CN115069218A - Preparation method of metal organic framework composite GO/waste spinning cellulose aerogel - Google Patents
Preparation method of metal organic framework composite GO/waste spinning cellulose aerogel Download PDFInfo
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- CN115069218A CN115069218A CN202110269545.2A CN202110269545A CN115069218A CN 115069218 A CN115069218 A CN 115069218A CN 202110269545 A CN202110269545 A CN 202110269545A CN 115069218 A CN115069218 A CN 115069218A
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- 229920002678 cellulose Polymers 0.000 title claims abstract description 117
- 239000001913 cellulose Substances 0.000 title claims abstract description 117
- 239000002699 waste material Substances 0.000 title claims abstract description 108
- 239000004964 aerogel Substances 0.000 title claims abstract description 79
- 238000009987 spinning Methods 0.000 title claims abstract description 53
- 239000012924 metal-organic framework composite Substances 0.000 title claims abstract description 41
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000004753 textile Substances 0.000 claims abstract description 50
- 238000001035 drying Methods 0.000 claims abstract description 23
- 239000000843 powder Substances 0.000 claims abstract description 16
- 239000000017 hydrogel Substances 0.000 claims abstract description 14
- 238000004061 bleaching Methods 0.000 claims abstract description 13
- 238000004140 cleaning Methods 0.000 claims abstract description 13
- 238000001179 sorption measurement Methods 0.000 claims abstract description 12
- 239000003431 cross linking reagent Substances 0.000 claims abstract description 7
- 239000004744 fabric Substances 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 6
- 238000004090 dissolution Methods 0.000 claims abstract description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 25
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 25
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 22
- 239000000243 solution Substances 0.000 claims description 22
- 239000012621 metal-organic framework Substances 0.000 claims description 21
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- UKLNMMHNWFDKNT-UHFFFAOYSA-M sodium chlorite Chemical compound [Na+].[O-]Cl=O UKLNMMHNWFDKNT-UHFFFAOYSA-M 0.000 claims description 15
- 229960002218 sodium chlorite Drugs 0.000 claims description 15
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- 229920003043 Cellulose fiber Polymers 0.000 claims description 13
- 238000000034 method Methods 0.000 claims description 12
- 239000004202 carbamide Substances 0.000 claims description 11
- 239000001569 carbon dioxide Substances 0.000 claims description 11
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 11
- 239000002243 precursor Substances 0.000 claims description 11
- 238000002791 soaking Methods 0.000 claims description 11
- 238000009210 therapy by ultrasound Methods 0.000 claims description 11
- 238000004108 freeze drying Methods 0.000 claims description 10
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 8
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 8
- 229920000742 Cotton Polymers 0.000 claims description 7
- 238000004132 cross linking Methods 0.000 claims description 7
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 6
- 239000005708 Sodium hypochlorite Substances 0.000 claims description 6
- HSJPMRKMPBAUAU-UHFFFAOYSA-N cerium(3+);trinitrate Chemical compound [Ce+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O HSJPMRKMPBAUAU-UHFFFAOYSA-N 0.000 claims description 6
- 239000002131 composite material Substances 0.000 claims description 6
- QQVIHTHCMHWDBS-UHFFFAOYSA-N isophthalic acid Chemical compound OC(=O)C1=CC=CC(C(O)=O)=C1 QQVIHTHCMHWDBS-UHFFFAOYSA-N 0.000 claims description 6
- 239000013110 organic ligand Substances 0.000 claims description 6
- 239000003960 organic solvent Substances 0.000 claims description 6
- 239000004627 regenerated cellulose Substances 0.000 claims description 6
- SUKJFIGYRHOWBL-UHFFFAOYSA-N sodium hypochlorite Chemical compound [Na+].Cl[O-] SUKJFIGYRHOWBL-UHFFFAOYSA-N 0.000 claims description 6
- 238000000352 supercritical drying Methods 0.000 claims description 6
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-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
- OERNJTNJEZOPIA-UHFFFAOYSA-N zirconium nitrate Chemical compound [Zr+4].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O OERNJTNJEZOPIA-UHFFFAOYSA-N 0.000 claims description 6
- LXBGSDVWAMZHDD-UHFFFAOYSA-N 2-methyl-1h-imidazole Chemical compound CC1=NC=CN1 LXBGSDVWAMZHDD-UHFFFAOYSA-N 0.000 claims description 5
- 244000025254 Cannabis sativa Species 0.000 claims description 5
- 235000012766 Cannabis sativa ssp. sativa var. sativa Nutrition 0.000 claims description 5
- 235000012765 Cannabis sativa ssp. sativa var. spontanea Nutrition 0.000 claims description 5
- 235000009120 camo Nutrition 0.000 claims description 5
- 235000005607 chanvre indien Nutrition 0.000 claims description 5
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 5
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 5
- 238000007710 freezing Methods 0.000 claims description 5
- 239000011487 hemp Substances 0.000 claims description 5
- 238000011065 in-situ storage Methods 0.000 claims description 5
- 238000005406 washing Methods 0.000 claims description 5
- 239000011837 N,N-methylenebisacrylamide Substances 0.000 claims description 4
- 229960000583 acetic acid Drugs 0.000 claims description 4
