CN103316632A - Bamboo reed biocarbon, preparation method, and method for strengthening ammonia-nitrogen absorbing ability - Google Patents
Bamboo reed biocarbon, preparation method, and method for strengthening ammonia-nitrogen absorbing ability Download PDFInfo
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- CN103316632A CN103316632A CN2013102184541A CN201310218454A CN103316632A CN 103316632 A CN103316632 A CN 103316632A CN 2013102184541 A CN2013102184541 A CN 2013102184541A CN 201310218454 A CN201310218454 A CN 201310218454A CN 103316632 A CN103316632 A CN 103316632A
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- 241001494508 Arundo donax Species 0.000 title claims abstract description 95
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 17
- 238000005728 strengthening Methods 0.000 title claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000002994 raw material Substances 0.000 claims abstract description 5
- 230000007935 neutral effect Effects 0.000 claims abstract description 4
- 239000012299 nitrogen atmosphere Substances 0.000 claims abstract description 4
- 235000014676 Phragmites communis Nutrition 0.000 claims description 86
- 239000003610 charcoal Substances 0.000 claims description 78
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical group [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 45
- 238000010521 absorption reaction Methods 0.000 claims description 14
- 238000000197 pyrolysis Methods 0.000 claims description 14
- 239000000376 reactant Substances 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 239000008367 deionised water Substances 0.000 claims description 3
- 229910021641 deionized water Inorganic materials 0.000 claims description 3
- 238000007598 dipping method Methods 0.000 claims description 3
- 238000001035 drying Methods 0.000 claims description 3
- 239000000463 material Substances 0.000 claims description 3
- 238000002203 pretreatment Methods 0.000 abstract description 8
- 239000010902 straw Substances 0.000 abstract description 8
- 239000002689 soil Substances 0.000 abstract description 4
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract description 2
- 229910052760 oxygen Inorganic materials 0.000 abstract description 2
- 239000001301 oxygen Substances 0.000 abstract description 2
- 239000002699 waste material Substances 0.000 abstract description 2
- 239000003513 alkali Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 13
- 238000001179 sorption measurement Methods 0.000 description 6
- 230000003647 oxidation Effects 0.000 description 5
- 238000007254 oxidation reaction Methods 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000005070 sampling Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- 238000004458 analytical method Methods 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 230000001105 regulatory effect Effects 0.000 description 3
- 238000002441 X-ray diffraction Methods 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 238000005899 aromatization reaction Methods 0.000 description 1
- 239000012620 biological material Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000003306 harvesting Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 229910001410 inorganic ion Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 150000002894 organic compounds Chemical class 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 239000012265 solid product Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
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- Disinfection, Sterilisation Or Deodorisation Of Air (AREA)
Abstract
The invention discloses a bamboo reed biocarbon, a preparation method, and a method for strengthening ammonia-nitrogen absorbing ability. Bamboo reed straws are cut and dried, and then added into and dipped in a mild alkali reaction solution for a pre-treatment. The straws after pre-treatment are washed by water to become neutral and then dried. Then the straws are thermally decomposed in the absence of oxygen to produce bamboo reed biocarbon at the nitrogen atmosphere. The bamboo reed biocarbon is grinded and sieved, and then subjected to a water process to strengthen ammonia-nitrogen absorbing ability. The biocarbon produced by the method has a larger specific surface area and a larger hole diameter, therefore the absorbing ability of the biocarbon is improved. The method of preparing bamboo reed biology charcoals adopts bamboo reed straws as the raw materials, not only solves the problem of disposal and treatment of harvested bamboo reed straws, but also produces biocarbon to repair polluted water and soil, and changes waste materials into valuable things.
Description
Technical field
The present invention relates to the improvement of water pollution control technology, specifically refer to the preparation method of a kind of giantreed charcoal, this giantreed charcoal and the method that this giantreed charcoal is used for strengthening ammonia nitrogen absorption, belong to water treatment field.
