CN116651403A - Preparation method of humic acid modified collagen fiber material capable of efficiently capturing iodine vapor - Google Patents
Preparation method of humic acid modified collagen fiber material capable of efficiently capturing iodine vapor Download PDFInfo
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- CN116651403A CN116651403A CN202310767139.8A CN202310767139A CN116651403A CN 116651403 A CN116651403 A CN 116651403A CN 202310767139 A CN202310767139 A CN 202310767139A CN 116651403 A CN116651403 A CN 116651403A
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- humic acid
- collagen fiber
- acid modified
- iodine vapor
- humate
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- 102000008186 Collagen Human genes 0.000 title claims abstract description 98
- 108010035532 Collagen Proteins 0.000 title claims abstract description 98
- 229920001436 collagen Polymers 0.000 title claims abstract description 98
- ZCYVEMRRCGMTRW-UHFFFAOYSA-N 7553-56-2 Chemical compound [I] ZCYVEMRRCGMTRW-UHFFFAOYSA-N 0.000 title claims abstract description 79
- 229910052740 iodine Inorganic materials 0.000 title claims abstract description 79
- 239000011630 iodine Substances 0.000 title claims abstract description 79
- QJZYHAIUNVAGQP-UHFFFAOYSA-N 3-nitrobicyclo[2.2.1]hept-5-ene-2,3-dicarboxylic acid Chemical compound C1C2C=CC1C(C(=O)O)C2(C(O)=O)[N+]([O-])=O QJZYHAIUNVAGQP-UHFFFAOYSA-N 0.000 title claims abstract description 77
- 239000004021 humic acid Substances 0.000 title claims abstract description 70
- 239000002657 fibrous material Substances 0.000 title claims abstract description 44
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 239000000835 fiber Substances 0.000 claims abstract description 58
- 239000008367 deionised water Substances 0.000 claims abstract description 33
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 33
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 33
- 238000001914 filtration Methods 0.000 claims abstract description 27
- 239000000463 material Substances 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 24
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 238000005406 washing Methods 0.000 claims abstract description 11
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 10
- 239000003513 alkali Substances 0.000 claims abstract description 8
- 238000004140 cleaning Methods 0.000 claims abstract description 8
- 230000007935 neutral effect Effects 0.000 claims abstract description 7
- 238000004090 dissolution Methods 0.000 claims abstract description 5
- 239000007787 solid Substances 0.000 claims abstract description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 16
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 11
- 239000011734 sodium Substances 0.000 claims description 11
- 229910052708 sodium Inorganic materials 0.000 claims description 11
- 238000004506 ultrasonic cleaning Methods 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 6
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 5
- 241001465754 Metazoa Species 0.000 claims description 4
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- LEQAOMBKQFMDFZ-UHFFFAOYSA-N alpha-ketodiacetal Natural products O=CC=O LEQAOMBKQFMDFZ-UHFFFAOYSA-N 0.000 claims description 4
- 239000011591 potassium Substances 0.000 claims description 4
- 229910052700 potassium Inorganic materials 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 238000007796 conventional method Methods 0.000 claims description 3
- PUKLDDOGISCFCP-JSQCKWNTSA-N 21-Deoxycortisone Chemical compound C1CC2=CC(=O)CC[C@]2(C)[C@@H]2[C@@H]1[C@@H]1CC[C@@](C(=O)C)(O)[C@@]1(C)CC2=O PUKLDDOGISCFCP-JSQCKWNTSA-N 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 2
- FCYKAQOGGFGCMD-UHFFFAOYSA-N Fulvic acid Natural products O1C2=CC(O)=C(O)C(C(O)=O)=C2C(=O)C2=C1CC(C)(O)OC2 FCYKAQOGGFGCMD-UHFFFAOYSA-N 0.000 claims description 2
- UIIMBOGNXHQVGW-DEQYMQKBSA-M Sodium bicarbonate-14C Chemical compound [Na+].O[14C]([O-])=O UIIMBOGNXHQVGW-DEQYMQKBSA-M 0.000 claims description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 2
- 239000011575 calcium Substances 0.000 claims description 2
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- NVBNILSJHNPYKC-UHFFFAOYSA-L calcium 5-methylidenecyclopenta-1,3-diene-1-carboxylate Chemical compound [Ca++].[O-]C(=O)C1=CC=CC1=C.[O-]C(=O)C1=CC=CC1=C NVBNILSJHNPYKC-UHFFFAOYSA-L 0.000 claims description 2
- 239000002509 fulvic acid Substances 0.000 claims description 2
- 229940095100 fulvic acid Drugs 0.000 claims description 2
- 229940015043 glyoxal Drugs 0.000 claims description 2
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 claims description 2
- 238000005554 pickling Methods 0.000 claims description 2
- 235000011118 potassium hydroxide Nutrition 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 235000017550 sodium carbonate Nutrition 0.000 claims description 2
- 238000002791 soaking Methods 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 42
- 239000002028 Biomass Substances 0.000 abstract description 8
- 239000000243 solution Substances 0.000 description 19
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 11
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 9
- 230000002285 radioactive effect Effects 0.000 description 8
- 239000002699 waste material Substances 0.000 description 8
- 239000010985 leather Substances 0.000 description 7
- 230000000694 effects Effects 0.000 description 6
- 229940001482 sodium sulfite Drugs 0.000 description 6
- 235000010265 sodium sulphite Nutrition 0.000 description 6
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 5
- 150000001408 amides Chemical class 0.000 description 5
- 229940101006 anhydrous sodium sulfite Drugs 0.000 description 5
- 150000002466 imines Chemical group 0.000 description 5
- 150000003385 sodium Chemical class 0.000 description 5
- 239000003463 adsorbent Substances 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 4
- 238000010586 diagram Methods 0.000 description 4
- 210000002966 serum Anatomy 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000002411 thermogravimetry Methods 0.000 description 4