- 230000008014 freezing Effects 0.000 claims description 4
- 239000012362 glacial acetic acid Substances 0.000 claims description 4
- RBTARNINKXHZNM-UHFFFAOYSA-K iron trichloride Chemical compound Cl[Fe](Cl)Cl RBTARNINKXHZNM-UHFFFAOYSA-K 0.000 claims description 4
- 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 4
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 4
- 238000000643 oven drying Methods 0.000 claims description 4
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims description 3
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 3
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 3
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 claims description 3
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 3
- 241000219146 Gossypium Species 0.000 claims description 3
- 229910021578 Iron(III) chloride Inorganic materials 0.000 claims description 3
- 229920000433 Lyocell Polymers 0.000 claims description 3
- 239000013177 MIL-101 Substances 0.000 claims description 3
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 3
- 239000002202 Polyethylene glycol Substances 0.000 claims description 3
- 229920000297 Rayon Polymers 0.000 claims description 3
- 239000011425 bamboo Substances 0.000 claims description 3
- 239000007844 bleaching agent 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
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 3
- 238000007599 discharging Methods 0.000 claims description 3
- 239000007789 gas Substances 0.000 claims description 3
- 238000010335 hydrothermal treatment Methods 0.000 claims description 3
- 239000012535 impurity Substances 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 3
- 238000003760 magnetic stirring Methods 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- UWJJYHHHVWZFEP-UHFFFAOYSA-N pentane-1,1-diol Chemical compound CCCCC(O)O UWJJYHHHVWZFEP-UHFFFAOYSA-N 0.000 claims description 3
- 229920001223 polyethylene glycol Polymers 0.000 claims description 3
- 235000010413 sodium alginate Nutrition 0.000 claims description 3
- 239000000661 sodium alginate Substances 0.000 claims description 3
- 229940005550 sodium alginate Drugs 0.000 claims description 3
- 239000013176 zeolitic imidazolate framework-12 Substances 0.000 claims description 3
- 239000013154 zeolitic imidazolate framework-8 Substances 0.000 claims description 3
- 239000013173 zeolitic imidazolate framework-9 Substances 0.000 claims description 3
- MFLKDEMTKSVIBK-UHFFFAOYSA-N zinc;2-methylimidazol-3-ide Chemical compound [Zn+2].CC1=NC=C[N-]1.CC1=NC=C[N-]1 MFLKDEMTKSVIBK-UHFFFAOYSA-N 0.000 claims description 3
- -1 divinyl vanadium Chemical compound 0.000 claims description 2
- 244000082204 Phyllostachys viridis Species 0.000 claims 1
- 238000002604 ultrasonography Methods 0.000 claims 1
- 229910052751 metal Inorganic materials 0.000 abstract description 4
- 239000002184 metal Substances 0.000 abstract description 4
- 238000011084 recovery Methods 0.000 abstract description 3
- 239000010865 sewage Substances 0.000 abstract description 3
- 239000000463 material Substances 0.000 abstract description 2
- 150000001875 compounds Chemical class 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- 239000000975 dye Substances 0.000 description 14
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 description 9
- 230000015556 catabolic process Effects 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 4
- 230000032683 aging Effects 0.000 description 3
- 239000003344 environmental pollutant Substances 0.000 description 3
- 231100000719 pollutant Toxicity 0.000 description 3
- 241001330002 Bambuseae Species 0.000 description 2
- 230000004913 activation Effects 0.000 description 2
- 230000003197 catalytic effect Effects 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000018109 developmental process Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 238000004064 recycling Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- LRWZZZWJMFNZIK-UHFFFAOYSA-N 2-chloro-3-methyloxirane Chemical compound CC1OC1Cl LRWZZZWJMFNZIK-UHFFFAOYSA-N 0.000 description 1
- 240000008564 Boehmeria nivea Species 0.000 description 1
- 206010007269 Carcinogenicity Diseases 0.000 description 1
- 239000013179 MIL-101(Fe) Substances 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
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- 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
- B01J20/223—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material containing metals, e.g. organo-metallic compounds, coordination complexes
- B01J20/226—Coordination polymers, e.g. metal-organic frameworks [MOF], zeolitic imidazolate frameworks [ZIF]
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- 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
- B01J13/00—Colloid chemistry, e.g. the production of colloidal materials or their solutions, not otherwise provided for; Making microcapsules or microballoons
- B01J13/0091—Preparation of aerogels, e.g. xerogels
-
- 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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28047—Gels
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- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/1691—Coordination polymers, e.g. metal-organic frameworks [MOF]
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- 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
- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/18—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms
