CN114984923A - Preparation method of jute fiber-based high-adsorbability hydrophobic cellulose aerogel - Google Patents
Preparation method of jute fiber-based high-adsorbability hydrophobic cellulose aerogel Download PDFInfo
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- 240000000491 Corchorus aestuans Species 0.000 title claims abstract description 100
- 235000011777 Corchorus aestuans Nutrition 0.000 title claims abstract description 100
- 235000010862 Corchorus capsularis Nutrition 0.000 title claims abstract description 100
- 239000001913 cellulose Substances 0.000 title claims abstract description 60
- 229920002678 cellulose Polymers 0.000 title claims abstract description 60
- 239000000835 fiber Substances 0.000 title claims abstract description 56
- 239000004964 aerogel Substances 0.000 title claims abstract description 39
- 230000002209 hydrophobic effect Effects 0.000 title claims abstract description 26
- 238000002360 preparation method Methods 0.000 title claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims description 49
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 42
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 29
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 20
- 239000000017 hydrogel Substances 0.000 claims description 20
- 238000005406 washing Methods 0.000 claims description 15
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims description 12
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 230000007935 neutral effect Effects 0.000 claims description 10
- 238000001291 vacuum drying Methods 0.000 claims description 10
- 238000001179 sorption measurement Methods 0.000 claims description 9
- 238000005303 weighing Methods 0.000 claims description 9
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 7
- 239000004202 carbamide Substances 0.000 claims description 7
- 239000003431 cross linking reagent Substances 0.000 claims description 6
- 239000005055 methyl trichlorosilane Substances 0.000 claims description 6
- JLUFWMXJHAVVNN-UHFFFAOYSA-N methyltrichlorosilane Chemical compound C[Si](Cl)(Cl)Cl JLUFWMXJHAVVNN-UHFFFAOYSA-N 0.000 claims description 6
- BFXIKLCIZHOAAZ-UHFFFAOYSA-N methyltrimethoxysilane Chemical compound CO[Si](C)(OC)OC BFXIKLCIZHOAAZ-UHFFFAOYSA-N 0.000 claims description 6
- 239000011148 porous material Substances 0.000 claims description 6
- 239000005051 trimethylchlorosilane Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 5
- 238000004140 cleaning Methods 0.000 claims description 5
- 238000005520 cutting process Methods 0.000 claims description 5
- 239000012153 distilled water Substances 0.000 claims description 5
- 238000004108 freeze drying Methods 0.000 claims description 5
- 238000007710 freezing Methods 0.000 claims description 5
- 230000008014 freezing Effects 0.000 claims description 5
- 239000011521 glass Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 229910000077 silane Inorganic materials 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 230000008961 swelling Effects 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- AOBIOSPNXBMOAT-UHFFFAOYSA-N 2-[2-(oxiran-2-ylmethoxy)ethoxymethyl]oxirane Chemical compound C1OC1COCCOCC1CO1 AOBIOSPNXBMOAT-UHFFFAOYSA-N 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- 239000003607 modifier Substances 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 3
- 239000011837 N,N-methylenebisacrylamide Substances 0.000 claims description 3
- 238000006243 chemical reaction Methods 0.000 claims description 3
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 3
- 238000002444 silanisation Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 claims description 2
- 239000003960 organic solvent Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 22
- 239000003921 oil Substances 0.000 description 8
- 239000003463 adsorbent Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 230000004048 modification Effects 0.000 description 3
- 238000012986 modification Methods 0.000 description 3
- 238000011084 recovery Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000010842 industrial wastewater Substances 0.000 description 2
- 238000006884 silylation reaction Methods 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 239000004743 Polypropylene Substances 0.000 description 1
- 239000011358 absorbing material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000010170 biological method Methods 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003610 charcoal Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 239000010779 crude oil Substances 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 239000002283 diesel fuel Substances 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229940057995 liquid paraffin Drugs 0.000 description 1
- 244000005700 microbiome Species 0.000 description 1
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 1
- 229920005615 natural polymer Polymers 0.000 description 1
- 238000000053 physical method Methods 0.000 description 1
- -1 polypropylene Polymers 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 239000010902 straw Substances 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
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
-
- 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
- B01J20/28—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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/36—After-treatment
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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
- 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
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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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
- 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
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
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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
- 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
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2201/00—Foams characterised by the foaming process
- C08J2201/04—Foams characterised by the foaming process characterised by the elimination of a liquid or solid component, e.g. precipitation, leaching out, evaporation
- C08J2201/048—Elimination of a frozen liquid phase
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
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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
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A20/00—Water conservation; Efficient water supply; Efficient water use
- Y02A20/20—Controlling water pollution; Waste water treatment
- Y02A20/204—Keeping clear the surface of open water from oil spills
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- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
The invention discloses a preparation method of jute fiber based high-adsorbability hydrophobic cellulose aerogel. The jute used in the invention has wide source and low price. The cellulose content is high. The preparation method has simple process and convenient operation, and the product has excellent hydrophobic property, better adsorbability to oil stains and partial organic solvents and higher economic and social benefits.