- 238000005303 weighing Methods 0.000 description 4
- DPXJVFZANSGRMM-UHFFFAOYSA-N acetic acid;2,3,4,5,6-pentahydroxyhexanal;sodium Chemical compound [Na].CC(O)=O.OCC(O)C(O)C(O)C(O)C=O DPXJVFZANSGRMM-UHFFFAOYSA-N 0.000 description 3
- 238000005452 bending Methods 0.000 description 3
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 3
- 239000001768 carboxy methyl cellulose Substances 0.000 description 3
- 230000006378 damage Effects 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 125000000524 functional group Chemical group 0.000 description 3
- PNDPGZBMCMUPRI-UHFFFAOYSA-N iodine Chemical compound II PNDPGZBMCMUPRI-UHFFFAOYSA-N 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 238000004064 recycling Methods 0.000 description 3
- 235000019812 sodium carboxymethyl cellulose Nutrition 0.000 description 3
- 229920001027 sodium carboxymethylcellulose Polymers 0.000 description 3
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 description 3
- 241000282414 Homo sapiens Species 0.000 description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000002715 modification method Methods 0.000 description 2
- 102000004169 proteins and genes Human genes 0.000 description 2
- 108090000623 proteins and genes Proteins 0.000 description 2
- 239000002901 radioactive waste Substances 0.000 description 2
- 238000001878 scanning electron micrograph Methods 0.000 description 2
- 238000007789 sealing Methods 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 230000004580 weight loss Effects 0.000 description 2
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- 241000282412 Homo Species 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 239000002841 Lewis acid Substances 0.000 description 1
- 208000036626 Mental retardation Diseases 0.000 description 1
- 208000024770 Thyroid neoplasm Diseases 0.000 description 1
- 229910021536 Zeolite Inorganic materials 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000004964 aerogel Substances 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 125000002723 alicyclic group Chemical group 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 238000006065 biodegradation reaction Methods 0.000 description 1
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- 125000002915 carbonyl group Chemical group [*:2]C([*:1])=O 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 101150021494 cof gene Proteins 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000013310 covalent-organic framework Substances 0.000 description 1
- 230000001186 cumulative effect Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000003337 fertilizer Substances 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
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- 150000007517 lewis acids Chemical class 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
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- 208000030159 metabolic disease Diseases 0.000 description 1
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- 229920005615 natural polymer Polymers 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- 230000037361 pathway Effects 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 229920001184 polypeptide Polymers 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 102000004196 processed proteins & peptides Human genes 0.000 description 1
- 108090000765 processed proteins & peptides Proteins 0.000 description 1
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- 125000005493 quinolyl group Chemical group 0.000 description 1
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- 230000003595 spectral effect Effects 0.000 description 1
- 239000002915 spent fuel radioactive waste Substances 0.000 description 1
- 201000002510 thyroid cancer Diseases 0.000 description 1
- 239000010457 zeolite Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D53/00—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols
- B01D53/02—Separation of gases or vapours; Recovering vapours of volatile solvents from gases; Chemical or biological purification of waste gases, e.g. engine exhaust gases, smoke, fumes, flue gases, aerosols by adsorption, e.g. preparative gas chromatography
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/30—Processes for preparing, regenerating, or reactivating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D2257/00—Components to be removed
- B01D2257/20—Halogens or halogen compounds
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4887—Residues, wastes, e.g. garbage, municipal or industrial sludges, compost, animal manure; fly-ashes
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E30/00—Energy generation of nuclear origin
- Y02E30/30—Nuclear fission reactors
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- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a preparation method of a humic acid modified collagen fiber material for efficiently capturing iodine vapor, which comprises the following steps: adding collagen fibers into deionized water, ultrasonically cleaning in an ultrasonic cleaner, washing to be neutral, filtering, and drying in an oven; crushing the cleaned collagen fibers in a crusher, adding the crushed collagen fibers into deionized water, and adding alkali to adjust the pH of the solution; washing with deionized water after ultrasonic treatment, filtering, and drying in a vacuum oven for later use; adding humate into deionized water, and performing ultrasonic dissolution to obtain humate solution; adding collagen fiber into humate solution, and placing in a constant-temperature shaking table for curing treatment; filtering the obtained material, adding the filtered solid into a cross-linking agent solution, stirring, filtering, and drying in vacuum to obtain the humic acid modified collagen fiber material for efficiently capturing iodine vapor. The material obtained by the invention has high adsorption capacity to iodine vapor, is outstanding in other biomass materials of the same type, and has rapid adsorption dynamics characteristics.