Background technology
Charcoal is the solid product that biological material forms through high temperature pyrolysis under anaerobism or anoxic oxygen condition, has highly developed pore structure and more surface negative charge, can effectively adsorb inorganic ions in fixedly water, soil or the deposit (such as Cu
2+, Pb
2+, Hg
2+And NH
4 +Deng) and organic compound.Simultaneously, the height aromatization structure of charcoal makes it have higher biology, chemistry and heat endurance, has very large application potential aspect water body reparation and the soil improvement.But the effect of charcoal in water treatment that present technology of preparing obtains is limited, is difficult to give full play to its potential and advantage.
Giantreed is a kind of plant commonly used for the Wetland ecological reparation, and still along with the long-play of wetland, effective removal of pollutant need to realize by the periodical reaping giantreed.For a long time, owing to lacking effective application technology as the second resource, giantreed stalk majority can not in time be utilized harvested giantreed stalk by direct returning to farmland or burning, and environment is caused secondary pollution, also causes the wasting of resources simultaneously.Therefore, how harvested giantreed stalk being carried out recycling, is the problem that the needs of pendulum in face of those skilled in the art solve.
Summary of the invention
For the deficiency of traditional biological charcoal on the water treatment effect, the purpose of this invention is to provide the preparation method of a kind of giantreed charcoal, this giantreed charcoal and the method that this giantreed charcoal is used for strengthening ammonia nitrogen absorption, this giantreed charcoal and method can improve the ammonia nitrogen absorption performance greatly.
The present invention realizes that the technical solution of above-mentioned purpose is as follows:
A kind of preparation method of giantreed charcoal carries out as follows,
(1) raw material preparation: the giantreed stalk is cleaned, prescinded to 4 ~ 5cm dry for standby;
(2) giantreed stalk preliminary treatment: the giantreed stalk that (1) step was obtained adds dipping pretreatment in the irenine reactant liquor, and the irenine reactant liquor is NaOH and H
2O
2The mixed aqueous solution that forms, wherein the NaOH mass fraction is 0.25～2%, H
2O
2Mass fraction is 0.14～1.01 %, and surplus is water; Pretreatment parameter is: 40～80 ℃ of temperature, and solid-to-liquid ratio (g/mL) 1:30～1:10, processing time 4h～32h washes with water to neutral post-drying giantreed stalk after pretreatment for subsequent use;
(3) with the pyrogenically prepared giantreed charcoal of (2) step pretreated giantreed stalk anoxybiotic under nitrogen atmosphere, wherein pyrolysis temperature is 400 ~ 800 ℃, and pyrolysis time is 1.5 ~ 2.5h;
(4) the giantreed charcoal of (3) step preparation is put into pulverizer broken, sieve, get 80 ~ 40 purpose giantreed charcoals as sorbing material, wash so that the pH value of giantreed charcoal is reduced to 7.5 ~ 8 with deionized water, because freshly prepd charcoal is alkalescence, pH is about 10 ~ 11, and washing is to be reduced to 7.5 ~ 8 for the pH that makes charcoal,, put into afterwards the baking oven oven dry and namely prepare final giantreed charcoal finished product with ammonia state volatilization effusion to prevent ammonia nitrogen.
Further, during described (2) step giantreed stalk preliminary treatment, the preferred 1-1.5% of NaOH mass fraction in the irenine reactant liquor, H
2O
2The preferred 0.3-0.6% of mass fraction; The preferred 55-70 of pretreatment temperature ℃, the preferred 1:15-25 of solid-to-liquid ratio (g/ml), the preferred 15-28h of pretreatment time.
Giantreed charcoal of the present invention is namely prepared by said method.
The giantreed charcoal of as stated above preparation added to strengthen ammonia nitrogen absorption in the pending water and process.
The present invention is by carrying out the irenine oxidation pre-treatment to the giantreed stalk before the pyrolysis charring, itself superpower lignocellulosic crystal structure is destroyed, the element that has changed charcoal forms, by contrast through and do not have the scanning electron microscope (SEM) photograph of two kinds of charcoals that the giantreed stalk through the irenine oxidation pre-treatment obtains the analysis showed that: the skeleton structure that makes charcoal occurs obviously to cave in without the charcoal of preliminary treatment preparation, and specific area and aperture increase; The element of analyzing two kinds of charcoals forms: the C of giantreed charcoal after pretreatment, H, N content all reduce, and O content increases, and the ratio of H/C, (C+H)/O reduces, (O+N)/and the ratio of C increases.These can show: charcoal armaticity grow, the degree of polymerization for preparing after the irenine oxidation pre-treatment uprises, reproducibility weakens, surface polarity increases, these all are conducive to the increase of charcoal adsorbance, improved the absorption property of charcoal, also the way it goes for experiment confirm.
