CN115672285A - Biomass adsorbent and preparation method thereof - Google Patents
Biomass adsorbent and preparation method thereof Download PDFInfo
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- CN115672285A CN115672285A CN202211406880.3A CN202211406880A CN115672285A CN 115672285 A CN115672285 A CN 115672285A CN 202211406880 A CN202211406880 A CN 202211406880A CN 115672285 A CN115672285 A CN 115672285A
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- deionized water
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- 239000002028 Biomass Substances 0.000 title claims abstract description 117
- 239000003463 adsorbent Substances 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 235000011114 ammonium hydroxide Nutrition 0.000 claims abstract description 52
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 51
- 239000008367 deionised water Substances 0.000 claims abstract description 37
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 37
- 239000000843 powder Substances 0.000 claims abstract description 37
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 23
- 238000000967 suction filtration Methods 0.000 claims abstract description 20
- 238000000926 separation method Methods 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 14
- 229910021645 metal ion Inorganic materials 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000007598 dipping method Methods 0.000 claims abstract description 10
- 229910052751 metal Inorganic materials 0.000 claims abstract description 10
- 239000002184 metal Substances 0.000 claims abstract description 10
- 150000003863 ammonium salts Chemical class 0.000 claims abstract description 7
- 239000012266 salt solution Substances 0.000 claims abstract description 7
- NLXLAEXVIDQMFP-UHFFFAOYSA-N Ammonium chloride Substances [NH4+].[Cl-] NLXLAEXVIDQMFP-UHFFFAOYSA-N 0.000 claims description 29
- 239000010902 straw Substances 0.000 claims description 26
- 239000012535 impurity Substances 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 10
- PLKATZNSTYDYJW-UHFFFAOYSA-N azane silver Chemical compound N.[Ag] PLKATZNSTYDYJW-UHFFFAOYSA-N 0.000 claims description 7
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 7
- QYTBWVFCSVDTEC-UHFFFAOYSA-N azane;iron Chemical compound N.[Fe] QYTBWVFCSVDTEC-UHFFFAOYSA-N 0.000 claims description 6
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 6
- ONDPHDOFVYQSGI-UHFFFAOYSA-N zinc nitrate Chemical compound [Zn+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O ONDPHDOFVYQSGI-UHFFFAOYSA-N 0.000 claims description 6
- 229910002651 NO3 Inorganic materials 0.000 claims description 5
- NHNBFGGVMKEFGY-UHFFFAOYSA-N Nitrate Chemical compound [O-][N+]([O-])=O NHNBFGGVMKEFGY-UHFFFAOYSA-N 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 5
- 241000196324 Embryophyta Species 0.000 claims description 4
- NBFQLHGCEMEQFN-UHFFFAOYSA-N N.[Ni] Chemical compound N.[Ni] NBFQLHGCEMEQFN-UHFFFAOYSA-N 0.000 claims description 4
- PAIKTXYQXFUCKQ-UHFFFAOYSA-N azane mercury Chemical compound N.[Hg] PAIKTXYQXFUCKQ-UHFFFAOYSA-N 0.000 claims description 4
- 150000001875 compounds Chemical class 0.000 claims description 4
- QKSIFUGZHOUETI-UHFFFAOYSA-N copper;azane Chemical compound N.N.N.N.[Cu+2] QKSIFUGZHOUETI-UHFFFAOYSA-N 0.000 claims description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims description 3
- 229910021380 Manganese Chloride Inorganic materials 0.000 claims description 3
- GLFNIEUTAYBVOC-UHFFFAOYSA-L Manganese chloride Chemical compound Cl[Mn]Cl GLFNIEUTAYBVOC-UHFFFAOYSA-L 0.000 claims description 3
- 229910021607 Silver chloride Inorganic materials 0.000 claims description 3
- LJAOOBNHPFKCDR-UHFFFAOYSA-K chromium(3+) trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].[Cl-].[Cl-].[Cr+3] LJAOOBNHPFKCDR-UHFFFAOYSA-K 0.000 claims description 3
- 229940044175 cobalt sulfate Drugs 0.000 claims description 3