Description
Technical Field
The invention belongs to the field of environmental protection of radioactive iodine vapor adsorption in the environment, and particularly relates to a preparation method of a humic acid modified collagen fiber material for efficiently capturing iodine vapor, which belongs to the field of biomass resource recycling of waste leather materials.
Background
Along with the rapid development of the leather industry, the leather industry brings convenience to us and brings economic benefit to enterprises, and simultaneously causes pollution and harm to the environment. Animal skins are renewable animal biomass resources with the largest resource amount, and the waste amount is continuously increased along with the rapid development of industry. Therefore, the recycling of the waste leather material solves the ecological pollution problem to a certain extent. Therefore, how to develop the recovery of waste leather for secondary use in a direction beneficial to human beings is a topic of great attention of many researchers.
Studies have shown that leather waste can be converted into loose collagen fibers after simple pretreatment by conventional methods. Collagen Fiber (CF) is the most abundant renewable natural polymer material in nature, is composed of three polypeptide chains which are intertwined, contains abundant active groups such as carboxyl, amino, imine and hydroxyl, and is convenient for subsequent modification treatment by utilizing the active groups. Collagen fiber belongs to biomass resources, the material of the collagen fiber is easy to carry out biodegradation treatment, the environment is not polluted, the collagen fiber is very friendly to the ecology, and the collagen fiber is widely researched and applied.
Humic acid is an amorphous mixture of various polymers, the basic structure is aromatic ring and alicyclic ring, and the ring is connected with carboxyl, hydroxyl, carbonyl, quinolyl, phenol and other functional groups, and the functional groups can provide a plurality of different potential binding sites for grafting other materials. Based on the functional group, it can be used as agricultural chemical fertilizer and is naturally biodegraded. Humic acid has also been widely studied by many researchers.
Under the condition that fossil fuels are increasingly exhausted, nuclear energy is used as a novel clean energy source, the nuclear energy industry is rapidly developed, and the cumulative amount of nuclear power generation is steadily increased. But the nuclear energy releases radionuclides that cause environmental damage. There has therefore been an increasing focus on the proper disposal of radioactive waste. In radioactive waste, the radioactive iodine value is of concern. Wherein the method comprises the steps of 129 I half-life is longer (1.6X10) 7 Years), 131 i has a short half-life of 8 days, but has high toxicity and strong activity, and iodine can cause serious harm to the environment. It is particularly noted that long-term exposure of humans to radioactive iodine can cause mental retardation, metabolic disorders, increased probability of thyroid cancer, etc., and radioactive iodine in nature can be finally enriched in the human body through the food chain pathway, resulting in internal irradiation hazard. Thus, the separation and enrichment of radioactive iodine is of great importance for post-treatment of spent fuel. The prior adsorption materials for radioactive gaseous iodine mainly comprise porous zeolite, porous carbon materials, COFs, MOFs, aerogel and the like, have larger specific surface area, and are easy to modify adsorption sites and high adsorption capacity, so that the adsorption materials are widely studied. However, the preparation process is complex, the preparation cost is high, the stability is poor, the mass production is not easy to realize, the practical feasibility is further researched, and the practical application is limited. Therefore, there is an urgent need to find an alternative adsorbent material which can be mass-produced and has a simple process
Disclosure of Invention
It is an object of the present invention to address at least the above problems and/or disadvantages and to provide at least the advantages described below.