- B01J31/1805—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes containing nitrogen, phosphorus, arsenic or antimony as complexing atoms, e.g. in pyridine ligands, or in resonance therewith, e.g. in isocyanide ligands C=N-R or as complexed central atoms the ligands containing nitrogen
- B01J31/181—Cyclic ligands, including e.g. non-condensed polycyclic ligands, comprising at least one complexing nitrogen atom as ring member, e.g. pyridine
- B01J31/1815—Cyclic ligands, including e.g. non-condensed polycyclic ligands, comprising at least one complexing nitrogen atom as ring member, e.g. pyridine with more than one complexing nitrogen atom, e.g. bipyridyl, 2-aminopyridine
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- B01J31/00—Catalysts comprising hydrides, coordination complexes or organic compounds
- B01J31/16—Catalysts comprising hydrides, coordination complexes or organic compounds containing coordination complexes
- B01J31/22—Organic complexes
- B01J31/2204—Organic complexes the ligands containing oxygen or sulfur as complexing atoms
- B01J31/2208—Oxygen, e.g. acetylacetonates
- B01J31/2226—Anionic ligands, i.e. the overall ligand carries at least one formal negative charge
- B01J31/223—At least two oxygen atoms present in one at least bidentate or bridging ligand
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- B01J35/60—Catalysts, in general, characterised by their form or physical properties characterised by their surface properties or porosity
- B01J35/61—Surface area
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- B01J2531/00—Additional information regarding catalytic systems classified in B01J31/00
- B01J2531/80—Complexes comprising metals of Group VIII as the central metal
- B01J2531/84—Metals of the iron group
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Abstract
The invention relates to a preparation method of metal organic framework composite Graphene Oxide (GO)/waste spinning cellulose aerogel, and belongs to the technical field of materials. The preparation method of the metal organic framework composite Graphene Oxide (GO)/waste spinning cellulose aerogel comprises the following steps: a. cleaning, bleaching and crushing the waste cellulose textile to obtain textile powder, wherein the particle size of the textile powder is 0.2-4 mm; b. will the fabrics powder is dissolved under the low temperature dissolution system, adds graphene oxide, adds the cross-linking agent and forms the hydrogel, obtains GO/useless spinning cellulose aerogel c through the drying at last and with GO/useless spinning cellulose aerogel normal position generation metal organic frame, obtains the compound GO/useless spinning cellulose aerogel of metal organic frame that has adsorption performance, low cost, easy recovery, has solved the pollution problem that old and useless cellulose fabrics caused, and can be used to sewage treatment.
Description
Technical Field
The invention relates to a preparation method of metal organic framework composite GO/waste spinning cellulose aerogel, belonging to the technical field of materials.
Background
Over the past few decades, the increase in global income and living standards has led to a steady increase in the production and consumption of textiles and fibers, bringing about a large amount of waste cellulosic textiles while escalating raw material costs. However, most of the waste cellulose textiles are not well recycled, most of the waste cellulose textiles are directly buried underground in a landfill mode or are incinerated in a specific place, and the methods not only occupy land resources, consume resources such as coal and electric power, but also bring burden to the environment and cause pollution.
With the worldwide acceleration of industrialization, water resource pollution has become an important component of environmental safety issues. Organic dyes, heavy metal ions and antibiotic drugs are common hazardous pollutants, and cause serious harm to human health and biodiversity. Currently, over 100000 commercial dyes are used in areas including textile, paper, plastics, food, cosmetics and paint industries. Organic dyes are the most common pollutants in water sources and have potential hazards of complex structure, non-biodegradability, carcinogenicity and the like. The development of functional materials with dye recovery and dye degradation is of great significance.
The metal organic framework has the advantages of large specific surface area, controllable porosity and structure and the like, and has high commercial value in the fields of catalysis, adsorption and the like. Currently, various metal-organic frameworks are used in adsorption, e.g. CN111992185A, CN112023893A and CN 112138634A. However, these metal-organic frameworks are very difficult to separate after adsorbing target pollutants, resulting in resource waste and secondary pollution. The cellulose aerogel has a light and three-dimensional net-shaped porous structure, and the existence of hydrophilic groups of cellulose is easy to combine with the metal-organic framework, which is undoubtedly the best carrier of the metal-organic framework. The cellulose fiber is one of the most important textile raw materials, occupies a great share in the waste textiles, is prepared into a cellulose aerogel load metal organic framework for sewage treatment, and realizes the cyclic green re-development of the waste cellulose textiles.
