methylene blue close to 100%, K-BC-3 to the removal rate of methylene blue close to 70%.In summary it prepares
Active carbon condition, which can be seen that activation temperature, has a great impact to the preparation of different ox bone active carbons.
Four, influence of the activator species to adsorption effect of activated carbon in water
40 active carbon now for weighing the preparation of 0.3g difference activator respectively, is added to the Asia of 100mL concentration 100mg/L
In methyl blue solution, every 2h measurement active carbon to the removal rate of methylene blue, to removal effect such as Fig. 4 of methylene blue
It is shown.
Fig. 4 is removal rate curve of the active carbon to methylene blue of different activator preparations, from fig. 4, it can be seen that different
Type activator prepares going for the Z-BC-3 that active carbon is different to the adsorption effect of methylene blue, and wherein prepared by zinc chloride activation
Except effect is best, reach maximum value in 3h or so, removal rate adsorbs close to 100% and reaches balance, and activation of potassium hydroxide system
Standby K-BC-3 takes second place to the removal effect of methylene blue, and removal effect reaches maximum value in 8h, and removal rate reaches 73%, phosphoric acid
The H-BC-3 for activating preparation is worst to the removal effect of methylene blue with this condition, reaches in 6h to methylene blue removal rate
Maximum value, removal rate are about 43%.Analysis it is found that the active carbon Z-BC-3 for preparing as activator of zinc chloride to methylene blue
Removal effect it is best, the time used is most short, and the active carbon K-BC-3 that potassium hydroxide is prepared as activator is to methylene blue
Although high 20% or so, the K-BC-3 of active carbon H-BC-3 removal rate for preparing than phosphoric acid as activator of removal rate inhale
Attached methylene blue reaches the ratio H-BC-3 of time used in maximum removal effect and is mostly used 2h.Analysis the reason is that: the activation of different activators
Active carbon because the difference of surface functional group and gap structure causes adsorption efficiency and time of equilibrium adsorption different.
Five, influence of the active carbon dosage to adsorption effect
1, influence of the Z-BC-3 dosage to adsorption effect of activated carbon in water
The Z-BC- of 0.1g, 0.2g, 0.3g, 0.4g and 0.5g are added to the 100mg/L methylene blue solution of 100mL respectively
3, methylene blue solution is measured using ultraviolet-uisible spectrophotometer every 2h, calculates active carbon to methylene blue
Removal rate, result are as shown in Figure 5.
Fig. 5 is the removal rate curve that the zinc chloride activation of different dosages prepares Z-BC-3 to methylene blue, can be with by Fig. 5
Find out: with gradually increasing for active carbon dosage, methylene blue removal rate is constantly being increased, and adsorption effect is with throwing
The increase of dosage shows a kind of straight line increase effect, and when dosage is 0.3g, removal rate is increased to by initial 53.8%
Nearly 100%, it is not further added by substantially then and is reaching adsorption equilibrium in 4.5h or so, while with the increase of dosage, inhaling
Attached equilibration time is being gradually reduced.The reason is that because of the increase with active carbon dosage, suction-operated site constantly increases for analysis
More, suction-operated enhancing reaches maximum in 0.3g, then no longer changes, it can be seen that the work prepared with zinc chloride activation agent
Property charcoal be 0.3g/ (100mg/L) to the optimal dosage of methylene blue removal rate.
2, influence of the K-BC-3 dosage to adsorption effect of activated carbon in water
The hydrogen-oxygen of 0.1g, 0.2g, 0.3g, 0.4g and 0.5g is added in the 100mg/L methylene blue solution of 100mL respectively
The K-BC-3 for changing potassium activation preparation, at regular intervals surveys methylene blue solution using ultraviolet-uisible spectrophotometer
It is fixed, active carbon is calculated to the removal rate of methylene blue, and result is as shown in Figure 6.