To achieve these objects and other advantages and in accordance with the purpose of the invention, there is provided a method for preparing a material for efficiently capturing iodine vapor by using humic acid modified collagen fibers, comprising the steps of:
step one, adding collagen fibers into deionized water, ultrasonically cleaning in an ultrasonic cleaner, then washing to be neutral, filtering, and then drying in an oven;
step two, crushing the cleaned collagen fibers in a crusher, adding the crushed collagen fibers into deionized water, and adding alkali to adjust the pH of the solution; ultrasonic cleaning with deionized water, filtering, and drying in a vacuum oven for later use;
thirdly, adding sodium humate into deionized water, and performing ultrasonic dissolution to obtain a humate solution;
step four, adding the collagen fiber obtained in the step two into a sodium humate solution, and placing the solution in a constant-temperature shaking table for curing treatment;
and step five, filtering the material obtained in the step four, adding the filtered solid into a cross-linking agent solution, stirring, filtering, and drying in vacuum to obtain the humic acid modified collagen fiber material for efficiently capturing iodine vapor.
Preferably, the collagen fiber in the first step is untreated animal skin, and the raw material is obtained by washing, softening, mercerizing, pickling, drying and the like according to a conventional method, and then crushing by a crusher.
Preferably, the ultrasonic cleaning temperature and the oven temperature in the first step are in the range of room temperature to 90 ℃, and the ultrasonic cleaning time is 5 hours.
Preferably, the alkali in the second step is one or more of potassium hydroxide, sodium bicarbonate, sodium carbonate, ammonia water and the like; adding alkali to regulate the pH value of the solution to 8-13.
Preferably, the different pH values in the second step correspond to different ultrasonic time, the pH value is 8-13, and the corresponding time is 10-5 h; and the ultrasonic time in the second step is 6h.
Preferably, in the third step, the humate includes one or more of sodium humate, potassium humate, calcium humate, fulvic acid, sodium fulvate, potassium fulvate and calcium fulvate.
Preferably, in the third step, the concentration of the humate solution is 0.001-5% by mass.
Preferably, in the fourth step, the mass percentage of the collagen fiber to the humate solution is 0.01-50: 100%;
preferably, the temperature of the constant temperature shaking table in the fourth step is 20-130 ℃.
Preferably, in the fifth step, the cross-linking agent includes, but is not limited to, one or more of formaldehyde, glyoxal, glutaraldehyde; the concentration of the cross-linking agent is 3-8%wt, and the mass-volume ratio of the solid to the cross-linking agent is 5g:40mL; and in the fifth step, the stirring time is 12h.
Preferably, in order to further improve the adsorption effect of the humic acid modified collagen fiber on iodine vapor, the modified humic acid salt is used for replacing the humate, and the modification method of the modified humic acid salt comprises the following steps:
s1, weighing 5-10 parts of anhydrous sodium sulfite according to parts by weight, and dissolving the anhydrous sodium sulfite in deionized water, wherein the mass volume ratio of the anhydrous sodium sulfite to the deionized water is 1g to 5mL; magnetically stirring and heating to 60-80 deg.c to obtain sodium sulfite solution;
s2, dropwise adding concentrated sulfuric acid into the sodium sulfite solution after the sodium sulfite solution is cooled to room temperature, wherein the volume ratio of the concentrated sulfuric acid to deionized water is 3:100; then adding 4-8 parts of humic acid, heating and stirring for 5-12 h at the rotating speed of 500-800 r/min, wherein the heating temperature is 90-105 ℃; filtering and drying to obtain sulfonated humic acid;
s3, weighing 0.5-1 part of sodium carboxymethyl cellulose powder, adding 2 parts of sulfonated humic acid into deionized water, wherein the mass volume ratio of the sulfonated humic acid to the deionized water is 1g to 10mL, adding the sodium carboxymethyl cellulose powder, heating to 45-60 ℃, stirring at a rotating speed of 160-300 r/min for 40-60 min, filtering and drying to obtain the modified humate.
The invention at least comprises the following beneficial effects:
(1) The material used in the invention is waste materials generated by leather factories, and the waste materials are recycled and processed into functional biomass fibers, so that the resource utilization rate is improved, and the problem of environmental pollution is also reduced. The cost is low, and the biomass material is safe and harmless and is easy to degrade.
(2) The humic acid has strong adsorption capacity on carboxyl, hydroxyl and other active groups, and has wide source, low cost and easy degradation. The modified collagen fiber is crosslinked on the collagen fiber, presents a form that the surface of the collagen fiber is dyed with dark brown from yellow-brown, presents high adsorption capacity to iodine vapor, is prominent in other biomass materials of the same type, and has rapid adsorption dynamics characteristics.