Disclosure of Invention
The first purpose of the invention is to provide a new method for recycling waste cellulose textile.
In order to achieve the first object of the invention, the preparation method of the metal organic framework composite GO/waste spinning cellulose aerogel comprises the following steps:
a. cleaning, bleaching and crushing waste cellulose textiles to obtain textile powder;
b. dissolving the textile powder by using a low-temperature dissolving system, adding graphene oxide, adding a cross-linking agent, removing water and drying to obtain GO/waste spinning cellulose aerogel;
c. generating a metal organic framework on the GO/waste spinning cellulose aerogel in situ, and cleaning and drying to obtain a composite aerogel;
in a specific embodiment, the cleaning in the step a is to perform ultrasonic treatment on the waste cellulose textile in an organic solvent, remove impurities and dry the waste cellulose textile; the organic solvent is preferably at least one of acetone and ethanol, and more preferably the volume ratio of the acetone to the ethanol is 1-3: 1; and a, the ultrasonic treatment time in the step a is 20-35 min.
In one embodiment, the dissolving system in step b is at least one of sodium hydroxide, potassium hydroxide, sodium hydroxide/urea, lithium hydroxide/urea, and sodium hydroxide/thiourea; preferred sodium hydroxide/urea; the mass ratio of the sodium hydroxide to the urea to the water is 5-8: 12-14: 78-83; the dissolution temperature is as follows: the dissolving time is 4-24h at-8 to-12 ℃.
In a specific embodiment, the mass ratio of the GO in the step b to the waste cellulose textile is 0.5 wt% -4 wt%.
In a specific embodiment, the crosslinking agent in the step b is at least one of N, N-methylene bisacrylamide, epichlorohydrin, pentanediol, sodium alginate, glutaraldehyde, divinylalum and polyethylene glycol glycidyl ether; magnetic stirring or ultrasonic treatment is carried out for 1 to 3 hours, the crosslinking temperature is between 25 and 55 ℃, and the crosslinking time is between 8 and 24 hours.
In one embodiment, the drying in step b is at least one of freeze drying and supercritical drying; pre-freezing for 2-10 h at-20 to-50 ℃, and freeze-drying for 24-48 h under the air pressure of 1-20 Pa; or drying by using supercritical carbon dioxide, firstly soaking GO/waste spinning cellulose hydrogel in acetone for 1-4 d, then placing the soaked GO/waste spinning cellulose hydrogel in liquid carbon dioxide for 4-12 h, and then uniformly discharging gas to obtain the dried aerogel, wherein the state of the supercritical carbon dioxide is 40-80 ℃ and 9-20 MPa.
In a specific embodiment, the in-situ generation in the step c is to mix GO/waste cellulose aerogel with a metal organic framework precursor solution to obtain a mixed solution, and perform aging or hydrothermal treatment to obtain the metal organic framework composite GO/waste cellulose aerogel. The mass ratio of the GO/waste spinning cellulose aerogel to the metal organic framework precursor is 1: 3-7;
in a specific embodiment, the metal-organic framework precursor solution in step c is a mixed solution of cobalt nitrate, at least one of ferric nitrate, ferric chloride, zinc nitrate, cerium nitrate and zirconium nitrate, and an organic ligand, wherein the organic ligand is at least one of isophthalic acid, terephthalic acid and 2-methylimidazole;
the metal organic framework is preferably at least one of ZIF-67, ZIF-8, ZIF-9, ZIF-12, MIL-88 and MIL-101.
In one embodiment, the washing in step c may be performed with at least one of methanol, ethanol, and N, N-dimethylformamide; the drying is at least one of oven drying, freeze drying and supercritical drying.
In one embodiment, the bleaching agent used in the bleaching is at least one of sodium chlorite, sodium hypochlorite or hydrogen peroxide; preferably, the bleaching system used is sodium chlorite; more preferably, the method of bleaching comprises: soaking the waste cellulose textile in 3-12 wt% sodium chlorite solution, adjusting the pH value to 4-4.5 by using glacial acetic acid, and treating for 4-16 h at 70-80 ℃; preferably, the mass ratio of the sodium chlorite dosage to the waste cellulose textile is 3-6: 1.
In a specific embodiment, the waste cellulose textile is at least one of natural cellulose fiber, regenerated cellulose fiber and a blended textile fabric of the natural cellulose fiber and the regenerated cellulose fiber; preferably, the waste cellulose textile is at least one of cotton, hemp, bamboo, viscose, modal and tencel.