- 229910000361 cobalt sulfate Inorganic materials 0.000 claims description 3
- KTVIXTQDYHMGHF-UHFFFAOYSA-L cobalt(2+) sulfate Chemical compound [Co+2].[O-]S([O-])(=O)=O KTVIXTQDYHMGHF-UHFFFAOYSA-L 0.000 claims description 3
- RUTXIHLAWFEWGM-UHFFFAOYSA-H iron(3+) sulfate Chemical compound [Fe+3].[Fe+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O RUTXIHLAWFEWGM-UHFFFAOYSA-H 0.000 claims description 3
- 229910000360 iron(III) sulfate Inorganic materials 0.000 claims description 3
- 229940099607 manganese chloride Drugs 0.000 claims description 3
- 235000002867 manganese chloride Nutrition 0.000 claims description 3
- 239000011565 manganese chloride Substances 0.000 claims description 3
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 3
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 3
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 claims description 3
- 150000003841 chloride salts Chemical class 0.000 claims description 2
- RCTYPNKXASFOBE-UHFFFAOYSA-M chloromercury Chemical compound [Hg]Cl RCTYPNKXASFOBE-UHFFFAOYSA-M 0.000 claims description 2
- 235000013399 edible fruits Nutrition 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 claims description 2
- MYSWGUAQZAJSOK-UHFFFAOYSA-N ciprofloxacin Chemical compound C12=CC(N3CCNCC3)=C(F)C=C2C(=O)C(C(=O)O)=CN1C1CC1 MYSWGUAQZAJSOK-UHFFFAOYSA-N 0.000 abstract description 18
- 238000001179 sorption measurement Methods 0.000 abstract description 14
- 229960001180 norfloxacin Drugs 0.000 abstract description 10
- OGJPXUAPXNRGGI-UHFFFAOYSA-N norfloxacin Chemical compound C1=C2N(CC)C=C(C(O)=O)C(=O)C2=CC(F)=C1N1CCNCC1 OGJPXUAPXNRGGI-UHFFFAOYSA-N 0.000 abstract description 10
- 229960003405 ciprofloxacin Drugs 0.000 abstract description 9
- 229960004236 pefloxacin Drugs 0.000 abstract description 9
- FHFYDNQZQSQIAI-UHFFFAOYSA-N pefloxacin Chemical compound C1=C2N(CC)C=C(C(O)=O)C(=O)C2=CC(F)=C1N1CCN(C)CC1 FHFYDNQZQSQIAI-UHFFFAOYSA-N 0.000 abstract description 9
- 239000003242 anti bacterial agent Substances 0.000 abstract description 5
- 229940088710 antibiotic agent Drugs 0.000 abstract description 5
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 abstract description 3
- 238000004064 recycling Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 19
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 12
- -1 silver ions Chemical class 0.000 description 10
- 240000008042 Zea mays Species 0.000 description 9
- 235000005824 Zea mays ssp. parviglumis Nutrition 0.000 description 9
- 235000002017 Zea mays subsp mays Nutrition 0.000 description 9
- 235000005822 corn Nutrition 0.000 description 9
- 244000068988 Glycine max Species 0.000 description 7
- 235000010469 Glycine max Nutrition 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 229920000742 Cotton Polymers 0.000 description 5
- 241000219000 Populus Species 0.000 description 5
- 238000001914 filtration Methods 0.000 description 5
- 241000209140 Triticum Species 0.000 description 4
- 235000021307 Triticum Nutrition 0.000 description 4
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 229910052742 iron Inorganic materials 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 229910052709 silver Inorganic materials 0.000 description 4
- 239000004332 silver Substances 0.000 description 4
- 235000017060 Arachis glabrata Nutrition 0.000 description 3
- 244000105624 Arachis hypogaea Species 0.000 description 3
- 235000010777 Arachis hypogaea Nutrition 0.000 description 3
- 235000018262 Arachis monticola Nutrition 0.000 description 3
- 240000007594 Oryza sativa Species 0.000 description 3
- 235000007164 Oryza sativa Nutrition 0.000 description 3
- 235000008331 Pinus X rigitaeda Nutrition 0.000 description 3
- 235000011613 Pinus brutia Nutrition 0.000 description 3
- 241000018646 Pinus brutia Species 0.000 description 3
