CN105566673A - Preparation method of multifunctional cellulose elastic aerogel - Google Patents

Preparation method of multifunctional cellulose elastic aerogel Download PDF

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Publication number
CN105566673A
CN105566673A CN201510948650.3A CN201510948650A CN105566673A CN 105566673 A CN105566673 A CN 105566673A CN 201510948650 A CN201510948650 A CN 201510948650A CN 105566673 A CN105566673 A CN 105566673A
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cellulose
aerogel
preparation
silane
modified
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CN105566673B (en
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张俊平
李凌霄
李步成
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Lanzhou Institute of Chemical Physics LICP of CAS
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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
    • 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
    • C08J3/00—Processes of treating or compounding macromolecular substances
    • C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
    • 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
    • C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
    • C08J2301/02—Cellulose; Modified cellulose

Abstract

The invention discloses a preparation method of a multifunctional cellulose elastic aerogel, belonging to the field of aerogel materials. The preparation method comprises the following steps: dispersing cellulose in water, carrying out pretreatment by adding sodium chlorite or/and in a solvothermal way, and cleaning with deionized water to obtain a purified cellulose dispersion solution; adding a modifier to perform chemical modification, thereby obtaining a modified cellulose suspension; dispersing the modified cellulose suspension in an organic solvent, forming, drying to form a modified cellulose gel, and finally, carrying out heat treatment on the modified cellulose gel to obtain the multifunctional cellulose elastic aerogel. The cellulose is subjected to pretreatment and chemical modification, thereby lowering the density of the aerogel, greatly enhancing the elasticity and mechanical strength of the aerogel, endowing the aerogel with excellent magnetism, electric conductivity, superhydrophobicity, superoleophobicity and many other functions, and widening the application range of the traditional cellulose aerogel.

Description

A kind of preparation method of multifunctional fibre element elasticity aerogel
Technical field
The present invention relates to a kind of preparation of cellulose aerogels, particularly relate to the preparation method of a kind of multifunctional fibre element elasticity aerogel, belong to aerogel material field.
Background technology
Mierocrystalline cellulose is renewable, degradable, is present in the environmental protection natural polysaccharide macro-molecular of occurring in nature, is widely used in the fields such as food, building, weaving.Cellulose aerogels, as three-dimensional porous material, while remaining traditional aerogel performance, also has himself excellent characteristic.Therefore, cellulose aerogels gets the attention.In patent CN103205015B, take ionic liquid as solvent, by cellulose dissolution deaeration, then regenerate in ionic liquid aqueous solution or the precipitation bath of ionic liquid alcoholic solution, through solvent exchange, more namely obtain cellulose aerogels by supercritical drying.In patent CN201410354796, be raw material with cellulosetri-acetate, add 1,4-dioxane, absolute alcohol kind solvent be abundant dispersed with stirring also, and then in injection moulding mould, Temperature fall forms wet gel, remove desolventizing through supercritical drying again, obtain cellulosetri-acetate aerogel.But, above-mentioned cellulose aerogels mainly utilize the hydrogen bond action of cellulosic molecule in microtexture interlink formed reticulated structure, wherein part hydrogen bond cannot complete effective hydrogen bond action.Therefore, there are the problems such as nonelastic and physical strength is low in most of cellulose aerogels.
In recent years, got the attention by the aspect of performance that composition is improving cellulose aerogels of adjustment preparation method and reaction mass.In patent CN103709435A, by the cellulose solution prepared after freezing-solution melts circulation for several times, join in acidic solution and carry out cellulose solution displacement, then obtain light-high-strength cellulose aerogels by drying.In patent CN103756006A, by the Mierocrystalline cellulose dispersion liquid of obtained nanofibrils, carry out gelation and lyophilize process, then drip hydrophobic modifier and obtain hydrophobicity cellulose aerogel.In patent CN103980530A, with seaweed fiber element for raw material, through purifying, mechanical glue mill, lyophilize, obtain cellulose aerogels, then by phenyltrimethoxysila,e, the cellulose aerogels that hydrophobically modified obtains can be used for oil suction is carried out to it.Although the preparation of cellulose aerogels is through certain improvement, but still there is preparation method's complexity in above-mentioned technology, cost is higher, and obtained cellulose aerogels function singleness, mechanical property still need the problems such as improvement further, and these deficiencies greatly limit the application of cellulose aerogels.Therefore, the elasticity of cellulose aerogels and multifunction are this field problems in the urgent need to address.