(3) The preparation method disclosed by the invention is simple in preparation process, easy to operate, capable of realizing large-scale preparation, safe and environment-friendly, and effectively improving the high-efficiency utilization rate of biomass and recycling waste materials.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention.
Drawings
FIG. 1 is an SEM image of the humic acid modified collagenous fiber material prepared in example 1 of the present invention after adsorbing iodine vapor;
FIG. 2 is a diagram of the humic acid modified collagen fiber material prepared in example 1 of the present invention;
fig. 3 is a physical diagram of the humic acid modified collagen fiber material prepared in example 1 of the present invention after iodine vapor is adsorbed;
FIG. 4 is a graph showing FTIR results of the humic acid modified collagen fiber material prepared in example 1, the humic acid modified collagen fiber material after iodine vapor adsorption, and the activated collagen fiber prepared in comparative example 1 according to the present invention;
FIG. 5 is a thermogravimetric analysis (TGA) of the weight loss of the humic acid modified collagen fiber material prepared in example 1 according to the present invention at different temperatures;
FIG. 6 is a graph showing the adsorption results of iodine vapor at different intervals of the humic acid modified collagen fiber material prepared in example 1 of the present invention;
FIG. 7 is a graph of the full energy X-ray photoelectron spectrum before and after adsorption of the humic acid modified collagen fiber material prepared in example 1 of the present invention;
FIG. 8 is an X-ray photoelectron spectrum of two peaks of I3d before and after adsorption of the humic acid modified collagen fiber material prepared in example 1 of the present invention;
FIG. 9 is an X-ray photoelectron spectrum of the humic acid modified collagen fiber material prepared in example 1 before and after N adsorption;
FIG. 10 is an X-ray photoelectron spectrum of the humic acid modified collagen fiber material O prepared in example 1 of the present invention before and after adsorption;
FIG. 11 is a graph showing the adsorption results of iodine vapor at different intervals of the humic acid modified collagenous fiber material prepared in example 1 and example 2 of the present invention;
FIG. 12 is a graph showing the adsorption results of iodine vapor at 75℃for the different modified collagen fiber materials prepared in example 1, comparative example 1 and comparative example 2.
Detailed Description
The present invention is described in further detail below with reference to the drawings to enable those skilled in the art to practice the invention by referring to the description.
It will be understood that terms, such as "having," "including," and "comprising," as used herein, do not preclude the presence or addition of one or more other elements or groups thereof.
Example 1:
a preparation method of a humic acid modified collagen fiber material for efficiently capturing iodine vapor comprises the following steps:
firstly, adding 50g of collagen fibers into deionized water, ultrasonically cleaning for 5 hours in an ultrasonic cleaning machine, washing to be neutral, filtering, and drying in an oven;
step two, crushing the cleaned collagen fibers by a crusher, adding the crushed collagen fibers into deionized water, and adding sodium hydroxide to adjust the pH value of the solution to 12; ultrasonic cleaning with deionized water after 6 hours, filtering, and drying in a vacuum oven for standby;
step three, adding 0.1g of sodium humate into 40ml of deionized water, and performing ultrasonic dissolution to obtain sodium humate aqueous solution;
and step four, adding 1g of the collagen fiber obtained in the step two into 40ml of sodium humate aqueous solution, and filtering after ultrasonic treatment at 45 ℃ for 4 hours. The mass ratio of the collagen fiber to the sodium humate is 10:1; the use ratio of the collagen fiber to the deionized water in the step three is 0.025g/ml;
and step five, adding 1g of the filtered collagen fiber obtained in the step four into 40ml of glutaraldehyde solution with the concentration of 5% (V/V), stirring for 12 hours, filtering, and drying in a vacuum oven to obtain the humic acid modified collagen fiber material for efficiently capturing iodine vapor, namely HA@ACF.
Example 2:
a preparation method of a humic acid modified collagen fiber material for efficiently capturing iodine vapor comprises the following steps:
firstly, adding 50g of collagen fibers into deionized water, ultrasonically cleaning for 5 hours in an ultrasonic cleaning machine, washing to be neutral, filtering, and drying in an oven;
step two, crushing the cleaned collagen fibers by a crusher, adding the crushed collagen fibers into deionized water, and adding sodium hydroxide to adjust the pH value of the solution to 12; ultrasonic cleaning with deionized water after 6 hours, filtering, and drying in a vacuum oven for standby;
step three, adding 0.1g of modified sodium humate into 40ml of deionized water, and performing ultrasonic dissolution to obtain a modified sodium humate aqueous solution;
and step four, adding 1g of the collagen fiber obtained in the step two into 40ml of modified sodium humate aqueous solution, and filtering after ultrasonic treatment at 45 ℃ for 4 hours. The mass ratio of the collagen fiber to the modified sodium humate is 10:1; the use ratio of the collagen fiber to the deionized water in the step three is 0.025g/ml;
and step five, adding 1g of the filtered collagen fiber obtained in the step four into 40ml of glutaraldehyde solution with the concentration of 5% (V/V), stirring for 12 hours, filtering, and drying in a vacuum oven to obtain the humic acid modified collagen fiber material for efficiently capturing iodine vapor.