- 241000124033 Salix Species 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 235000020232 peanut Nutrition 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 230000035484 reaction time Effects 0.000 description 3
- 235000009566 rice Nutrition 0.000 description 3
- 238000002791 soaking Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 2
- 241001465754 Metazoa Species 0.000 description 2
- VEQPNABPJHWNSG-UHFFFAOYSA-N Nickel(2+) Chemical compound [Ni+2] VEQPNABPJHWNSG-UHFFFAOYSA-N 0.000 description 2
- 241001251949 Xanthium sibiricum Species 0.000 description 2
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 2
- 229940124350 antibacterial drug Drugs 0.000 description 2
- WRWZNPYXEXPBAY-UHFFFAOYSA-N azane cobalt Chemical compound N.[Co] WRWZNPYXEXPBAY-UHFFFAOYSA-N 0.000 description 2
- ZRUWFKRETRELPY-UHFFFAOYSA-N azane;nickel(2+) Chemical compound N.[Ni+2] ZRUWFKRETRELPY-UHFFFAOYSA-N 0.000 description 2
- IWLXWEWGQZEKGZ-UHFFFAOYSA-N azane;zinc Chemical compound N.[Zn] IWLXWEWGQZEKGZ-UHFFFAOYSA-N 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 229910001429 cobalt ion Inorganic materials 0.000 description 2
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 2
- 229910001431 copper ion Inorganic materials 0.000 description 2
- 239000003814 drug Substances 0.000 description 2
- 229910001437 manganese ion Inorganic materials 0.000 description 2
- 229910052753 mercury Inorganic materials 0.000 description 2
- 229910001453 nickel ion Inorganic materials 0.000 description 2
- 208000031295 Animal disease Diseases 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- 206010059866 Drug resistance Diseases 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 241001506766 Xanthium Species 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 125000003277 amino group Chemical group 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 238000009395 breeding Methods 0.000 description 1
- 230000001488 breeding effect Effects 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 229910001430 chromium ion Inorganic materials 0.000 description 1
- 239000000356 contaminant Substances 0.000 description 1
- 230000006806 disease prevention Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 229940124307 fluoroquinolone Drugs 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000001727 in vivo Methods 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 229960002523 mercuric chloride Drugs 0.000 description 1
- LWJROJCJINYWOX-UHFFFAOYSA-L mercury dichloride Chemical compound Cl[Hg]Cl LWJROJCJINYWOX-UHFFFAOYSA-L 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 230000004660 morphological change Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000002957 persistent organic pollutant Substances 0.000 description 1
- 238000007781 pre-processing Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000010907 stover Substances 0.000 description 1
- 229960000278 theophylline Drugs 0.000 description 1
- ZFXYFBGIUFBOJW-UHFFFAOYSA-N theophylline Chemical compound O=C1N(C)C(=O)N(C)C2=C1NC=N2 ZFXYFBGIUFBOJW-UHFFFAOYSA-N 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
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- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention belongs to the technical field of biomass recycling, and particularly relates to a biomass adsorbent and a preparation method thereof. The preparation method comprises the following steps: (1) Uniformly mixing the pretreated biomass with metal ions, deionized water and ammonia water, and dipping for 3-4h at the speed of 20-30r/min while stirring to obtain modified biomass; (2) And carrying out suction filtration separation and drying on the modified biomass and the metal ammonium salt solution to obtain the biomass adsorbent powder loaded with metal ions. The invention can have excellent adsorption performance on amino antibiotics such as pefloxacin, ciprofloxacin, norfloxacin and the like and other amino organic matters.