Description
Technical Field
The invention relates to the technical field of preparation of aerogel adsorbents, in particular to a preparation method of jute fiber-based high-adsorbability hydrophobic cellulose aerogel.
Background
At present, the problem of floating oil pollution caused by industrial wastewater and oil leakage is receiving more and more attention, and the main problems to be solved are physical methods (floating oil recovery by using adsorbent, combustion agent and mechanical device), chemical methods (floating oil removal by using dispersant and curing agent) and biological methods (floating oil degradation by using natural microorganisms). The floating oil treatment by using the adsorbent is a simple, safe and convenient method. The traditional adsorbents (such as straw, sawdust and charcoal) have the problems of poor selectivity, low adsorption efficiency, unfavorable recovery and the like, while the polymeric adsorbents synthesized by polypropylene fibers and the like have high adsorption capacity, but have high loss of self mass and are unfavorable for recovery and reutilization. Cellulose is the most abundant natural polymer in the world, and has the characteristics of wide source range, low price, natural regeneration, high rigidity, good biocompatibility, degradability and the like, so that the developed cellulose aerogel not only has the characteristics of cellulose, but also has the characteristics of low density and high porosity. The cellulose aerogel is subjected to hydrophobic modification so as to achieve the effect of absorbing oil stains, and more attention is paid. Cellulose aerogels offer unique advantages over a wide variety of oil absorbing materials.
Disclosure of Invention
In order to achieve the purpose, the invention provides a preparation method of jute fiber based high-adsorbability hydrophobic cellulose aerogel.
The invention adopts the following technical scheme:
a preparation method of jute fiber based high adsorption hydrophobic cellulose aerogel is characterized in that: the method comprises the following steps:
firstly, cutting the jute raw material into jute fiber sections with the length of 4cm-5cm, soaking the jute fiber sections in 0.1-0.5wt% of sulfuric acid solution, treating the jute fiber sections for 1-2 hours at the temperature of 60 ℃, and then washing the jute fiber sections to be neutral by using deionized water.
And secondly, treating the cleaned jute fiber with dimethyl sulfoxide (DMSO), reacting for 2-3 hours at the water bath temperature of 80 ℃, washing the jute fiber with distilled water, and drying the sample in a vacuum oven at the drying temperature of 60-80 ℃ for 24 hours to obtain the pretreated jute fiber.
And thirdly, smashing the pretreated jute fiber into powder by a grinder, and sieving the powder by a 60-mesh sieve to obtain the pretreated jute powder. Adding pretreated jute powder into H with certain concentration under the condition of 70-80 deg.C water bath 2 O 2 Treating in NaOH solution for 90-120 min.
Fourthly, carrying out ultrasonic treatment with the power of 50W for 30-50min, and cleaning and drying the treated jute powder at low temperature to obtain jute powder.
Fifthly, weighing 2-5g of jute powder, placing the jute powder in a vacuum drying oven for drying for 24 hours, dissolving the jute powder in a precooled NaOH/urea/water solution at the temperature of-10 ℃ and dissolving the jute powder to obtain a cellulose solution with a certain concentration. Centrifuging at 4000-.
And sixthly, weighing 0.5-1g of cross-linking agent, adding the cross-linking agent into the centrifuged cellulose solution, stirring for 30-60min at room temperature, pouring the mixture into a pore plate, and standing for 4-6 h to obtain the cross-linked cellulose hydrogel.
And seventhly, washing the obtained cellulose hydrogel with deionized water and absolute ethyl alcohol for many times until the hydrogel is in swelling balance and neutral, then placing the hydrogel in a refrigerator with the temperature of-30 ℃ for freezing for 4-6 hours, and obtaining the cellulose aerogel through freeze drying.
And eighthly, placing the obtained aerogel in a sealed dryer, and simultaneously placing an open glass containing 2-4mL of hydrophobic modifier in the dryer, and then sealing the dryer at 50 ℃ for 24 hours to carry out silanization reaction.