The present invention is prepared into charcoal take the giantreed stalk as raw material, has both solved disposal, processing problem behind the wetland plant giantreed straw harvesting, also can be used for repairing contaminated water body and soil, turns waste into wealth.
Description of drawings
Fig. 1-without preliminary treatment (a) with through the standby charcoal electron-microscope scanning figure of the giantreed straw of irenine preliminary treatment (b).
Fig. 2-the absorption property of ammonia nitrogen is tested comparison chart without preliminary treatment with through the standby charcoal of the pretreated giantreed straw of irenine.
The specific embodiment
Below in conjunction with accompanying drawing the present invention is further elaborated.
The preparation method of giantreed charcoal of the present invention the steps include:
(1) raw material preparation: the giantreed stalk is cleaned, prescinded to 4 ~ 5cm dry for standby;
(2) giantreed stalk preliminary treatment: the giantreed stalk that (1) step was obtained adds dipping pretreatment in the irenine reactant liquor, and the irenine reactant liquor is NaOH and H
2O
2The mixed aqueous solution that forms, wherein the NaOH mass fraction is 0.25～2%, H
2O
2Mass fraction is 0.14～1.01 %, and surplus is water; Pretreatment parameter is: 40～80 ℃ of temperature, and solid-to-liquid ratio (g/mL) 1:30～1:10, processing time 4h～32h washes with water to neutral post-drying stalk after pretreatment for subsequent use;
(3) with the pyrogenically prepared giantreed charcoal of (2) step pretreated giantreed stalk anoxybiotic under nitrogen atmosphere, wherein pyrolysis temperature is 400 ~ 800 ℃, and pyrolysis time is 1.5 ~ 2.5h;
(4) the giantreed charcoal of preparation is put into pulverizer broken, sieve, get 80 ~ 40 purpose giantreed charcoals as sorbing material, with deionized water washing several times, because freshly prepd charcoal is alkalescence, pH is about 10 ~ 11, and washing is to be reduced to 7.5 ~ 8 for the pH that makes charcoal, with ammonia state volatilization effusion, put into afterwards the baking oven dry for standby to prevent ammonia nitrogen;
During described (2) step giantreed stalk preliminary treatment, the preferred 1-1.5% of NaOH mass fraction in the irenine reactant liquor, H
20
2The preferred 0.3-0.6% of mass fraction; The preferred 55-70 of pretreatment temperature ℃, the preferred 1:15-25 of solid-to-liquid ratio (g/ml), the preferred 15-28h of pretreatment time.More preferably, the NaOH mass fraction is preferred 1.24% in the irenine reactant liquor, H
2O
2Mass fraction preferred 0.35%; Preferred 64 ℃ of pretreatment temperature, the preferred 1:22.2 of solid-to-liquid ratio (g/ml), the preferred 26.5h of pretreatment time.The NaOH mass fraction is 1.14%, H in also can the irenine reactant liquor
2O
2Mass fraction is 0.46%; Pretreatment temperature is 55 ℃, and solid-to-liquid ratio (g/ml) is 1:18, and pretreatment time is 20h.
In described (3) step, when the giantreed stalk prepared the giantreed charcoal in pyrolysis, pyrolysis temperature was preferably 500 ℃, and pyrolysis time is preferably 2h.
The giantreed charcoal of as stated above preparation added to strengthen ammonia nitrogen absorption in the pending water and process.
For the proterties of the giantreed charcoal that the present invention prepares is described, the present invention prepares the giantreed charcoal by this method respectively, by prepare the giantreed charcoal without preprocess method, then the proterties of two kinds of giantreed charcoals is analyzed simultaneously.Above-mentioned preparation process is except having or not pre-treatment step, and other step is identical.In the pre-treatment step, the NaOH mass fraction is 1.24%, H in the irenine reactant liquor
2O
2Mass fraction is 0.35%; Pretreatment temperature is 64 ℃, and solid-to-liquid ratio (g/ml) is 1:22.2, and pretreatment time is 26.5h.