Description
Technical Field
The invention belongs to the technical field of biomass recycling, and particularly relates to a biomass adsorbent and a preparation method thereof.
Background
A large amount of organic pollutants containing amino groups have strong toxicity and influence on an ecosystem in a form of reducing dissolved oxygen in a water body, and are harmful to human health. The sarcin antibiotics are representative amino-containing organic matters, are synthetic third-generation fluoroquinolone antibacterial drugs, are one of the antibacterial drugs abroad, have large use amount, are widely applied to human medicine and animal disease prevention due to small side effect, short action time, wide antibacterial spectrum and low drug resistance, and are also widely applied to fishery and animal husbandry, so the antibiotic pollutants mainly exist in waste water generated in pharmacy, medicine, breeding and the like. In reality, only a small part of antibiotics applied in the prior art is absorbed by animals, most of the antibiotics are metabolized in vivo, and then enter the environment along with excrement in an original form and remain in the water body environment, which seriously threatens the safety of the ecological environment.
Disclosure of Invention
The invention aims to provide a biomass adsorbent capable of effectively adsorbing antibiotics and a preparation method thereof.
A preparation method of a biomass adsorbent comprises the following steps: (1) Uniformly mixing the pretreated biomass with metal ions, deionized water and ammonia water, and dipping for 3-4h at the speed of 20-30r/min while stirring to obtain modified biomass; (2) And carrying out suction filtration separation and drying on the modified biomass and the metal ammonium salt solution to obtain the biomass adsorbent powder loaded with metal ions.
The preparation method of the biomass adsorbent comprises the following steps of (1) pretreating biomass: the biomass crushed into 80-120 meshes is put in a water bath at 70-80 ℃ for 3-4h to remove soluble impurities, the biomass powder is separated from deionized water by suction filtration, the separation is repeated for a plurality of times until the soluble impurities are completely dissolved, and then the biomass is dried in an oven at 90-100 ℃ for 20-24 h to constant weight.
Further, the metal ions are obtained from a compound containing metal source ions, and the compound is any one of chloride, nitrate and sulfate.
Further, the metal ammonium salt solution is any one of a silver ammonia solution, a copper ammonia solution, a nickel ammonia solution, an iron ammonia solution and a mercury ammonia solution.
Further, the mass volume ratio of the pretreated biomass to the metal ions, the deionized water and the ammonia water is 4-6g:0.2-0.4g:180-220mL:8-12ml.
Furthermore, the biomass is prepared from any one of straws, branches, plant fruits or stems and plant seedlings.
Further, the chloride salt is any one of silver chloride, mercury chloride, chromium chloride hexahydrate or manganese chloride; the nitrate is any one of ferric nitrate, cupric nitrate or zinc nitrate; the sulfate is any one of cobalt sulfate, nickel sulfate or ferric sulfate.
Further, the concentration of the metal ammonium salt solution is 2000-3000ppm.
A biomass adsorbent powder loaded with metal ions prepared by the preparation method.
The preparation method provided by the invention has the advantages that the waste biomass is used as a raw material, nitrate or sulfate or chloride and the like are used as metal sources, the waste biomass is modified, the waste biomass can be recycled, and the environmental pollution is reduced.
Drawings
FIG. 1 is an electron microscope scan of biomass and untreated corn stover made according to example 1 of the present invention;
FIG. 2 is a graph showing the adsorption effect of ciprofloxacin on biomass prepared in example 1 of the present invention and commercial activated carbon;
FIG. 3 is a graph showing the adsorption effect of the biomass prepared in example 2 and commercial activated carbon on norfloxacin;
FIG. 4 is a graph showing the adsorption effect of the biomass prepared in example 3 and commercial activated carbon on pefloxacin.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1:
a preparation method of a biomass adsorbent is prepared by the following steps: (1) Uniformly mixing the pretreated corn straws with silver chloride, deionized water and ammonia water, and dipping for 3 hours at the speed of 20r/min while stirring to obtain modified biomass; (2) And carrying out suction filtration separation and drying on the modified biomass and the silver-ammonia solution to obtain the biomass adsorbent powder loaded with silver ions. The mass volume ratio of the pretreated corn straws to silver ions, deionized water and ammonia water is 4g:0.2g:180mL:8ml. The concentration of the silver ammonia solution is 2000ppm.