Summary of the invention
The object of this invention is to provide the preparation method of a kind of multifunctional fibre element elasticity aerogel, with the problem such as solve that existing cellulose aerogels is nonelastic, physical strength is low and preparation method is complicated.
The preparation of multifunctional fibre element elasticity aerogel of the present invention, comprises by following processing step:
(1) cellulosic pre-treatment: be scattered in by Mierocrystalline cellulose in water, adds Textone and carries out pre-treatment or/and adopt solvent thermal to carry out pre-treatment, clean, obtain the purifying cellulose dispersion liquid of concentration 0.01 ~ 100g/mL with deionized water.
Described Mierocrystalline cellulose comprises the vegetable fibres such as cotton fibre, bombax cotton, poplar (willow) wadding, bamboo fibers, timber, coconut husk, stalk, bagasse and sunflower stalk, the modified-celluloses such as Microcrystalline Cellulose, carboxymethyl cellulose and nano-cellulose, bacteria cellulose, seaweed fiber element and the regenerated cellulose prepared by waste paper, carton, newspaper etc.
Described Textone process is under acidic or neutral conditions, in 25 ~ 100 DEG C of process 0.5 ~ 4h; The consumption of Textone is 0.01 ~ 0.05g/mL.
Described solvent heat treatment is in water, ethanol or methyl alcohol, processes 1 ~ 48h at 80 ~ 230 DEG C.
(2) cellulosic chemically modified: the properties-correcting agent adding Mierocrystalline cellulose quality 0.25% ~ 50% in purifying cellulose dispersion liquid, reacts 1 ~ 48h, obtains modified-cellulose suspension at 25 ~ 230 DEG C.
Described properties-correcting agent is at least one in organosilane, iron(ic) chloride, Dopamine HCL, carbon nanotube, graphene oxide, Z 250, trimeric cyanamide, silicon-dioxide, montmorillonite, attapulgite, sepiolite, halloysite, hydrotalcite, vermiculite, mica, kaolinite, hectorite.
Described organosilane is methylethyl diethoxy silane, methylvinyldimethoxysilane, γ-aminopropyltriethoxy diethoxy silane, dodecyltrimethoxysilane, propyl-triethoxysilicane, 3-chloropropyl triethoxysilane, urea propyl-triethoxysilicane, phenyltrimethoxysila,e, phenyl triethoxysilane, n-octytriethoxysilane, vinyltrimethoxy silane, allyltriethoxysilane, propyl trimethoxy silicane, vinyl three (2-methoxy ethoxy) silane, 3-aminopropyl trimethoxysilane, methyltrimethoxy silane, 3-r-chloropropyl trimethoxyl silane, Union carbide A-162, trifluoro propane Trimethoxy silane, perfluoro capryl Trimethoxy silane, perfluoro capryl triethoxyl silane, perfluoro decyl Trimethoxy silane, perfluoro decyl triethoxyl silane, perfluoro capryl dimethyl methoxy silane, at least one in perfluoro decyl dimethyl methoxy silane.
Described pre-treatment and chemically modified can be carried out successively.But consider Simplified flowsheet and cost, pre-treatment and chemically modified also can be carried out simultaneously.
(3) preparation of Multifunctional elastic aerogel: by the dispersion of modified-cellulose suspension in organic solvent, shaping by suction filtration, dries at 25 ~ 120 DEG C of normal pressures, makes modified-cellulose gel; Finally modified-cellulose gel is processed 1 ~ 24h at 80 ~ 1200 DEG C, i.e. obtained Multifunctional elastic aerogel.
Described organic solvent is at least one in ethanol, methyl alcohol, acetone.
The present invention obtains beneficial effect: by carrying out pre-treatment to Mierocrystalline cellulose, removes the impurity in raw material and reduces its density, making the reactive group of cellulose surface activate simultaneously; By different properties-correcting agent, chemically modified is carried out to Mierocrystalline cellulose, give Mierocrystalline cellulose various new performance; Cellulosic pre-treatment and chemically modified, not only reduce the density of aerogel, and also substantially increase elasticity and the physical strength of aerogel, its density is less than 20mg/cm 3, the shrinking percentage compressing 1000 times is less than 15%.By selecting suitable low boiling point solvent to disperse modified-cellulose, reduce the contraction of cellulose aerogels in normal pressure drying course; Realize heat cross-linking and the carbonization of modified-cellulose gel finally by thermal treatment, obtain the elasticity aerogel with several functions such as excellent magnetic, electroconductibility, super-hydrophobicity and super oleophobic properties, extend the range of application of traditional fibre element aerogel.