Then adopt Fourier's infrared spectrum analysis (FTIR), electron microscope scanning (SEM), X-ray diffraction analysis (XRD) that the proterties through the charcoal of preliminary treatment and the preparation of being untreated is analyzed, measure simultaneously specific area and the aperture of two kinds of charcoals.Following table is that the Elemental Composition of charcoal is analysed table.
Element forms
As above shown in the table, C, H, the N content of charcoal of preparation all reduces after pretreatment, and the content of O increases, and the ratio of H/C, (C+H)/O reduces, (O+N)/and the ratio of C increases.H/C ratio reduces the charcoal armaticity grow that explanation giantreed stalk prepares after pretreatment, and the degree of polymerization uprises; (C+H)/ reproducibility that the ratio of O reduces the explanation charcoal weakens; (O+N)/ratio of C increases explanation charcoal surface polarity to be increased.So can judge by with irenine oxidation pre-treatment giantreed stalk, the charcoal absorption property that makes is improved.
The specific area of the charcoal that the giantreed stalk makes after the irenine preliminary treatment is 821.31 m
2/ g, the aperture is 35.8 nm, and is 345.92 m without the specific area that preliminary treatment makes charcoal
2/ g, the aperture is 5.1 nm.Contrasting two kinds of charcoals amplifies 2000 times of lower SEM figure (see figure 1)s and the analysis showed that: usefulness irenine oxidation processes giantreed stalk, destroyed the superpower crystal structure of lignocellulosic, the skeleton structure of the charcoal of preparation occurs obviously to cave in without the charcoal of preliminary treatment preparation.The increase in specific area and aperture is conducive to the carrying out of adsorbing.
For further verifying the adsorption effect of the charcoal of processing rear preparation, the inventor has carried out adsorption test according to following step.
Test procedure: take by weighing through preliminary treatment and untreated each 0.5g of giantreed charcoal, join in the 250ml conical flask, add 100ml ammonia nitrogen solution, wherein select three kinds of ammonia nitrogen initial concentration: 2mmol/L, 4mmol/L, 8mmol/L, pH all are adjusted to 7.Put into constant temperature oscillator, Temperature Setting is 25 ℃, and rotating speed is 150rpm, and water sampling is measured ammonia nitrogen concentration at set intervals, calculates the adsorbance of giantreed charcoal.
The giantreed charcoal is calculated as follows the adsorbance of ammonia nitrogen among the present invention:
C in the formula
oAnd C
eBe the initial concentration of ammonia nitrogen and the concentration after the adsorption equilibrium, V is the volume (L) of ammonia nitrogen solution, and W is the quality (g) of giantreed charcoal.
Embodiment one:
Take by weighing respectively each 0.5g of giantreed charcoal through irenine processing and unprocessed preparation, respectively join in the 250ml conical flask, adding concentration is the ammonia nitrogen solution 100ml of 2mmol/L again, adopt concentration be 0.001,0.01,0.1,1.0 and HCl and the NaOH of 2.0mol/L pH value of solution is regulated, making the pH value is 7.Put into constant temperature oscillator, Temperature Setting is 25 ℃, and rotating speed is 150rpm, and water sampling is measured ammonia nitrogen concentration at set intervals, calculates the adsorbance of giantreed charcoal.Result of the test is shown in Fig. 2 a, when the ammonia nitrogen initial concentration solution is 2mmol/L, after 72h is carried out in adsorption test, two kinds of charcoals all are in poised state to the absorption of ammonia nitrogen, wherein, the adsorbance of pretreated giantreed charcoal is 0.45mg/g, and the adsorbance of undressed giantreed charcoal is 0.33mg/g.