The pretreatment of the corn straws in the step (1) comprises the following steps: and (3) removing soluble impurities from the corn straws crushed into 80 meshes in a water bath at 70 ℃ for 3h, performing suction filtration to separate the corn straw powder from deionized water, repeating the operation for several times until the soluble impurities are completely dissolved, and then drying the corn straws in an oven at 90 ℃ for 20h to constant weight.
Example 2:
a preparation method of a biomass adsorbent comprises the following steps: (1) Uniformly mixing the pretreated cotton straw with ferric nitrate, deionized water and ammonia water, and dipping for 3-4h at the speed of 25r/min while stirring to obtain modified biomass; (2) And carrying out suction filtration separation and drying on the modified biomass and the iron ammonia solution to obtain the biomass adsorbent powder loaded with iron ions. The mass volume ratio of the cotton straw to the iron ions, the deionized water and the ammonia water after pretreatment is 5g:0.3g:200mL of: 10ml. The concentration of the iron ammonia solution is 2500ppm.
The step (1) of cotton straw pretreatment comprises the following steps: and (3) removing soluble impurities from the cotton straw crushed into 100 meshes in a water bath at 75 ℃ for 3.5h, filtering to separate cotton straw powder from deionized water, repeating the steps for several times until the soluble impurities are completely dissolved, and drying in an oven at 95 ℃ for 22h to constant weight.
Example 3:
a preparation method of a biomass adsorbent comprises the following steps: (1) Uniformly mixing the pretreated poplar branches with mercuric chloride, deionized water and ammonia water, and dipping for 4 hours at the speed of 30r/min while stirring to obtain modified biomass; (2) And carrying out suction filtration separation and drying on the modified biomass and the mercury ammonia solution to obtain biomass adsorbent powder loaded with mercury ions. The mass volume ratio of the pretreated poplar branches to mercury ions, deionized water and ammonia water is 6g:0.4g:220mL of: 12ml. The concentration of the mercury ammonia solution is 3000ppm.
The pretreatment of the poplar branches in the step (1) comprises the following steps: and (3) removing soluble impurities from the biomass crushed into 120 meshes in a water bath at 80 ℃ for 4h, performing suction filtration to separate poplar branch powder from deionized water, repeating the process for several times until the soluble impurities are completely dissolved, and drying the poplar branch powder in an oven at 100 ℃ for 24h to constant weight.
Example 4:
a preparation method of a biomass adsorbent is prepared by the following steps: (1) Uniformly mixing the pretreated wheat straws with chromium chloride hexahydrate, deionized water and ammonia water, and soaking for 3.2 hours at the speed of 27r/min while stirring to obtain modified biomass; (2) And carrying out suction filtration separation and drying on the modified silver ammonia solution to obtain the biomass adsorbent powder loaded with metal ion chromium. The mass volume ratio of the pretreated wheat straw to the chromium ions, the deionized water and the ammonia water is 5g:0.3g:200mL of the solution: 11ml. The concentration of the silver ammonia solution is 2200ppm.
The pretreatment of the wheat straw in the step (1) comprises the following steps: and (3) removing soluble impurities from the wheat straws crushed into 85 meshes in water bath at 77 ℃ for 3.6h, filtering to separate biomass powder from deionized water, repeating the steps for several times until the soluble impurities are completely dissolved, and drying in an oven at 98 ℃ for 21h to constant weight.