The modification method of the modified sodium humate comprises the following steps:
s1, weighing 5g of anhydrous sodium sulfite, and dissolving the anhydrous sodium sulfite in 25mL of deionized water; magnetically stirring and heating to 60 ℃ to obtain sodium sulfite solution;
s2, dropwise adding 0.75mL of concentrated sulfuric acid into the sodium sulfite solution after the sodium sulfite solution is cooled to room temperature; then adding 4g of humic acid, heating and stirring for 5 hours at the rotation speed of 500r/min, wherein the heating temperature is 90 ℃; filtering and drying to obtain sulfonated humic acid;
s3, weighing 0.5g of sodium cellulose powder, adding 2g of sulfonated humic acid into 20mL of deionized water, adding sodium carboxymethyl cellulose powder, heating to 45 ℃, stirring at 160r/min for 40min, filtering and drying to obtain modified humate.
Comparative example 1:
a method for preparing an activated collagen fiber iodine vapor capturing material, comprising the following steps:
firstly, adding 50g of collagen fibers into deionized water, ultrasonically cleaning for 5 hours in an ultrasonic cleaning machine, washing to be neutral, filtering, and drying in an oven;
step two, crushing the cleaned collagen fibers by a crusher, adding the crushed collagen fibers into deionized water, and adding sodium hydroxide to adjust the pH value of the solution to 12; and (3) cleaning with deionized water after ultrasonic treatment for 6 hours, filtering, and drying in a vacuum oven for standby, so as to obtain the activated collagen fiber iodine capturing vapor material, which is marked as ACF.
Comparative example 2:
a method for preparing a collagen fiber iodine vapor capturing material, comprising the following steps:
step one, adding 50g of collagen fibers into deionized water, ultrasonically cleaning for 5 hours in an ultrasonic cleaner, washing to be neutral, filtering, and drying in an oven to obtain a collagen fiber iodine vapor capturing material, which is marked as CF.
Fig. 1 is an SEM image of the humic acid modified collagen fiber material prepared in example 1 of the present invention after adsorbing iodine vapor, and it can be seen from the image that the surface of the collagen fiber material is rough and filiform, and the morphology of ha@acf is basically unchanged after iodine capturing, which indicates that the adsorbent has good stability.
FIG. 2 is a diagram of a humic acid modified collagen fiber material according to the embodiment 1 of the present invention, which is a dense yellow brown substance; fig. 3 is a physical diagram of the humic acid modified collagen fiber material prepared in example 1 of the present invention after iodine vapor is adsorbed, the color is changed to dark black after iodine vapor is adsorbed, and local caking occurs in the appearance.
FIG. 4 shows a humic acid modified collagen fiber material (HA@ACF) prepared in example 1 of the invention, and a humic acid modified collagen fiber material (HA@ACF-I) after iodine vapor adsorption 2 ) And the Activated Collagen Fibers (ACF) prepared in comparative example 1 were recorded at 400 to 4000cm, respectively -1 Within the range ofFTIR results plot of (c). The results show that the FTIR spectra of the samples are all typical protein structures, and the characteristic adsorption peaks are amide I, amide II and amide III bands. 3421.1cm -1 The peak at this location is mainly due to the stretching vibration of O-H, and after Humic Acid (HA) is grafted to Activated Collagen Fibers (ACF), the peak vibration intensity of ha@acf at this location is enhanced, mainly due to the presence of a large number of phenolic hydroxyl structures in Humic Acid (HA), indicating that HA is successfully grafted to activated collagen fibers. 3421.1cm after iodine capture by HA@ACF -1 The peak at the position is obviously weakened, almost disappears and becomes smooth, which indicates that the capture of iodine vapor by HA@ACF is mainly through phenolic hydroxyl groups. At the same time at 1593cm -1 The adsorption peak at the position has small increase in intensity after the humic acid is grafted, which is attributed to the characteristic peak of the bending vibration of the benzene ring C-H. At 1529.2cm -1 The characteristic adsorption peak at this point is attributed to the characteristic peak of the amide II band of collagen of benzene ring N-H flexural vibration and C-N tensile vibration. And after grafting humic acid, the characteristic peak shifts to 1520cm -1 . The result shows that the humic acid is successfully grafted on the surface of the ACF. 1242.9cm -1 The peak at this point is due to the C-N in-plane bending vibration of the amide III band I of the protein, whose peak intensity decreases after iodine capture, which is probably due to the interaction of C-N with iodine. These results indicate that the hydroxyl content of ACF is greatly increased after grafting with humic acid by glutaraldehyde as a crosslinking agent, and the phenolic hydroxyl content is increased after the hydroxyl film is successfully constructed. Furthermore, 638.3cm -1 The peak vibration after grafting treatment was changed with enhanced change mainly due to out-of-plane bending vibration of O-H, indicating an increased O-H group content in the grafted ACF.