Fig. 6 is removal rate curve of the K-BC-3 to methylene blue of the activation of potassium hydroxide preparation of different dosages, by Fig. 6
Known to: with the increase of dosage, the K-BC-3 of activation of potassium hydroxide preparation is equally constantly increasing the removal rate of methylene blue
Add, the time of its adsorption equilibrium is longer, although dosage removal rate in 0.5g reaches 91.5%, but it is flat to reach absorption
The time weigh but to need 10h, moreover, with the increase of dosage, although removal effect is increasing, reach adsorption equilibrium
Time also slowly increasing, adsorption equilibrium needs the time to be about 3.5h to add to being gradually incremented to when from dosage being 0.1g
It is 10h that 0.5g, which reaches adsorption equilibrium to need the time,.Analyze reason: the increase of dosage increases adsorption site really, causes
Removal rate increases, but with the increase of dosage, because certain reason inhibitory activity charcoals are to the adsorption-desorption of methylene blue
Rate causes the time for reaching adsorption equilibrium to increase.
3, influence of the H-BC-3 dosage to adsorption effect of activated carbon in water
0.1g, 0.2g, 0.3g, 0.4g and 0.5g are added respectively in the methylene blue solution that 100mL concentration is 100mg/L
The H-BC-3 of phosphoric acid activation preparation, at regular intervals surveys methylene blue solution using ultraviolet-uisible spectrophotometer
It is fixed, active carbon is calculated to the removal rate of methylene blue, and result is as shown in Figure 7.
Fig. 7 is the H-BC-3 of the phosphoric acid activation preparation of different dosages to the removal rate curve of methylene blue, can by Fig. 7
Know: as the H-BC-3 dosage of phosphoric acid activation preparation is continuously increased, to the removal rate of Methylene Blue in Solution also by
It is cumulative to add, but also there was only 62.3% when it adds the maximum material removal rate that 0.5g reaches adsorption equilibrium.And it reaches adsorption equilibrium
Time it is also very long, need 14h to get to adsorption equilibrium.Analysis reason: the H-BC-3 of phosphoric acid activation preparation itself adsorbs effect
Fruit is with regard to poor, although making of phosphoric acid, activator yield is relatively high, its adsorption effect will be nothing like zinc chloride and hydrogen-oxygen
Change potassium and does the effect that activator prepares active carbon.
The prepared active carbon of different activator activation carries out adsorption experiment under comprehensive Different adding amount, at regular intervals
Methylene blue solution is measured using ultraviolet-uisible spectrophotometer, calculates active carbon to the removal rate of methylene blue,
As a result as shown in Figure 8.
Fig. 8 is removal rate curve of the different activator difference dosages to methylene blue, as seen from Figure 8, zinc chloride
It is best to the adsorption effect of methylene blue to cook ox bone active carbon prepared by activator, and the used time is most short.Potassium hydroxide activates
Active carbon prepared by agent takes second place, and it is worst to the adsorption effect of methylene blue that phosphoric acid does active carbon prepared by activator, and phosphorus
Acid under the same conditions, the time of equilibrium adsorption reached also longest.Phosphoric acid makees activator, compare other two kinds of activators and
Speech, prepared by adsorption effect of activated carbon in water can not show a candle to other two kinds.And not for active carbon effect prepared by potassium hydroxide
Such as zinc chloride.Preliminary analysis is that potassium hydroxide is caused to be lower than chlorine to the removal rate of methylene blue due to surface functional group
Change zinc and does active carbon prepared by activator.
Six, influence of the active carbon size to adsorption effect
Individually methylene blue is adsorbed using Z-BC-3 prepared by the zinc chloride activation of different meshes, while being investigated not
With dosage to different meshes Z-BC-3 to the adsorption effect of methylene blue, as shown in Figure 9.