Example 5:
a preparation method of a biomass adsorbent comprises the following steps: (1) Uniformly mixing the pretreated soybean straws with copper nitrate, deionized water and ammonia water, and stirring and dipping for 4 hours at the speed of 30r/min to obtain modified biomass; (2) And carrying out suction filtration separation and drying on the modified biomass and the copper ammonia solution to obtain biomass adsorbent powder loaded with copper ions. The mass volume ratio of the pretreated soybean straw to copper ions, deionized water and ammonia water is 6g:0.4g:220mL of: 12ml. The concentration of the copper ammonia solution is 3000ppm.
The pretreatment of the soybean straws in the step (1) comprises the following steps: and (3) removing soluble impurities from the biomass crushed into 120 meshes in a water bath at 80 ℃ for 4h, performing suction filtration to separate biomass powder from deionized water, repeating the steps for several times until the soluble impurities are completely dissolved, and drying the biomass in an oven at 100 ℃ for 24h to constant weight.
Example 6:
a preparation method of a biomass adsorbent comprises the following steps: (1) Uniformly mixing the pretreated rice straws with cobalt sulfate, deionized water and ammonia water, and soaking for 3.5 hours at the speed of 22r/min while stirring to obtain modified biomass; (2) And carrying out suction filtration separation and drying on the modified biomass and the cobalt ammonia solution to obtain biomass adsorbent powder loaded with cobalt ions. The mass volume ratio of the pretreated rice straw to cobalt ions, deionized water and ammonia water is 6g:0.4g:220mL of: 12ml. The concentration of the cobalt ammonia solution is 2600ppm.
The pretreatment of the rice straws in the step (1) comprises the following steps: and (3) removing soluble impurities from the biomass crushed into 86 meshes in water bath at 76 ℃ for 3.5h, filtering to separate biomass powder from deionized water, repeating the steps for several times until the soluble impurities are completely dissolved, and drying in an oven at 100 ℃ for 24h to constant weight.
Example 7:
a preparation method of a biomass adsorbent comprises the following steps: (1) Uniformly mixing the pretreated peanut seedlings with zinc nitrate, deionized water and ammonia water, and soaking for 4 hours at the speed of 30r/min while stirring to obtain modified biomass; (2) And carrying out suction filtration separation and drying on the modified biomass and a zinc ammonia solution to obtain biomass adsorbent powder loaded with zinc ions. The mass volume ratio of the pretreated peanut seedlings to zinc ions, deionized water and ammonia water is 6g:0.4g:220mL of: 12ml. The concentration of the zinc ammonia solution is 3000ppm.
The pretreatment of the peanut seedlings in the step (1) comprises the following steps: and (3) removing soluble impurities from the biomass crushed into 120 meshes in a water bath at 80 ℃ for 4h, performing suction filtration to separate biomass powder from deionized water, repeating the steps for several times until the soluble impurities are completely dissolved, and drying the biomass in an oven at 100 ℃ for 24h to constant weight.
Example 8:
a preparation method of a biomass adsorbent comprises the following steps: (1) Uniformly mixing the pretreated and dried pine branches with manganese chloride, deionized water and ammonia water, and dipping for 3 hours at the speed of 28r/min while stirring to obtain modified biomass; (2) And carrying out suction filtration separation and drying on the modified biomass and the nickel ammonium solution to obtain the biomass adsorbent powder loaded with manganese ions. The mass volume ratio of the pretreated and dried pine branches to manganese ions, deionized water and ammonia water is 5g:0.3g:220mL of: 12ml. The concentration of the nickel ammonium solution is 2500ppm.
The step of preprocessing the dried pine branches in the step (1) is as follows: and (3) carrying out water bath on the biomass crushed into 100 meshes for 4h at 78 ℃ to remove soluble impurities, carrying out suction filtration to separate biomass powder from deionized water, repeating the steps for a plurality of times until the soluble impurities are completely dissolved, and then drying the biomass in an oven at 96 ℃ for 21h to constant weight.