FIG. 5 is a graph of HA@ACF-I under a nitrogen atmosphere at a heating rate of 10 ℃/min 2 Thermogravimetric analysis of the release of medium iodine (TGA). As shown in fig. 5, the thermal stability of ACF (comparative example 1) and ha@acf (example 1) were almost uniform. After iodine vapor capture on ha@acf, the weight loss at 100 ℃ was only 4wt%.
The iodine adsorbed on ha@acf is relatively stable below 100 ℃ in view of moisture loss. The release rate of iodine then increased with increasing temperature, significantly losing weight (68.43 wt%) at 280 ℃ and was much higher than ha@acf at the same temperature, indicating that iodine had been released in the adsorbent.
FIG. 6 is an iodine vapor adsorption experiment performed on the humic acid modified collagenous fiber materials prepared in example 1 and example 2; the method comprises the following steps: adopting a non-radioactive iodine simple substance to replace a radioactive iodine simple substance; firstly, placing excessive iodine simple substance at the bottom of a 250mL serum bottle, respectively placing 50mg of humic acid modified collagen fiber materials (example 1 and example 2) in filter papers folded into a funnel shape, placing the filter papers in a serum bottle mouth, screwing a bottle cap, sealing the bottle cap by using a sealing film, placing the serum bottle in a 75 ℃ oven at different time intervals, taking out the serum bottle after longest absorption for 32 hours, cooling to room temperature, and measuring the content of iodine vapor absorbed by the modified collagen fiber according to a gravimetric method. The calculation formula is as follows:
Q＝(m 2 -m 1 )/m 1 ×100wt％
wherein Q (wt%) is the adsorption amount of iodine, m 1 (mg) and m 2 (mg) is the weight of the humic acid modified collagenous fiber material before and after iodine adsorption, respectively, and each adsorption material was subjected to 3 adsorption experiments in parallel, and the average value was taken, and the result is shown in FIG. 6.
The adsorption performance of ha@acf on iodine vapor was studied by a dynamic adsorption experiment, and the result is shown in fig. 6. The iodine vapor adsorption amount of HA@ACF is obviously increased in the first 22 hours, and a rapid adsorption effect is shown. Then the adsorption rate of iodine vapor is reduced, dynamic adsorption equilibrium is reached at 28h, and the adsorption amount of iodine vapor is up to 2816.2mg/g. It is possible that the hydroxyl groups on the surface of ACF have strong specific recognition to iodine, which is the main reason why the adsorbent has strong adsorption capacity to iodine vapor.
Fig. 11 is a graph showing the results of adsorption of iodine vapor at different intervals of the humic acid modified collagen fiber material prepared in example 1 and example 2, and it can be seen from fig. 11 that the humic acid modified collagen fiber material prepared in example 2 has a better adsorption effect on iodine vapor.
Fig. 12 is a graph showing the adsorption results of iodine vapor at 75 ℃ for the different modified collagen fiber materials prepared in example 1, comparative example 1 and comparative example 2, and it can be seen from fig. 12 that the humic acid modified collagen fiber prepared in example 1 has superior adsorption effect compared with comparative example 1 and comparative example 2.
Fig. 7-10 are X-ray photoelectron spectra of the change in valence state of each element of the material studied using XPS, further revealing the binding of ha@acf to iodine. As can be seen from FIG. 7, the new peaks appearing at 619eV and 631eV are I after iodine capture, respectively 3 d 5 2 and I 3 d 3 Characteristic peaks of/2, indicating that iodine is adsorbed on ha@acf. In FIG. 8, HA@ACF-I 2 I of (2) 3 d spectral decomposition into I 2 (620.4 eV and 631.7 eV) and I 3 - (618.9 eV and 630.3 eV). XPS O of HA@ACF 1 The s-spectrum is broken down into two peaks of 532.2eV (-OH) and 533.2eV (C-O-R) (FIG. 9). After iodine capture, the hydroxyl peak shifted from 532.2eV to 532.3eV, indicating that the hydroxyl group had an induced adsorption effect on iodine. Meanwhile, XPS N of HA@ACF 1 The s spectrum is decomposed into 400.3eV (-NH) 2 ) And 401.6eV (R-NH-R) (FIG. 10). After iodine capture, the peak of the imine was shifted from 401.6eV to 401.8eV, indicating that the imine was also involved in iodine capture. Thus, these results indicate that iodine is easily induced by electron rich hydroxyl and imine due to the lewis acid nature of the iodine molecule, resulting in chemisorption between iodine and hydroxyl or imine being the primary mechanism of high adsorption capacity of the material.