Embodiment two:
Take by weighing respectively the giantreed charcoal 0.5g through irenine processing and unprocessed preparation, respectively join in the 250ml conical flask, adding concentration is the ammonia nitrogen solution 100ml of 4mmol/L, adopt concentration be 0.001,0.01,0.1,1.0 and HCl and the NaOH of 2.0mol/L pH value of solution is regulated, making the pH value is 7.Put into constant temperature oscillator, Temperature Setting is 25 ℃, and rotating speed is 150rpm, and water sampling is measured ammonia nitrogen concentration at set intervals, calculates the adsorbance of giantreed charcoal.Result of the test is shown in Fig. 2 b, when the ammonia nitrogen initial concentration solution is 4mmol/L, after 72h is carried out in adsorption test, two kinds of charcoals all are in poised state to the absorption of ammonia nitrogen, wherein, the adsorbance of pretreated giantreed charcoal is 0.8mg/g, and the adsorbance of undressed giantreed charcoal is 0.6mg/g.
Embodiment three:
Take by weighing respectively the giantreed charcoal 0.5g through irenine processing and unprocessed preparation, respectively join in the 250ml conical flask, adding concentration is the ammonia nitrogen solution 100ml of 8mmol/L, adopt concentration be 0.001,0.01,0.1,1.0 and HCl and the NaOH of 2.0mol/L pH value of solution is regulated, making the pH value is 7.Put into constant temperature oscillator, Temperature Setting is 25 ℃, and rotating speed is 150rpm, and water sampling is measured ammonia nitrogen concentration at set intervals, calculates the adsorbance of giantreed charcoal.Result of the test is shown in Fig. 2 c, and when the ammonia nitrogen initial concentration solution was 8mmol/L, after 72h was carried out in adsorption test, two kinds of charcoals all were in poised state to the absorption of ammonia nitrogen, and basic identical to the adsorbance of ammonia nitrogen, are about 1.1mg/g.
Explanation is at last, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although with reference to preferred embodiment the present invention is had been described in detail, those of ordinary skill in the art is to be understood that, can make amendment or be equal to replacement technical scheme of the present invention, and not breaking away from aim and the scope of technical solution of the present invention, it all should be encompassed in the middle of the claim scope of the present invention.
Claims (5)
1. the preparation method of a giantreed charcoal is characterized in that: carries out as follows,
(1) raw material preparation: the giantreed stalk is cleaned, prescinded to 4 ~ 5cm dry for standby;
(2) giantreed stalk preliminary treatment: the giantreed stalk that (1) step was obtained adds dipping pretreatment in the irenine reactant liquor, and the irenine reactant liquor is NaOH and H
2O
2The mixed aqueous solution that forms, wherein the NaOH mass fraction is 0.25～2%, H
2O
2Mass fraction is 0.14～1.01 %, and surplus is water; Pretreatment parameter is: 40～80 ℃ of temperature, and solid-to-liquid ratio (g/mL) 1:30～1:10, processing time 4h～32h washes with water to neutral post-drying giantreed stalk after pretreatment for subsequent use;
(3) with the pyrogenically prepared giantreed charcoal of (2) step pretreated giantreed stalk anoxybiotic under nitrogen atmosphere, wherein pyrolysis temperature is 400 ~ 800 ℃, and pyrolysis time is 1.5 ~ 2.5h;
(4) the giantreed charcoal of (3) step preparation is put into pulverizer broken, sieve, get 80 ~ 40 purpose giantreed charcoals as sorbing material,, put into afterwards the baking oven oven dry and namely prepare final giantreed charcoal finished product so that the pH value of giantreed charcoal is reduced to 7.5 ~ 8 with the deionized water washing.
2. the preparation method of giantreed charcoal according to claim 1 is characterized in that: during described (2) step giantreed stalk preliminary treatment, and the preferred 1-1.5% of NaOH mass fraction in the irenine reactant liquor, H
20
2The preferred 0.3-0.6% of mass fraction; The preferred 55-70 of pretreatment temperature ℃, the preferred 1:15-25 of solid-to-liquid ratio (g/ml), the preferred 15-28h of pretreatment time.
3. the preparation method of giantreed charcoal according to claim 1 is characterized in that: when described (3) step, the pyrolysis of giantreed stalk prepared the giantreed charcoal, pyrolysis temperature was preferably 500 ℃, and pyrolysis time is preferably 2h.
4. a giantreed charcoal is characterized in that: prepare by claim 1 or 2 or 3 described methods.
5. a method of strengthening giantreed charcoal absorption ammonia nitrogen is characterized in that: giantreed charcoal claimed in claim 4 is added can strengthen the ammonia nitrogen absorption processing in the pending water.
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