Example 9:
a preparation method of a biomass adsorbent comprises the following steps: (1) Uniformly mixing the pretreated and dried willow branches with nickel sulfate, deionized water and ammonia water, and dipping for 4 hours at the speed of 28r/min while stirring to obtain modified biomass; (2) And carrying out suction filtration separation and drying on the modified biomass and the nickel-ammonia solution to obtain the biomass adsorbent powder loaded with nickel ions. The mass volume ratio of the pretreated and dried willow branches to nickel ions, deionized water and ammonia water is 6g:0.4g:220mL of: 12ml. The concentration of the nickel ammonia solution is 3000ppm.
The pretreatment of the dried willow branches in the step (1) comprises the following steps: and (3) removing soluble impurities from the biomass crushed into 110 meshes in a water bath at 75 ℃ for 4h, filtering to separate biomass powder from deionized water, repeating the steps for a plurality of times until the soluble impurities are completely dissolved, and drying in an oven at 100 ℃ for 24h to constant weight.
Example 10:
a preparation method of a biomass adsorbent is prepared by the following steps: (1) Uniformly mixing the pretreated xanthium sibiricum with ferric sulfate, deionized water and ammonia water, and dipping for 4 hours at the speed of 26r/min while stirring to obtain modified biomass; (2) And carrying out suction filtration separation and drying on the modified biomass and the iron ammonia solution to obtain the biomass adsorbent powder loaded with iron ions. The mass volume ratio of the pretreated xanthium to iron ions, deionized water and ammonia water is 4g:0.2g:180mL:8ml. The concentration of the iron ammonia solution is 2000ppm.
The pretreatment of the xanthium sibiricum in the step (1) comprises the following steps: and (3) removing soluble impurities from the biomass crushed into 120 meshes in a water bath at 80 ℃ for 4h, filtering to separate biomass powder from deionized water, repeating the steps for several times until the soluble impurities are completely dissolved, and drying in an oven at 100 ℃ for 20h to constant weight.
Test example 1:
scanning the biomass loaded with silver ions and the untreated corn stalks prepared in example 1 by using an SEM (scanning electron microscope) respectively, as shown in figure 1, the untreated corn stalks on the left side and the biomass loaded with silver ions prepared in example 1 on the right side show that the surface on the left side is smooth and flat, the whole morphology on the right side is broken, the straight grain structure and the cross grain structure of the soybean stalks are completely destroyed, and protruding particles and wrinkles appear. And a large number of volcanic holes raised on the surface of the treated soybean straw, the structure may be formed by naked partially broken fibers. The morphological changes show that the lignin and hemicellulose of the soybean straws treated by the silver ammonia solution are removed to a certain extent, and the specific surface area of the soybean straws is increased.
Test example 2:
75mg of the biomass adsorbent powder (a) prepared in example 1 and 75mg of the commercial activated carbon (b) were added to a ciprofloxacin solution, the concentration of which was 20mg/L, and the adsorption reaction was carried out by stirring at 500r/min, and the concentration of the ciprofloxacin solution was measured at 5min, 10min, 15min, 20min, 30min, 40min, 50min, 60min, 90min, and 120min, respectively, as a result, as shown in fig. 2, the horizontal axis represents the reaction time 2h of the whole adsorption process, the C on the vertical axis represents the concentration of ciprofloxacin at a certain time, the C0 represents the initial concentration of ciprofloxacin in the solution of 20mg/L, and the 1-C/C0 represents the removal rate of the target pollutant ciprofloxacin, and it can be seen from fig. 2 that the biomass adsorbent powder prepared in the present invention has better adsorption performance on the ciprofloxacin solution, and the biomass adsorbent powder prepared in the present invention has excellent adsorption performance on the ciprofloxacin solution.