And step nine, placing the silanized cellulose aerogel in a vacuum drying oven at normal temperature for 24 hours to remove unreacted silane, thus obtaining the hydrophobic cellulose aerogel.
As a preferable technical solution of the present invention, H in the third step 2 O 2 And NaOH concentrations of 3 to 4wt% and 4 to 5wt%, respectively.
As a preferable aspect of the present invention, the concentration ratio of NaOH/urea/water in the fifth step is 7: 12: 81.
in a preferred embodiment of the present invention, the crosslinking agent in the sixth step is one of N, N-Methylene Bisacrylamide (MBA), polyethylene glycol diglycidyl ether (PEGDE), polyvinyl alcohol (PVA), and glutaraldehyde.
As a preferred embodiment of the present invention, the hydrophobic modifier in the eighth step is one of Methyltrichlorosilane (MTCS), methyltrimethoxysilane (MTMS), and Trimethylchlorosilane (TMCS).
The invention has the beneficial effects that:
the jute fiber-based high-adsorbability hydrophobic cellulose aerogel prepared by the invention has good hydrophobicity, excellent mechanical property and outstanding pore channel structure. The adsorption capacity is large, and the adsorbent can be recycled within a certain range. Has better adsorption capacity on organic matters in crude oil, diesel oil, liquid paraffin and industrial wastewater, including benzene, toluene, normal hexane, cyclohexane and other chemical substances.
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
A preparation method of jute fiber based high-adsorbability hydrophobic cellulose aerogel comprises the following steps:
firstly, cutting a jute raw material into jute fiber sections with the length of 4cm, soaking the jute fiber sections in 0.2wt% of sulfuric acid solution, treating the jute fiber sections at the temperature of 60 ℃ for 1 hour, and then washing the jute fiber sections to be neutral by using deionized water.
And secondly, treating the cleaned jute fiber with dimethyl sulfoxide (DMSO), reacting for 2 hours at the water bath temperature of 80 ℃, washing the jute fiber with distilled water, and drying the sample in a vacuum oven at the drying temperature of 60 ℃ for 24 hours to obtain the pretreated jute fiber.
And thirdly, smashing the pretreated jute fiber into powder by a grinder, and sieving the powder by a 60-mesh sieve to obtain the pretreated jute powder. Adding pretreated jute powder into 3wt% of H under the condition of 70 ℃ water bath 2 O 2 Treatment in 4wt% NaOH solution for 90 min.
Fourthly, then carrying out ultrasonic treatment with the power of 50W for 30min, and cleaning and drying the treated jute powder at low temperature to obtain jute powder.
Fifthly, weighing 4g of jute powder, placing the jute powder in a vacuum drying oven for drying for 24 hours, dissolving the jute powder in a 7wt% NaOH/12wt% urea/81 wt% aqueous solution precooled at the temperature of minus 10 ℃ and dissolving the jute powder to obtain a cellulose solution with a certain concentration. And centrifuging at 4000r/min for 15 minutes to remove insoluble substances and air bubbles in the cellulose solution.
Sixthly, 0.7g of N, N-Methylene Bisacrylamide (MBA) is weighed and added into the centrifuged cellulose solution, stirred for 40min at room temperature, poured into a pore plate and placed for 4 h to obtain the crosslinked cellulose hydrogel.
And seventhly, washing the obtained cellulose hydrogel for multiple times by using deionized water and absolute ethyl alcohol until the hydrogel reaches swelling balance and is neutral, then placing the hydrogel in a refrigerator at the temperature of minus 30 ℃ for freezing for 4 hours, and performing freeze drying to obtain the cellulose aerogel.
In the eighth step, the obtained aerogel was placed in a sealed desiccator while placing an open small glass containing 2mL of Methyltrichlorosilane (MTCS) in the desiccator, and then the desiccator was sealed at 50 ℃ for 24 hours to perform a silylation reaction.
And step nine, placing the silanized cellulose aerogel in a vacuum drying oven at normal temperature for 24 hours to remove unreacted silane, and thus obtaining the hydrophobic cellulose aerogel.
Example 2
A preparation method of jute fiber based high-adsorbability hydrophobic cellulose aerogel comprises the following steps:
firstly, cutting a jute raw material into jute fiber sections with the length of 5cm, soaking the jute fiber sections in 0.3 weight percent of sulfuric acid solution, treating the jute fiber sections for 1.5 hours at the temperature of 60 ℃, and then washing the jute fiber sections to be neutral by using deionized water.