Fig. 9 is removal rate curve of the different dosage different meshes active carbons to methylene blue, as seen from Figure 9, nothing
It is all the ox bone active carbon of 40 mesh by be dosage being the Z-BC-3 of the zinc chloride activation preparation of 0.2g in 0.1g or dosage
It is more preferable to the adsorption effect of methylene blue, so preliminary judgement, in 40 mesh, between three mesh number active carbons of 60 mesh and 100 mesh
In, 40 mesh are the best mesh numbers in the ox bone active carbon of zinc chloride activation, and analysis is the reason is that because 40 active carbon now is had
Some specific surface areas are maximum, and adsorption activity is most strong.
Seven, BET is analyzed
Specific surface area is the ratio of body surface area He its quality, and international unit is m2/ g, the experiment of this measurement active carbon
Condition is to draw isothermal curve carrying out adsorption-desorption to nitrogen by under the conditions of 77K, gradually increasing relative pressure, lead to
Cross the specific surface area that object is calculated, pore size etc..Respectively to BC-2, Z-BC-3, K-BC-3, H-BC-3 activity carbon sample
Product are detected, and the results are shown in Figure 10.
Figure 10 is non-activated ox bone charcoal BC-2 (a), the active carbon K-BC-3 (b) prepared by potassium hydroxide, uses phosphoric acid
Adsorption-desorption etc. in the BET of prepared active carbon H-BC-3 (c) and the active carbon Z-BC-3 (d) prepared by zinc chloride
Warm curve.As seen from Figure 10, non-activated ox bone charcoal curve and International Union of Pure and Applied Chemistry (UIPAC) mention
IV class in adsorption isotherm classification out is similar, is a kind of isothermal curve that typical mesoporous solid generates, with opposite pressure
The raising of power, there is adsorption curve in the later period and desorption curve is inconsistent, hysteresis loop occurs.And other three living with activator
Change the ox bone active carbon early period of preparation similar to I and II in UIPAC, early period, absorption increased rapidly with the raising of pressure,
Stage is similar to IV class, hysteresis loop occurs, and can be seen that the pressure ratio that hysteresis loop occurs in the active carbon after activation and do not live
That changes is many late, and hysteresis loop area ratio is non-activated wants small, illustrates, the ox bone active carbon central hole structure after activation is few, micro-
Pore structure is more.On the other hand, ox bone activated carbon adsorption-desorption isotherm after as can be seen from the figure activating is unactivated
Above ox bone charcoal, the adsorbance of the ox bone active carbon ox bone charcoal after can deducing activation is big.In addition more different activators
The ox bone active carbon of preparation, it is found that the adsorption-desorption isothermal curve highest of Z-BC-3 (Figure 10 d), K-BC-3 (Figure 10 b)
Take second place, H-BC-3 (Figure 10 c) is minimum.It is inferred that ox bone adsorption effect of activated carbon in water should be most prepared by zinc chloride activation
Good, this also matches with the experimental result before us.
The active carbon specific surface area of the different activator preparations of table 3
| Activator species | Specific surface area (m2/g) | Active carbon title |
| It is unactivated | 1.087 | BC-2 |
| Zinc chloride | 105.186 | Z-BC-3 |
| Potassium hydroxide | 72.586 | K-BC-3 |
| Phosphoric acid | 57.338 | H-BC-3 |
The active carbon specific surface area data of the different activator preparations of table 3 is as shown in table 3, as can be seen from Table 3: difference activation
The specific surface area of the active carbon of agent preparation is not identical.Wherein Z-BC-3 specific surface area maximum is up to 105.186m2/ g, K-BC-
3 take second place, and are 72.586m2The minimum 57.338m of/g, H-BC-32/ g, but it is above non-activated bone black BC-2.It can be seen that living
Agent to improve bone black specific surface area be effective, and activate after specific surface area be far longer than it is unactivated.
Eight, sem analysis
Analysis and observation is carried out by macrostructure of the Schottky field emission scanning electron microscope to body surface, observation is lived
The gap structure etc. of property carbon surface.Its working principle is that: electron gun clicks through after anode accelerates by cathode generation becomes electricity
Beamlet, then nanoscale electron probe is converted by object lens and condenser, sample surfaces are bombarded, contrast picture is formed.