A second objective to be achieved by the present invention is to provide a metal organic framework composite GO/waste cellulose aerogel.
In order to achieve the second purpose of the invention, the metal organic framework composite GO/waste spinning cellulose aerogel is prepared by adopting the method;
preferably, the density of the metal organic framework composite GO/waste spinning cellulose aerogel is 30-100 mg/cm 3 ；
More preferably, the maximum adsorption capacity of the metal organic framework composite GO/waste spinning cellulose aerogel on the dye can reach 70 mg/g-1300 mg/g.
Has the advantages that:
the GO/waste spinning cellulose aerogel prepared by taking the waste cellulose fabric as the raw material has the advantages of high mechanical property, good chemical stability, porosity, light weight, large specific surface area, low price, easiness in obtaining, no harm to a human body and the like. The introduction of the metal organic frame can further increase the specific surface area and the porosity of the aerogel, effectively realize the adsorption of the dye, and the light aerogel can realize the recovery and the reutilization of the metal organic frame and the dye. The invention creatively explores the advantages of the whole process flow for preparing the composite cellulose aerogel with good performance from the waste cellulose textiles:
1) the metal organic framework composite GO/cellulose aerogel prepared by the method is light in weight, excellent in mechanical property and 30-100 mg/cm in density 3 ；
2) The maximum adsorption capacity of the metal organic framework composite GO/cellulose aerogel prepared by the method can reach 70-1300 mg/g for dyes.
3) The metal organic framework composite GO/cellulose aerogel prepared by the invention is extremely easy to recover and convenient to recycle after dyes are adsorbed, and the problem that the adsorbent is difficult to separate is solved.
4) The invention takes the waste cellulose textile as the raw material, can solve the problem of dye sewage in the industries of textile, food and the like, and can realize the circular, green and high-valued development of the textile industry.
Drawings
Fig. 1 is a flow chart of the preparation method of metal-organic framework composite GO/waste-spun cellulose aerogel in example 1 of the present invention.
Figure 2 is an XRD pattern of the metal-organic framework composite GO/waste cellulose aerogel in example 1 of the present invention.
FIG. 3 is the dye adsorption performance of the metal-organic framework composite GO/waste cellulose aerogel in example 1 of the present invention.
FIG. 4 is the catalytic degradation performance of the metal-organic framework composite GO/waste cellulose aerogel on dyes in example 1 of the present invention.
Detailed Description
The first purpose of the invention is to provide a new method for recycling waste cellulose textile.
In order to achieve the first object of the invention, the preparation method of the metal organic framework composite GO/waste spinning cellulose aerogel comprises the following steps:
a. cleaning, bleaching and crushing waste cellulose textiles to obtain textile powder;
b. dissolving the textile powder by using a low-temperature dissolving system, adding graphene oxide, adding a cross-linking agent, removing water and drying to obtain GO/waste spinning cellulose aerogel;
c. generating a metal organic framework on the GO/waste spinning cellulose aerogel in situ, and cleaning and drying to obtain a composite aerogel;
in a specific embodiment, the cleaning in the step a is to perform ultrasonic treatment on the waste cellulose textile in an organic solvent, remove impurities and dry the waste cellulose textile; the organic solvent is preferably at least one of acetone and ethanol, and more preferably the volume ratio of the acetone to the ethanol is 1-3: 1; and a, the ultrasonic treatment time in the step a is 20-35 min.
In one embodiment, the dissolving system in step b is at least one of sodium hydroxide, potassium hydroxide, sodium hydroxide/urea, lithium hydroxide/urea, and sodium hydroxide/thiourea; preferred sodium hydroxide/urea; the mass ratio of the sodium hydroxide to the urea to the water is 5-8: 12-14: 78-83; the dissolution temperature is as follows: the dissolving time is 4-24h at-8 to-12 ℃.
In a specific embodiment, the mass ratio of the GO in the step b to the waste cellulose textile is 0.5 wt% -4 wt%.
In a specific embodiment, the crosslinking agent in the step b is at least one of N, N-methylene bisacrylamide, epichlorohydrin, pentanediol, sodium alginate, glutaraldehyde, divinylalum and polyethylene glycol glycidyl ether; magnetic stirring or ultrasonic treatment is carried out for 1 to 3 hours, the crosslinking temperature is between 25 and 55 ℃, and the crosslinking time is between 8 and 24 hours.