Embodiment
Be described further below by the preparation and property of specific embodiment to multifunctional fibre element elasticity aerogel of the present invention.
Embodiment 1
Take sugarcane waste residue 10g, after adding the immersion of 1L deionized water, broken, mechanical stirring 3h, makes the cellulose suspension of 0.01g/mL; Get 300mL cellulose suspension, be placed in 500mL round-bottomed flask, add 4g Textone and 1.2mL acetic acid, at 75 DEG C, mechanical stirring 3h carries out pre-treatment, cleans, obtain modified-cellulose suspension with deionized water; Then disperseed in ethanol, vacuum filtration is shaping, dry at 60 DEG C, forms cellulose gel; Finally by cellulose gel at N 2the lower 800 DEG C of carbonization 4h of atmosphere, obtain Multifunctional elastic cellulose aerogels.Performance is in table 1.
Embodiment 2
Take cotton fibre 7g, through fragmentation, be placed in 500mL round-bottomed flask, add 400mL deionized water, 1g Textone and 0.3mL acetic acid, at 80 DEG C, mechanical stirring 2.5h carries out pre-treatment, cleans, obtain modified-cellulose suspension with deionized water; Then disperseed in acetone, vacuum filtration is shaping, dry at 60 DEG C, forms cellulose gel; Finally by cellulose gel at N 2the lower 1000 DEG C of carbonization 3h of atmosphere, obtain Multifunctional elastic cellulose aerogels.Performance is in table 1.
Embodiment 3
Take nano-cellulose 20g, add 400mL deionized water, mechanical stirring 2h, make 0.05g/mL purifying cellulose suspension; Take 0.4gFe 3o 4nanoparticle, joins in 250mL polytetrafluoro hydro-thermal tank; Measuring 120mL purifying cellulose suspension joins in polytetrafluoro hydro-thermal tank, and magnetic agitation 10min, ultrasonic 30min, react 8h at 160 DEG C, obtains Mierocrystalline cellulose/ferriferrous oxide nano composite suspension liquid; Then disperseed in acetone, suction filtration is shaping, dry at 60 DEG C, forms Mierocrystalline cellulose/ferriferrous oxide nano plural gel; Finally by plural gel at N 2the lower 800 DEG C of carbonization 2h of atmosphere, obtain Multifunctional elastic cellulose aerogels.Performance is in table 1.
Embodiment 4
Take seaweed fiber element 25g, after adding the immersion of 500mL deionized water, mechanical stirring 3h, makes 0.05g/mL purifying cellulose suspension; Measure the cellulose suspension of 62mL purifying and the acetic acid of 10.5mL10mM, join in 100mL Erlenmeyer flask, magnetic agitation 10min, ultrasonic 30min; Take 0.35g poloxamer F127,2g urea, 0.6g urea propyl-triethoxysilicane and 0.9g γ-aminopropyltriethoxy diethoxy silane again, magnetic agitation 1h, obtain Mierocrystalline cellulose/silane composite suspension liquid; Then at 80 DEG C, react 16h, with deionized water and ethanol purge, in the ethanolic soln of 1% perfluoro capryl Trimethoxy silane, soak 6h(afterwards again reduce surface energy), dry at 60 DEG C, obtain Multifunctional elastic cellulose aerogels.Performance is in table 1.
Embodiment 5
Take bamboo fibers 30g, after adding the immersion of 1L deionized water, through broken, mechanical stirring 3h, make 0.03/gmL cellulose suspension; Get 400mL cellulose suspension and be placed in 500mL round-bottomed flask, add 2g Textone and 0.6mL acetic acid, at 80 DEG C, mechanical stirring 2h carries out pre-treatment, cleans with deionized water, obtains the cellulose suspension of purifying; Take 0.5gSiO 2nanoparticle, joins in 100mL Erlenmeyer flask, and measure 65mL purifying cellulose suspension and join in Erlenmeyer flask, magnetic agitation 10min, ultrasonic 30min, react 8h at 25 DEG C, obtains Mierocrystalline cellulose/silica nanometer composite suspension liquid; Then be dispersed in methyl alcohol, suction filtration is shaping, dry at 60 DEG C, forms Mierocrystalline cellulose/silica nanometer plural gel; Finally by plural gel at N 2the lower 1000 DEG C of carbonization 4h of atmosphere, obtain Multifunctional elastic cellulose aerogels.Performance is in table 1.
