CN109180993A - A kind of preparation method of fluorescent nano-fiber element composite aerogel - Google Patents
A kind of preparation method of fluorescent nano-fiber element composite aerogel Download PDFInfo
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- CN109180993A CN109180993A CN201810779682.9A CN201810779682A CN109180993A CN 109180993 A CN109180993 A CN 109180993A CN 201810779682 A CN201810779682 A CN 201810779682A CN 109180993 A CN109180993 A CN 109180993A
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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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- 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
- C08J2205/00—Foams characterised by their properties
- C08J2205/02—Foams characterised by their properties the finished foam itself being a gel or a gel being temporarily formed when processing the foamable composition
- C08J2205/026—Aerogel, i.e. a supercritically dried gel
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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
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/04—Oxycellulose; Hydrocellulose
Abstract
The invention discloses a kind of preparation methods of fluorescent nano-fiber element composite aerogel.Cellulose nanometer fento is extracted by raw material of cotton linter, prepares the cellulose nanometer fento that surface has carboxyl using TEMPO method；The carbon quantum dot of surface amination is prepared using hydrothermal synthesis method.Cellulose nanometer fento is prepared into aeroge by freeze-drying process, the aeroge being prepared is added in amination carbon quantum dot solution again, catalyst carbon quantum dot is chemically grafted on cellulose nanometer fento surface, and composite fluorescence aerogel material is prepared in freeze-drying process.It is low in cost, environmental-friendly, green non-poisonous the invention avoids using using inorganic compound as toxicity brought by aeroge skeleton, and the disadvantages of simple physical doping fluorescent material fluorescent effect does not continue.Product has preferable mechanical property, good fluorescent effect, realizes and carbon quantum dot is grafted to aerogel material surface in the form of covalent bond.
Description
Technical field
The invention belongs to technical field of composite materials, are related to a kind of preparation side of fluorescent nano-fiber element composite aerogel
Method.
Background technique
From cotton, timber, the Nanowire that separation and Extraction comes out in the native cellulose of the biological materials such as stalk and ascidian
Dimension element, according to the difference of its shape characteristic and physical property, mainly include two types: one is the rigidity with Rod-like shape
Cellulose nanocrystal, another kind are the cellulose nanometer fentos with backbone semi-flexible.With numerous inorganic nano-particle phases
Than nano-cellulose has many advantages outstanding, such as from a wealth of sources, cheap, high crystalline and Rod-like shape, Gao Bibiao
Area and rigidity modulus, hypotoxicity, biodegradable, good biocompatibility etc..Wherein, with backbone semi-flexible
Cellulose nanometer fento possesses the draw ratio of superelevation, and elasticity modulus is up to 100Gpa, is good aeroge skeleton source.Mesh
Preceding nano-cellulose is by the close attention of each field scientist, and scientists from all over the world are also in continuous nano-scale cellulose multiple
The application of condensation material and field of functional materials.
Carbon quantum dot is a kind of novel carbon-based zero dimension material, has outstanding optical property, good water-soluble, low toxicity
Property, many advantages, such as environmental-friendly, raw material sources are wide, at low cost, good biocompatibility.With tradition from the mixing of lead, cadmium and silicon
The quantum dot extracted in object is compared, and carbon quantum dot does not relate to during preparation as a kind of novel carbon nanomaterial
And the use of heavy metal, more there are some researchs directly to extract carbon quantum dot, such as egg white, wax gourd from food beverage.In addition, carbon
The chemical inertness of material is higher, because carbon property is stablized, and the heavy content in organism is very high, meanwhile, carbon quantum dot table
The hydrophilic functional group such as many carboxyls on face has excellent dissolubility in water.Therefore compared to metal quantum point material
Material, carbon quantum dot biocompatibility with higher and lower cytotoxicity.
Aeroge is to possess high hole by gel porous material as made from freeze-drying or supercritical carbon dioxide drying
The characteristic of gap rate and extremely-low density is often applied to adsorbent material, heat-barrier material, the application such as functional template.Wherein, fluorescence airsetting
Glue all has application with its special optical property, in many fields, is particularly applied to sensory field.In design fluorescence aeroge
In, the selection of fluorescent light source component and aeroge skeleton component, and be combineding with each other between the two, it is key factor.With fibre
Tieing up plain nanometer fento is the aeroge of skeleton preparation on the basis of possessing the good characteristic of traditional aeroge, there is preferable machinery
Intensity and biocompatibility.Due to the chain entanglement of cellulose nanometer fento height, it can directly pass through freeze-drying or overcritical
Aeroge is prepared in the dry method of carbon dioxide, and density can be down to 0.0046g/cm3, porosity can be 99.7%.And it passes
The fluorescent light source group of system is divided into inorganic-quantum-dot or organic dyestuff.Aeroge skeleton component in combination includes inorganic SiO2With
Organic-biological polymer (cellulose).The introducing of inorganic substances will unavoidably bring toxicity.And to organic-biological polymer
Processing (dissolution) often relates to the use of expensive solvent.On the other hand, between aeroge skeleton component and fluorescent light source component
Interaction be the key that influence the material can stabilized illumination property.Most fluorescence aerogel materials, fluorescent light source component is only
It is simply to adulterate, gentle gel skeleton component physics is compound, will lead to the aggregation of fluorescent components, in conjunction with unstable, to lead
Photoluminescence loss of efficiency, aeroge photoluminescent property do not continue.Utilize organic cellulose nanometer fento composite inorganic carbon quantum
Point is prepared a kind of with emission wavelength, fluorescence efficiency stabilization and high NEW TYPE OF COMPOSITE fluorescence aerogel material, promotion airsetting glue material
The development of material has very important realistic meaning.