In one embodiment, the drying in step b is at least one of freeze drying and supercritical drying; pre-freezing for 2-10 h at-20 to-50 ℃, and freeze-drying for 24-48 h under the air pressure of 1-20 Pa; or drying by using supercritical carbon dioxide, firstly soaking GO/waste spinning cellulose hydrogel in acetone for 1-4 d, then placing the soaked GO/waste spinning cellulose hydrogel in liquid carbon dioxide for 4-12 h, and then uniformly discharging gas to obtain the dried aerogel, wherein the state of the supercritical carbon dioxide is 40-80 ℃ and 9-20 MPa.
In a specific embodiment, the in-situ generation in the step c is to mix GO/waste cellulose aerogel with a metal organic framework precursor solution to obtain a mixed solution, and perform aging or hydrothermal treatment to obtain the metal organic framework composite GO/waste cellulose aerogel. The mass ratio of the GO/waste spinning cellulose aerogel to the metal organic framework precursor solution is 1: 3-7;
in a specific embodiment, the metal organic framework precursor solution in step c is a mixed solution of at least one of cobalt nitrate, ferric chloride, zinc nitrate, cerium nitrate and zirconium nitrate and an organic ligand, wherein the organic ligand is at least one of isophthalic acid, terephthalic acid and 2-methylimidazole;
the metal organic framework is preferably at least one of ZIF-67, ZIF-8, ZIF-9, ZIF-12, MIL-88 and MIL-101.
In one embodiment, the washing in step c may be performed with at least one of methanol, ethanol, and N, N-dimethylformamide; the drying is at least one of oven drying, freeze drying and supercritical drying.
In one embodiment, the bleaching agent used in the bleaching is at least one of sodium chlorite, sodium hypochlorite or hydrogen peroxide; preferably, the bleaching system used is sodium chlorite; more preferably, the method of bleaching comprises: soaking the waste cellulose textile in 3-12 wt% sodium chlorite solution, adjusting the pH value to 4-4.5 by using glacial acetic acid, and treating for 4-16 h at 70-80 ℃; preferably, the mass ratio of the sodium chlorite dosage to the waste cellulose textile is 3-6: 1.
In a specific embodiment, the waste cellulose textile is at least one of natural cellulose fiber, regenerated cellulose fiber and a blended textile fabric of the natural cellulose fiber and the regenerated cellulose fiber; preferably, the waste cellulose textile is at least one of cotton, hemp, bamboo, viscose, modal and tencel.
A second objective to be achieved by the present invention is to provide a metal organic framework composite GO/waste cellulose aerogel.
In order to achieve the second purpose of the invention, the metal organic framework composite GO/waste spinning cellulose aerogel is prepared by adopting the method;
preferably, the density of the metal organic framework composite GO/waste spinning cellulose aerogel is 30-100 mg/cm 3 ；
More preferably, the maximum adsorption capacity of the metal organic framework composite GO/waste spinning cellulose aerogel on the dye can reach 70 mg/g-1300 mg/g.
The following examples are provided to further illustrate the embodiments of the present invention and are not intended to limit the scope of the present invention.
Example 1
Ultrasonic cleaning waste cotton cloth with size of 5cm × 5cm with acetone and ethanol for 20min, and oven drying. Preparing a sodium chlorite solution by 6 wt%, completely soaking small pieces of cut waste cotton in the sodium chlorite solution, dropwise adding glacial acetic acid, adjusting the pH value to be 4.5, sealing a container, and treating for 12 hours in a warm water bath at 80 ℃. The mass ratio of the sodium chlorite dosage to the waste spinning is 5: 1, cleaning, drying and crushing for later use. Taking 2g of the cotton powder, and placing the cotton powder in a mass ratio of sodium hydroxide/urea/water of 7: 12: 81, freezing in a household refrigerator at-12 ℃ for 4h, stirring to form a uniform cellulose solution, adding 40mg of GO powder, and performing ultrasonic treatment for 30 min. And (3) carrying out ultrasonic treatment on 1.2g of N, N-Methylene Bisacrylamide (MBA) for 1 hour, carrying out room-temperature crosslinking for 4 hours, and soaking the obtained product in deionized water until the obtained product is neutral to obtain the GO/waste-spinning cellulose hydrogel. Pre-freezing GO/waste spinning cellulose hydrogel for 2h at-20 ℃, and carrying out freeze drying for 48h under the air pressure of 10Pa to obtain GO/waste spinning cellulose aerogel. 1.164g of cobalt nitrate and 2.6g of 2-methylimidazole were dissolved in 50ml of methanol, respectively. And (3) quickly adding the cobalt nitrate solution into the 2-methylimidazole solution, and stirring for 3 minutes to obtain a purple ZIF-67 precursor solution. Adding 0.3g of GO/waste spinning cellulose aerogel into the purple precursor solution, aging at room temperature for 24h, cleaning and drying to obtain the ZIF-67 composite GO/waste spinning cellulose aerogel.