Using Schottky field emission scanning electron microscope FEI Sirion200 to respectively to BC-2, Z-BC-3, K-BC-
3, H-BC-3 activated carbon sample is scanned, and is observed its microstructure, as a result as shown in figure 11.
Figure 11 is non-activated ox bone charcoal BC-2 (A), the active carbon Z-BC-3 (B) prepared by zinc chloride, uses hydroxide
The SEM spectrum of active carbon K-BC-3 (C) prepared by potassium and the active carbon H-BC-3 (D) prepared by phosphoric acid.From Figure 11
It can be seen that gap structure the surface A there is no, surface is made of some biggish particulate matters, and surface is smooth flat
It is whole.B surface has apparent harsh feeling, and multiple small spaces structures are not of uniform size, and shape is different.C Surface has apparent sheet
Layering, gap is big and deep, and sheet layering shows a kind of smooth texture.D figure is it can be seen that the more lines senses in surface, show
A kind of coarse embossment sense, the gap being slightly layered.Bone black after illustrating activation is since the bone surface that acts on of activator is formed
Certain microcellular structure, the micropore that wherein zinc chloride is formed as activator is small and more, potassium hydroxide is formed as activator
Gap it is big and deep, phosphoric acid is more as activator formation texture level.
Nine, FT-IR is analyzed
By different material to infrared characteristic absorption peaks difference, the composition of qualitative analysis substance.Its working principle is that
There is the phenomenon that selective absorbing to light using test substance, the function of substance is judged according to the specific absorption peak of compound
Group, and then analysis supposition is carried out to its structure.
The structure of functional groups that front and back active carbon is activated by comparison, can more specifically understand activator in active carbon system
Whether play the role of changing functional group during standby.Figure 12 is non-activated ox bone charcoal BC-2 (A), prepared by phosphoric acid
Active carbon H-BC-3 (B), the active carbon K-BC-3 (C) and the active carbon Z- prepared by zinc chloride prepared by potassium hydroxide
The infrared spectrogram of BC-3 (D).As seen from Figure 12, with the active carbon of zinc chloride activation compared with unactivated, almost without
What newborn functional group, this has also confirmed zinc chloride and has substantially only served dehydration in activation process, and makes of phosphoric acid
The non-activated active carbon of the active carbon ratio of activator preparation, more many acidic functionalities, moisture content peak values also reduce
Very much, the peak of C=O double bond is also small much and in figure, and explanation uses phosphoric acid to will appear many acidic functionalities as activator,
And dehydration is also played in this activation process.With potassium hydroxide do activator active carbon and it is unactivated before phase
Than being then more C-O key, preliminary analysis is considered many basic functionalities, it may be possible to the classes such as alcoholic extract hydroxyl group.
In addition, whether the functional group before and after the activated carbon adsorption methylene blue for passing through each different activator activation of comparison is sent out
Changing observes the principle of activated carbon adsorption methylene blue.As a result as illustrated in figs. 13-15.
Figure 13-15 is the absorption front and back infrared spectroscopy that active carbon is prepared using zinc chloride, phosphoric acid, activation of potassium hydroxide respectively
Figure is found by comparison zinc chloride (Figure 13) and phosphoric acid (Figure 14) absorption front and back functional group's situation of change, in both kind activation
Agent functional group before and after absorption changes significantly, and the functional groups such as more C ≡ N, C-N.Illustrate that both active carbons are being inhaled
Not only hole plays suction-operated when attached methylene blue, and in hole suction-operated, there are also the generations of chemical reaction.