And secondly, treating the cleaned jute fibers with dimethyl sulfoxide (DMSO), reacting for 2.5 hours at the water bath temperature of 80 ℃, washing the jute fibers with distilled water, and drying the sample in a vacuum oven at the drying temperature of 70 ℃ for 24 hours to obtain the pretreated jute fibers.
And thirdly, smashing the pretreated jute fiber into powder by a grinder, and sieving the powder by a 60-mesh sieve to obtain the pretreated jute powder. Under the condition of 75 ℃ water bath, the pretreatedAdding jute powder into 4wt% H with certain concentration 2 O 2 Treatment in 4wt% NaOH solution for 100 min.
And fourthly, performing ultrasonic treatment with the power of 50W for 40min, and cleaning and drying the treated jute powder at low temperature to obtain jute powder.
Fifthly, weighing 5g of jute powder, placing the jute powder in a vacuum drying oven for drying for 24 hours, dissolving the jute powder in a 7wt% NaOH/12wt% urea/81 wt% aqueous solution precooled at the temperature of minus 10 ℃, and dissolving the jute powder to obtain a cellulose solution with a certain concentration. 4500r/min for 10 min to remove insoluble matter and air bubbles from the cellulose solution.
And sixthly, weighing 1g of polyethylene glycol diglycidyl ether (PEGDE) and adding the weighed polyethylene glycol diglycidyl ether (PEGDE) into the centrifuged cellulose solution, stirring the mixture for 50min at room temperature, pouring the mixture into a pore plate, and standing the mixture for 5 hours to obtain the crosslinked cellulose hydrogel.
And seventhly, washing the obtained cellulose hydrogel for multiple times by using deionized water and absolute ethyl alcohol until the hydrogel reaches swelling balance and is neutral, then placing the hydrogel in a refrigerator at the temperature of minus 30 ℃ for freezing for 6 hours, and performing freeze drying to obtain the cellulose aerogel.
Eighthly, the obtained aerogel was placed in a sealed dryer while placing an open glass containing 4mL of Trimethylchlorosilane (TMCS) in the dryer, and then the dryer was sealed at 50 ℃ for 24 hours to perform a silanization reaction.
And step nine, placing the silanized cellulose aerogel in a vacuum drying oven at normal temperature for 24 hours to remove unreacted silane, thus obtaining the hydrophobic cellulose aerogel.
Example 3
A preparation method of jute fiber based high-adsorbability hydrophobic cellulose aerogel comprises the following steps:
firstly, cutting a jute raw material into jute fiber sections with the length of 4cm, soaking the jute fiber sections in 0.5 weight percent of sulfuric acid solution, treating the jute fiber sections at 70 ℃ for 1 hour, and then washing the jute fiber sections to be neutral by using deionized water.
And secondly, treating the cleaned jute fibers with dimethyl sulfoxide (DMSO), reacting for 3 hours at the water bath temperature of 80 ℃, washing the jute fibers with distilled water, and drying the sample in a vacuum oven at the drying temperature of 80 ℃ for 24 hours to obtain the pretreated jute fibers.
And thirdly, smashing the pretreated jute fiber into powder by a grinder, and sieving the powder by a 60-mesh sieve to obtain the pretreated jute powder. Adding pretreated jute powder into 3wt% H with a certain concentration under the condition of 60 deg.C water bath 2 O 2 Treatment in 5wt% NaOH solution for 100 min.
And fourthly, performing ultrasonic treatment with the power of 50W for 50min, and cleaning and drying the treated jute powder at low temperature to obtain jute powder.
Fifthly, weighing 3g of jute powder, placing the jute powder in a vacuum drying oven for drying for 24 hours, dissolving the jute powder in a 7wt% NaOH/12wt% urea/81 wt% aqueous solution precooled at the temperature of minus 10 ℃, and dissolving the jute powder to obtain a cellulose solution with a certain concentration. And centrifuging at 5000r/min for 20min to remove insoluble substances and air bubbles in the cellulose solution.
And sixthly, weighing 0.8g of glutaraldehyde, adding into the centrifuged cellulose solution, stirring at room temperature for 55min, pouring into a pore plate, and standing for 6 h to obtain the crosslinked cellulose hydrogel.
And seventhly, washing the obtained cellulose hydrogel for multiple times by using deionized water and absolute ethyl alcohol until the hydrogel reaches swelling balance and is neutral, then placing the hydrogel in a refrigerator at the temperature of minus 30 ℃ for freezing for 6 hours, and performing freeze drying to obtain the cellulose aerogel.