The number of equipment and the scale of processing described herein are intended to simplify the description of the present invention. Applications, modifications and variations of the present invention will be readily apparent to those skilled in the art.
Although embodiments of the present invention have been disclosed above, it is not limited to the details and embodiments shown and described, it is well suited to various fields of use for which the invention would be readily apparent to those skilled in the art, and accordingly, the invention is not limited to the specific details and illustrations shown and described herein, without departing from the general concepts defined in the claims and their equivalents.
Claims (10)
1. The preparation method of the humic acid modified collagen fiber material for efficiently capturing iodine vapor is characterized by comprising the following steps of:
step one, adding collagen fibers into deionized water, ultrasonically cleaning in an ultrasonic cleaner, then washing to be neutral, filtering, and then drying in an oven;
step two, crushing the cleaned collagen fibers in a crusher, adding the crushed collagen fibers into deionized water, and adding alkali to adjust the pH of the solution; washing with deionized water after ultrasonic treatment, filtering, and drying in a vacuum oven for later use;
thirdly, adding humate into deionized water, and performing ultrasonic dissolution to obtain a humate solution;
step four, adding the collagen fiber obtained in the step two into a humate solution, and placing the humate solution in a constant-temperature shaking table for curing treatment;
and step five, filtering the material obtained in the step four, adding the filtered solid into a cross-linking agent solution, stirring, filtering, and drying in vacuum to obtain the humic acid modified collagen fiber material for efficiently capturing iodine vapor.
2. The method for preparing the humic acid modified collagen fiber material capable of efficiently capturing iodine vapor according to claim 1, wherein the collagen fiber in the first step is untreated animal skin, and the raw material is obtained by crushing the raw material by a crusher after the raw material is subjected to washing, softening, alkali soaking, pickling, drying and the like according to a conventional method.
3. The method for preparing the humic acid modified collagen fiber material for efficiently capturing iodine vapor according to claim 1, wherein the ultrasonic cleaning temperature and the oven temperature in the first step are between room temperature and 90 ℃, and the ultrasonic cleaning time is 5 hours.
4. The method for preparing the humic acid modified collagen fiber material for efficiently capturing iodine vapor according to claim 1, wherein the alkali in the second step is one or more of potassium hydroxide, sodium bicarbonate, sodium carbonate, ammonia water and the like; adding alkali to regulate the pH value of the solution to 8-13.
5. The method for preparing the humic acid modified collagen fiber material for efficiently capturing iodine vapor according to claim 1, wherein different pH values in the second step correspond to different ultrasonic time, the pH value is 8-13, and the corresponding time is 10-5 h; and the ultrasonic time in the second step is 6h.
6. The method for preparing the material for efficiently capturing iodine vapor by using the humic acid modified collagen fibers according to claim 1, wherein in the third step, the humate comprises one or more of sodium humate, potassium humate, calcium humate, fulvic acid, sodium fulvate, potassium fulvate and calcium fulvate.
7. The method for preparing a material for efficiently capturing iodine vapor from humic acid modified collagen fibers according to claim 1, wherein in the third step, the concentration of the humate solution is 0.001-5% by mass.
8. The method for preparing the humic acid modified collagen fiber material capable of efficiently capturing iodine vapor according to claim 1, wherein in the fourth step, the mass percentage of the collagen fiber to the humate solution is 0.01-50: 100%.
9. The method for preparing the humic acid modified collagen fiber material for efficiently capturing iodine vapor according to claim 1, wherein the temperature of the constant-temperature shaking table in the fourth step is 20-130 ℃.
10. The method for preparing the humic acid modified collagen fiber material capable of efficiently capturing iodine vapor according to claim 1, wherein in the fifth step, the crosslinking agent comprises one or more of formaldehyde, glyoxal and glutaraldehyde; the concentration of the cross-linking agent is 3-8%wt, and the mass-volume ratio of the solid to the cross-linking agent is 5g:40mL; and in the fifth step, the stirring time is 12h.
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