Performance of metal organic framework composite GO/waste cellulose aerogel obtained in example 1:
the density of the metal organic framework composite GO/waste spinning cellulose aerogel is 45mg/cm 3
The maximum adsorption capacity of the aerogel on MG is 1300MG/g
The aerogel has PMS activation performance: the degradation rate of 50mg/l MB at 18min can reach 100 percent
Example 2
And (3) ultrasonically cleaning the waste linen with the size of 5cm multiplied by 5cm for 40min by using acetone and ethanol respectively, and drying. Preparing a sodium hypochlorite solution with the concentration of 2g/L, completely soaking the small pieces of the cut waste ramie in the sodium hypochlorite solution, and piling for 2 hours. The mass ratio of the sodium hypochlorite dosage to the waste spinning is 1: and 5, cleaning, drying and crushing for later use. Taking 4g of hemp powder, and placing the hemp powder in a reaction kettle with a mass ratio of lithium hydroxide/urea/water of 2.1: 1: 46.9 at-10 deg.C for 2h, stirring to form cellulose solution, adding 20mg GO powder, and ultrasonic treating for 30 min. And (3) dropwise adding 10ml of epoxy chloropropane, magnetically stirring for 2h, placing the whole sample in a constant-temperature water bath kettle at 45 ℃ for 10h, and soaking the sample in deionized water until the sample is neutral to obtain the GO/waste spinning cellulose hydrogel. Soaking the hydrogel in an acetone solution for 2d, then placing the hydrogel in supercritical carbon dioxide for 6h, and uniformly deflating to obtain GO/waste spinning cellulose aerogel, wherein the supercritical carbon dioxide state is 60 ℃ and 10 MPa. Adding 1.5g of ferric trichloride into 30ml of DMF for dissolving, adding 0.412g of terephthalic acid into the solution, stirring for 10min, performing ultrasonic treatment for 10min, adding 0.3g of GO/waste spinning cellulose aerogel into the mixed solution, transferring the mixed solution into a polytetrafluoroethylene reaction kettle, reacting for 20h at 110 ℃, respectively washing for 2 times by using N, N-dimethylformamide and methanol, and drying in an oven at 60 ℃ for 12h to obtain the MIL-101(Fe) composite GO/waste spinning cellulose aerogel.
The performance of the metal organic framework composite GO/waste cellulose aerogel obtained in example 2 is as follows:
the density of the metal organic framework composite GO/waste spinning cellulose aerogel is 68mg/cm 3
The maximum adsorption amount of the aerogel on AR is 300mg/g
The aerogel has PMS activation performance: the degradation rate of 10mg/l MB in 30min can reach 97.8 percent
The preparation method has the advantages of simple preparation process, good chemical stability, good adsorption performance and catalytic degradation performance, and wide application prospect in environmental management.
Claims (10)
1. The preparation method of the metal organic framework composite GO/waste spinning cellulose aerogel is characterized by comprising the following steps:
a. washing, bleaching and crushing the waste cellulose textile to obtain cellulose textile powder, wherein the size of the textile powder is 0.2-4 mm;
b. dissolving the cellulose textile powder by using a low-temperature dissolving system, adding Graphene Oxide (GO), adding a cross-linking agent, removing water and drying to obtain GO/waste spinning cellulose aerogel;
c. and generating a metal organic framework on the GO/waste spinning cellulose aerogel in situ, and cleaning and drying to obtain the composite aerogel.
2. The preparation method of the metal organic framework composite GO/waste cellulose aerogel according to claim 1, wherein the cleaning in step a is carried out by ultrasonic treatment of waste cellulose textiles in an organic solvent, impurity removal and drying; the organic solvent is preferably at least one of acetone and ethanol, and more preferably the volume ratio of the acetone to the ethanol is 1-3: 1;
and a, the ultrasonic treatment time in the step a is 20-35 min.
3. The preparation method of metal organic framework composite GO/waste cellulose aerogel according to claim 1, wherein the cellulose dissolution system in step b is at least one of sodium hydroxide, potassium hydroxide, sodium hydroxide/urea, sodium hydroxide/thiourea; the dissolution temperature is as follows: the temperature is minus 8 ℃ to minus 12 ℃, and the dissolving time is 4-24 h; the mass ratio of GO to the waste cellulose textile is 0.5 wt% -4 wt%.