Test example 3:
75mg of the biomass adsorbent powder (a) prepared in example 2 and 75mg of the commercial activated carbon (b) were added to norfloxacin solution, the concentration of the norfloxacin solution was 20mg/L, and the sample was taken at 500r/min to conduct adsorption reaction, and the concentration of the norfloxacin solution was measured at 5min, 10min, 15min, 20min, 30min, 40min, 50min, 60min, 90min and 120min, respectively, as a result, as shown in FIG. 3, the horizontal axis represents the reaction time of the whole adsorption process for 2h, the vertical axis C represents the concentration of norfloxacin at a certain time, C0 represents the initial concentration of norfloxacin in the solution of 20mg/L, and 1-C/C0 represents the removal rate of norfloxacin as a target pollutant, and it can be seen from FIG. 3 that the biomass adsorbent powder prepared in the present invention has a better adsorption effect on the norfloxacin solution, and the biomass adsorbent powder prepared in the present invention has an excellent adsorption effect on the norfloxacin solution.
Test example 3:
75mg of the biomass adsorbent powder (a) prepared in example 3 and 75mg of the commercial activated carbon (b) were added to a pefloxacin solution having a concentration of 20mg/L, and the mixture was stirred at a speed of 500r/min to carry out adsorption reaction, and the concentration of the pefloxacin solution was measured at 5min, 10min, 15min, 20min, 30min, 40min, 50min, 60min, 90min and 120min, respectively, as a result, as shown in FIG. 4, the horizontal axis represents the reaction time of the whole adsorption process for 2h, the C axis represents the concentration of pefloxacin at a certain time, C0 represents the initial concentration of pefloxacin in the solution of 20mg/L, and 1-C/C0 represents the removal rate of the target contaminant pefloxacin, and it can be seen from FIG. 4 that the biomass adsorbent powder prepared in the present invention has a better adsorbability to pefloxacin, and the biomass adsorbent powder prepared in the present invention has an excellent adsorbability to pefloxacin solution.
Claims (9)
1. The preparation method of the biomass adsorbent is characterized by comprising the following steps: (1) Uniformly mixing the pretreated biomass with metal ions, deionized water and ammonia water, and dipping for 3-4h at the speed of 20-30r/min while stirring to obtain modified biomass; (2) And carrying out suction filtration separation and drying on the modified biomass and the metal ammonium salt solution to obtain the biomass adsorbent powder loaded with metal ions.
2. The method for preparing the biomass adsorbent according to claim 1, wherein the step of pretreating the biomass in the step (1) comprises the following steps: the biomass crushed into 80-120 meshes is put in a water bath at 70-80 ℃ for 3-4h to remove soluble impurities, the biomass powder is separated from deionized water by suction filtration, the separation is repeated for a plurality of times until the soluble impurities are completely dissolved, and then the biomass is dried in an oven at 90-100 ℃ for 20-24 h to constant weight.
3. The method for preparing the biomass adsorbent according to claim 1, wherein the metal ions are obtained from a compound containing metal source ions, and the compound is any one of chloride, nitrate and sulfate.
4. The method for preparing the biomass adsorbent according to claim 1, wherein the metal ammonium salt solution is any one of silver ammonia solution, copper ammonia solution, nickel ammonia solution, iron ammonia solution and mercury ammonia solution.
5. The preparation method of the biomass adsorbent according to claim 1, wherein the mass-to-volume ratio of pretreated biomass to metal ions, deionized water and ammonia water is 4-6g:0.2-0.4g:180-220mL:8-12ml.
6. The method for preparing the biomass adsorbent according to claim 1, wherein the biomass is prepared from any one of straw, branches, plant fruits or stems, and plant seedlings.
7. The preparation method of the biomass adsorbent according to claim 1, wherein the chloride salt is any one of silver chloride, mercury chloride, chromium chloride hexahydrate and manganese chloride; the nitrate is any one of ferric nitrate, cupric nitrate or zinc nitrate; the sulfate is any one of cobalt sulfate, nickel sulfate or ferric sulfate.
8. The method for preparing the biomass adsorbent according to claim 1, wherein the concentration of the metal ammonium salt solution is 2000-3000ppm.
9. A biomass adsorbent powder loaded with metal ions, obtained by the method of any one of claims 1 to 8.
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