By two curves in Figure 15 it can be found that the functional group of potassium hydroxide absorption front and back active carbon does not occur significant change substantially,
Illustrating it is largely that hole is playing suction-operated when potassium hydroxide adsorbs methylene blue, chemical reaction is less, this
Why theoretically equally confirmed, which can prepare ox bone active carbon prepared by the activator (potassium hydroxide) of high-specific surface area, exists
There are no the active carbon effect of zinc chloride activation is good for effect when adsorbing methylene blue.On the one hand analyzing reason is to prepare item
On the other hand the reason of part causes is that aqueous solution of methylene blue itself shows alkalinity, cause with H-BC-3 surface functional group not
It can be chemically reacted with methylene blue solution.
The above content is just an example and description of the concept of the present invention, affiliated those skilled in the art
It makes various modifications or additions to the described embodiments or is substituted in a similar manner, without departing from hair
Bright design or beyond the scope defined by this claim, is within the scope of protection of the invention.
Claims (9)
1. a kind of preparation method of ox bone active carbon, which is characterized in that steps are as follows:
1. ox bone pre-processes
The substances such as remaining meat on ox bone are removed with scalpel, ox bone is sawed-off at fritter, remove internal marrow, flowing water punching
Wash clean, after be placed in baking oven it is dry；
2. the coarse crushing of ox bone
Pretreated ox bone is hammered into shape repeatedly and is pounded to fragment；
3. the degreasing of ox bone
Suitable water is added in ox bone fragment after coarse crushing, and boiling carries out degreasing repeatedly, until swimming in water-gage without grease
Layer, the ox bone after degreasing are dried after cleaning up；
4. ox bone is finely divided
It is finely divided to the ox bone progress after degreaser drying, cross 40-100 mesh；
5. charing prepares ox bone charcoal
Ox bone powder is put into vacuum tube furnace, heating charing, then cooling is ox bone charcoal；
6. the activation of ox bone charcoal
Impregnation is carried out to ox bone charcoal using activator, is successively dried after dipping, vacuum tube furnace high temperature is lived
Change；
7. pickling, washing
Pickling is carried out with the ox bone active carbon that hydrochloric acid completes preparation, then washes, is dry.
2. preparation method as described in claim 1, which is characterized in that 5. middle carburizing temperature is 400 DEG C to step, and carbonization time is
2h, heating rate are 10 DEG C/min, natural cooling after charing.
3. preparation method as described in claim 1, which is characterized in that step 6. in activator be zinc chloride, potassium hydroxide
Or phosphoric acid, dip time 12h.
4. preparation method as claimed in claim 3, which is characterized in that step 6. employed in liquor zinci chloridi quality point
Number is 40%, and potassium hydroxide solution concentration is 1g/L, and the mass fraction of phosphoric acid is 70%；Liquor zinci chloridi, potassium hydroxide solution
Additive amount be activator that every 1mg ox bone charcoal adds 2mL, the additive amount of phosphoric acid is the activation that every 1mg ox bone charcoal adds 3mL
Agent.
5. preparation method as described in claim 1, which is characterized in that 6. step after middle dipping, is dipped into object and is placed in
12h is dried in baking oven at 105 DEG C.
6. preparation method as described in claim 1, which is characterized in that step 6. in by after drying by the ox bone charcoal of dipping
It being placed again into vacuum tube furnace, is passed through nitrogen, be warming up to 400 DEG C with the speed of 10 DEG C/min, constant temperature 90min is activated,
Sample is taken out when it is naturally cooling to 80 DEG C.
7. preparation method as described in claim 1, which is characterized in that step 7. in be added in ox bone active carbon it is suitable
In 0.1mol/L hydrochloric acid solution, it is heated to boiling 20min.
8. preparation method as claimed in claim 1 or 7, which is characterized in that step 7. in it is pure with 70-80 DEG C after pickling
Water repeated flushing, in 6-7, then will be put into baking oven to pH after sample filtering, dry under the conditions of 105 DEG C to constant weight.
9. a kind of ox bone active carbon such as any one of claim 1-8 the method preparation is adsorbing answering in organic pollutant
With.
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