Embodiment 6
Take straw refuse 20g, after adding the immersion of 600mL deionized water, through broken, mechanical stirring 3h, make 0.03g/mL cellulose suspension; Get 200mL cellulose suspension and be placed in 500mL round-bottomed flask, add 3g Textone and 0.9mL acetic acid, at 85 DEG C, mechanical stirring 2h carries out pre-treatment, cleans with deionized water, obtains the cellulose suspension of purifying; Measure the cellulose suspension of 45mL purifying and the acetic acid of 3.5mL10mM respectively, join in 100mL Erlenmeyer flask, magnetic agitation 10min, ultrasonic 30min, add 0.15g Sodium dodecylbenzene sulfonate, 2.8g urea, 0.2g n-octytriethoxysilane and 0.3g phenyltrimethoxysila,e again, magnetic agitation 1h, obtains Mierocrystalline cellulose/silane composite suspension liquid; Then at 85 DEG C, 12h is reacted, with deionized water and ethanol purge, dry at 60 DEG C, obtain Multifunctional elastic cellulose aerogels.Performance is in table 1.
Embodiment 7
Take coconut husk 25g, after adding the immersion of 700mL deionized water, through broken, mechanical stirring 3h, make 0.036g/mL cellulose suspension; Get 400mL cellulose suspension, be placed in 500mL round-bottomed flask, add 3g Textone and 0.9mL acetic acid, at 80 DEG C, mechanical stirring 2.5h carries out pre-treatment, cleans with deionized water, obtains the cellulose suspension of purifying.Taking 0.4g diameter is 40-60nm multi-walled carbon nano-tubes, joins in 100mL Erlenmeyer flask, then measures the cellulose suspension of 50mL purifying, magnetic agitation 10min, ultrasonic 30min, at 180 DEG C of reaction water thermal response 12h, obtains cellulose/carbon nano composite suspension liquid.Then disperseed in ethanol, vacuum filtration, at 60 DEG C after drying, formed cellulose/carbon nano plural gel, finally by sample at N 2the lower 1100 DEG C of carbonization 2h of atmosphere, soak 8h(afterwards again and reduce surface energy in the ethanolic soln of 1% perfluoro decyl triethoxyl silane), obtain Multifunctional elastic cellulose aerogels.Performance is in table 1.
Embodiment 8
Take kapok 15g, through fragmentation, be placed in 250mL polytetrafluoro hydro-thermal tank, add 200mL ethylene glycol, 1g iron(ic) chloride and 10g polyoxyethylene glycol, at 200 DEG C after hydro-thermal reaction 24h, clean with deionized water, obtain the magnetic cellulose suspension of purifying; Take 1.5g attapulgite, join in 100mL Erlenmeyer flask, the magnetic cellulose suspension measuring 50mL purifying again joins in Erlenmeyer flask, ultrasonic 30min, at 25 DEG C, react 12h, obtain magnetic cellulose/attapulgite composite suspension liquid, suction filtration is shaping, at 60 DEG C after drying, form magnetic cellulose/attapulgite plural gel; Finally by plural gel at N 2the lower 1000 DEG C of carbonization 4h of atmosphere, obtain Multifunctional elastic cellulose aerogels.Performance is in table 1.

Claims (10)

1. a preparation method for multifunctional fibre element elasticity aerogel, is first scattered in water by Mierocrystalline cellulose, adds Textone and carries out pre-treatment or/and adopt solvent thermal to carry out pre-treatment, clean, obtain the Mierocrystalline cellulose dispersion liquid of purifying with deionized water; Add properties-correcting agent again to carry out chemically modified and obtain modified-cellulose suspension; Then by the dispersion of modified-cellulose suspension in organic solvent, by shaping, dry, form modified-cellulose gel, finally modified-cellulose gel is obtained Multifunctional elastic aerogel by thermal treatment.