4. The preparation method of the metal organic framework composite GO/waste spinning cellulose aerogel according to claim 1, wherein the cross-linking agent in the step b is at least one of N, N-methylene bisacrylamide, epichlorohydrin, pentanediol, sodium alginate, glutaraldehyde, divinyl vanadium and polyethylene glycol glycidyl ether, the cross-linking temperature is 25-55 ℃, the cross-linking time is 8-24 hours, GO/waste spinning cellulose hydrogel is formed by magnetic stirring or ultrasound for 1-3 hours, the GO/waste spinning cellulose hydrogel is washed by deionized water until the pH value is neutral, and the GO/waste spinning cellulose aerogel is obtained by drying.
5. The preparation method of the metal organic framework composite GO/waste cellulose aerogel according to any one of claims 1-4, wherein the drying in the step b is freeze drying or supercritical drying; pre-freezing for 2-10 h at-20 to-50 ℃, and freeze-drying for 24-48 h under the air pressure of 1-20 Pa; or drying by using supercritical carbon dioxide, firstly soaking GO/waste spinning cellulose hydrogel in acetone for 1-4 d, then placing the soaked GO/waste spinning cellulose hydrogel in liquid carbon dioxide for 4-12 h, and then uniformly discharging gas to obtain the dried aerogel, wherein the state of the supercritical carbon dioxide is 40-80 ℃ and 9-20 MPa.
6. The preparation method of the metal organic framework composite GO/waste spun cellulose aerogel according to any one of claims 1 to 5, wherein the GO/waste spun cellulose aerogel is mixed with a metal organic framework precursor solution to obtain a mixed solution, and the mixed solution is aged or subjected to hydrothermal treatment to obtain the metal organic framework composite GO/waste spun cellulose aerogel; the mass ratio of the GO/waste spinning cellulose aerogel to the metal organic framework precursor is 1: 3 to 7.
7. The preparation method of the metal-organic framework composite GO/waste cellulose aerogel according to any one of claims 1 to 6, wherein the metal-organic framework precursor solution is a mixed solution of at least one of cobalt nitrate, ferric chloride, ferric nitrate, zinc nitrate, cerium nitrate and zirconium nitrate and an organic ligand, and the organic ligand is at least one of isophthalic acid, terephthalic acid and 2-methylimidazole;
the metal organic framework is preferably at least one of ZIF-67, ZIF-8, ZIF-9, ZIF-12, MIL-88 and MIL-101.
8. The preparation method of the metal organic framework composite GO/waste spun cellulose aerogel according to any one of claims 1-7, wherein in the step c, the washing can be performed by using at least one of methanol, ethanol and N, N-dimethylformamide; the drying is at least one of oven drying, freeze drying and supercritical drying.
9. The preparation method of the metal organic framework composite GO/waste spun cellulose aerogel according to any one of claims 1 to 8, wherein the bleaching agent used for bleaching is at least one of sodium chlorite, sodium hypochlorite or hydrogen peroxide; preferably, the bleaching system used is sodium chlorite; more preferably, the method of bleaching comprises: soaking the waste cellulose textile in 3-12 wt% sodium chlorite solution, adjusting the pH value to 4-4.5 with glacial acetic acid, and treating for 4-16 h at 70-80 ℃; preferably, the mass ratio of the sodium chlorite to the waste cellulose textile is 3-6: 1; the waste cellulose textile is at least one of natural cellulose fiber, regenerated cellulose fiber and a blended textile fabric of the natural cellulose fiber and the regenerated cellulose fiber; preferably, the waste cellulose textile is at least one of cotton, hemp, bamboo, viscose, modal and tencel.
10. The metal organic framework composite GO/waste spinning cellulose aerogel is characterized by being prepared by the method of any one of claims 1-9;
preferably, the density of the metal organic framework composite GO/waste spinning cellulose aerogel is 30-100 mg/cm 3 ；
More preferably, the maximum adsorption capacity of the metal organic framework composite GO/waste spinning cellulose aerogel on the dye can reach 70-1400 mg/g.
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| CN115722202A (en) * | 2022-11-08 | 2023-03-03 | 中国科学院上海高等研究院 | Yttrium-zirconium-terephthalic acid based composite magnetic adsorption material for removing organic phosphine in water, preparation method and application thereof |
| CN115722202B (en) * | 2022-11-08 | 2024-03-29 | 中国科学院上海高等研究院 | Yttrium-zirconium-terephthalic acid-based composite magnetic adsorption material for removing organic phosphine in water, preparation method and application thereof |
| CN115678411A (en) * | 2022-12-19 | 2023-02-03 | 南昌航空大学 | Method for preparing GO/Ce-MOF @ PDA/PU super-hydrophobic self-repairing anti-corrosion coating |
| CN117427622A (en) * | 2023-12-14 | 2024-01-23 | 常熟理工学院 | ZIF-8 in-situ modified magnetic halloysite/polyvinylidene fluoride composite aerogel and preparation method and application thereof |
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