In the eighth step, the obtained aerogel was placed in a sealed desiccator while placing an open small glass containing 3mL of methyltrimethoxysilane (MTMS) in the desiccator, and then the desiccator was sealed at 50 ℃ for 24 hours to conduct silylation reaction.
And step nine, placing the silanized cellulose aerogel in a vacuum drying oven at normal temperature for 24 hours to remove unreacted silane, and thus obtaining the hydrophobic cellulose aerogel.
Finally, it should be noted that: these embodiments are merely illustrative of the present invention and do not limit the scope of the present invention. In addition, other variations and modifications will be apparent to persons skilled in the art based on the foregoing description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications of the invention may be made without departing from the scope of the invention.
Claims (5)
1. A preparation method of jute fiber based high-adsorbability hydrophobic cellulose aerogel is characterized by comprising the following steps: the method comprises the following steps:
firstly, cutting a jute raw material into jute fiber sections with the length of 4cm-5cm, soaking the jute fiber sections in 0.1-0.5wt% of sulfuric acid solution, treating the jute fiber sections for 1-2 hours at the temperature of 60 ℃, and then washing the jute fiber sections to be neutral by using deionized water;
secondly, treating the cleaned jute fibers with dimethyl sulfoxide (DMSO), reacting for 2-3 hours at the water bath temperature of 80 ℃, washing the jute fibers with distilled water, and drying the sample in a vacuum oven at the drying temperature of 60-80 ℃ for 24 hours to obtain the pretreated jute fibers;
thirdly, crushing the pretreated jute fiber into powder by a crusher, sieving the powder by a 60-mesh sieve to obtain pretreated jute powder, and adding the pretreated jute powder into H with certain concentration under the condition of 70-80 ℃ water bath 2 O 2 Treating in NaOH solution for 90-120 min;
fourthly, then carrying out ultrasonic treatment with the power of 50W for 30-50min, and cleaning and drying the treated jute powder at low temperature to obtain jute powder;
fifthly, weighing 2-5g of jute powder, placing the jute powder in a vacuum drying oven for drying for 24 hours, dissolving the jute powder in a precooled NaOH/urea/water solution at the temperature of-10 ℃ to obtain a cellulose solution with a certain concentration, centrifuging the cellulose solution for 10-20 minutes at the speed of 4000-;
sixthly, weighing 0.5-1g of cross-linking agent, adding the cross-linking agent into the centrifuged cellulose solution, stirring for 30-60min at room temperature, pouring the solution into a pore plate, and standing for 4-6 h to obtain cross-linked cellulose hydrogel;
seventhly, washing the obtained cellulose hydrogel for multiple times by using deionized water and absolute ethyl alcohol until the hydrogel is in swelling balance and neutral, then placing the hydrogel in a refrigerator with the temperature of-30 ℃ for freezing for 4-6 hours, and performing freeze drying to obtain cellulose aerogel;
eighthly, placing the obtained aerogel in a sealed dryer, simultaneously placing an open small glass cup containing 2-4mL of hydrophobic modifier in the dryer, and then sealing the dryer at 50 ℃ for 24 hours to perform silanization reaction;
and step nine, placing the silanized cellulose aerogel in a vacuum drying oven at normal temperature for 24 hours to remove unreacted silane, thus obtaining the hydrophobic cellulose aerogel.
2. The method for preparing jute fiber based high adsorption hydrophobic cellulose aerogel according to claim 1, wherein the method comprises the following steps: h in the third step 2 O 2 And NaOH concentrations of 3 to 4wt% and 4 to 5wt%, respectively.
3. The method for preparing jute fiber based high adsorption hydrophobic cellulose aerogel according to claim 1, wherein the method comprises the following steps: the concentration ratio of NaOH/urea/water in the fifth step is 7: 12: 81.
4. the method for preparing jute fiber based high adsorption hydrophobic cellulose aerogel according to claim 1, wherein: and the cross-linking agent in the sixth step is one of N, N-Methylene Bisacrylamide (MBA), polyethylene glycol diglycidyl ether (PEGDE), polyvinyl alcohol (PVA) and glutaraldehyde.
5. The method for preparing a jute fiber based high adsorption hydrophobic cellulose aerogel according to claim 1, wherein the hydrophobic modifier in the eighth step is one of Methyl Trichlorosilane (MTCS), Methyl Trimethoxysilane (MTMS) and Trimethylchlorosilane (TMCS).
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