2. the preparation method of multifunctional fibre element elasticity aerogel as claimed in claim 1, is characterized in that: described Mierocrystalline cellulose is vegetable fibre, modified-cellulose, regenerated cellulose.
3. the preparation method of multifunctional fibre element elasticity aerogel as claimed in claim 1, it is characterized in that: the pre-treatment of described employing Textone is: the add-on of Textone is 0.01 ~ 0.05g/mL, at acid or neutrallty condition, at temperature 25 ~ 100 DEG C, process 0.5 ~ 4h.
4. the preparation method of multifunctional fibre element elasticity aerogel as claimed in claim 1, is characterized in that: described solvent thermal pretreatment technology is: in water, ethanol or methyl alcohol, processes 1 ~ 48h at temperature 80 ~ 230 DEG C.
5. the preparation method of multifunctional fibre element elasticity aerogel as claimed in claim 1, is characterized in that: the properties-correcting agent that described chemically modified adopts is at least one in organosilane, iron(ic) chloride, Dopamine HCL, carbon nanotube, graphene oxide, Z 250, trimeric cyanamide, silicon-dioxide, montmorillonite, attapulgite, sepiolite, halloysite, hydrotalcite, vermiculite, mica, kaolinite, hectorite; The consumption of properties-correcting agent is 0.25% ~ 50% of Mierocrystalline cellulose quality.
6. the preparation method of multifunctional fibre element elasticity aerogel as claimed in claim 5, is characterized in that: described organosilane is methylethyl diethoxy silane, methylvinyldimethoxysilane, γ-aminopropyltriethoxy diethoxy silane, dodecyltrimethoxysilane, propyl-triethoxysilicane, 3-chloropropyl triethoxysilane, urea propyl-triethoxysilicane, phenyltrimethoxysila,e, phenyl triethoxysilane, n-octytriethoxysilane, vinyltrimethoxy silane, allyltriethoxysilane, propyl trimethoxy silicane, vinyl three (2-methoxy ethoxy) silane, 3-aminopropyl trimethoxysilane, methyltrimethoxy silane, 3-r-chloropropyl trimethoxyl silane, Union carbide A-162, trifluoro propane Trimethoxy silane, perfluoro capryl Trimethoxy silane, perfluoro capryl triethoxyl silane, perfluoro decyl Trimethoxy silane, perfluoro decyl triethoxyl silane, perfluoro capryl dimethyl methoxy silane, at least one in perfluoro decyl dimethyl methoxy silane.
7. the preparation method of multifunctional fibre element elasticity aerogel as claimed in claim 1, is characterized in that: the organic solvent of disperse modified cellulose suspension is at least one in ethanol, methyl alcohol, acetone.
8. the preparation method of multifunctional fibre element elasticity aerogel as claimed in claim 1, is characterized in that: the shaping of described modified-cellulose gel is shaping by suction filtration, dries and obtain at 25 ~ 120 DEG C of normal pressures.
9. the preparation method of multifunctional fibre element elasticity aerogel as claimed in claim 1, is characterized in that: the thermal treatment of described modified-cellulose gel is: at 80 ~ 1200 DEG C of reaction 1 ~ 24h.
10. the preparation method of multifunctional fibre element elasticity aerogel as claimed in claim 1, is characterized in that: described cellulosic pre-treatment and chemically modified are carried out simultaneously.
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CN106118301A (en) * 2016-07-18 2016-11-16 阜南县大自然工艺品有限公司 A kind of wood artwork water paint containing super-hydrophobic multiple cellulose acetate nanofiber and preparation method thereof
CN106432783A (en) * 2016-09-20 2017-02-22 东华大学 Cellulose/organic silicon/dopamine flame-retardant thermal-insulating aerogel and preparation method thereof
CN106517144A (en) * 2016-11-15 2017-03-22 中国科学技术大学 Method for preparing carbon nanofiber aerogel from wood
CN106732214A (en) * 2016-12-28 2017-05-31 淮阴工学院 A kind of hydrophobicity natural polymer/attapulgite composite aerogel and preparation method thereof
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CN106517144B (en) * 2016-11-15 2018-10-23 中国科学技术大学 A method of carbon nano-fiber aeroge is prepared by timber
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