Summary of the invention
It is an object of that present invention to provide a kind of preparation methods of fluorescent nano-fiber element aerogel composite, prepare
Journey is low in cost, environmental-friendly, and the fluorescence aeroge prepared has preferable mechanical property, good fluorescent effect.
In order to achieve the above objectives, as follows using technical solution:
A kind of preparation method of fluorescent nano-fiber element composite aerogel, comprising the following steps:
1) it the preparation of cellulose nanometer fento: using cotton linter as raw material, is had using the method preparation surface of TEMPO oxidation
The cellulose nanometer fento of carboxyl；
2) preparation of carbon quantum dot: with citric acid, polyethyleneimine is raw material, prepares surface amino groups using hydrothermal synthesis method
Change carbon quantum dot；
3) preparation of composite aerogel: use freeze-drying method preparation using step 1 gained cellulose nanometer fento as bone
The aeroge of frame is added in step 2 gained surface amination carbon quantum dot solution, utilizes n-hydroxysuccinimide (NHS)
It is that catalyst carbon quantum dot is chemically grafted to 1- (3- dimethylamino-propyl) -3- ethyl-carbodiimide hydrochloride (EDC)
On cellulose nanometer fento surface, after reaction, after repeatedly washing, it is multiple to obtain fluorescent nano-fiber element for freeze-drying again
Close aeroge.
According to the above scheme, TEMPO described in step 1 oxidation method the following steps are included:
Cotton linter is weighed to react at room temperature 12 hours with the sodium hydroxide solution of 2wt% 1:40 in mass ratio；It is resulting
Suspension is dried using Buchner funnel filtering and washing to neutrality；By the cotton linter and tetramethyl piperidine nitrogen oxygen after drying
Compound (TEMPO) is reacted at room temperature with the ratio that sodium bromide and sodium hypochlorite are 100:1.6:10:7.5 in mass ratio, reaction
It is 10.0 that the sodium hydroxide solution that period is 0.5% with mass fraction, which adjusts and keeps reacting solution pH value, reaction to reaction solution
A certain amount of ethyl alcohol is added after pH value is unchanged and terminates reaction, after multiple centrifuge washing, dialysis obtains surface with carboxyl
Cellulose nanometer fento suspension.
According to the above scheme, hydrothermal synthesis method described in step 2 the following steps are included:
It weighs citric acid and is reacted 20 hours for 180 DEG C in hydrothermal reaction kettle with polyethyleneimine 1:10 in mass ratio；It will be anti-
Product dialysis treatment is answered, carbon quantum dot is obtained.
According to the above scheme, it is used in step 3 with the step 1 gained cellulose nanometer fento that mass fraction is 1%~1.5%
Freeze-drying prepares aeroge；Gained aeroge is placed into the step 2 gained carbon quantum dot that mass fraction is 0.1% again
In solution, appropriate n-hydroxysuccinimide (NHS) and 1- (3- dimethylamino-propyl) -3- ethyl-carbodiimide hydrochloride is added
(EDC) catalysis reaction, after reacting 24 hours at room temperature, after washing several times, freeze-drying obtains fluorescent nano-fiber element again
Composite aerogel.
The present invention relates to the modification of cellulose nanometer fento carboxylated, the purpose of technology be to make Cellulose nanocrystal,
There are the reaction site of more chemical graft amination carbon quantum dots, the fluorescence gas that it is prepared in cellulose nanometer fento surface
Gel has higher fluorescence efficiency.
The present invention relates to utilization surface amination carbon quantum dot is prepared with polyethyleneimine, the purpose of technology is to make
The carbon quantum dot surface of preparation makes its carbon quantum dot be grafted to cellulose nanometer fento surface for more free amino group
It is more efficient.
The present invention relates to the chemical graft of fluorescence aeroge, technical purpose is the cellulose nanometer fento and ammonia of carboxylated
The carbon quantum dot of base chemically reacts, and is grafted to carbon quantum dot in the form of covalent bond on cellulose nanometer fento, increases
Add fluorescence aeroge fluorescent effect stability and duration.
The beneficial effect of the present invention compared with the existing technology is:
The present invention using carboxylated cellulose element nanometer fento with amination carbon quantum dot is compound prepares fluorescence aeroge, avoid
Use is using inorganic compound as toxicity brought by aeroge skeleton, and simple physical doping fluorescent material leads to fluorescence
The disadvantages of effect does not continue, has the advantages that low in cost, environmental-friendly, green non-poisonous.Meanwhile the fluorescence aeroge tool prepared
There are preferable mechanical property, good fluorescent effect, realizes and carbon quantum dot is grafted to airsetting glue material in the form of covalent bond
Expect surface.
Specific embodiment
Following embodiment further illustrates technical solution of the present invention, but not as limiting the scope of the invention.
The preparation of cellulose nanometer fento used in embodiment:
The cotton linter for weighing 25g reacts 12 hours at room temperature with the sodium hydroxide solution 1000g that mass fraction is 2%,
After resulting suspension is repeatedly carried out to neutrality using Buchner funnel filtering and washing, it is dried in drying box；It will
10g cotton linter after drying is added in 500ml distilled water, smashs 5min to pieces using bruisher, after filtering gained cotton linter again
It is added in 800ml distilled water；0.16g tetramethyl piperidine nitrogen oxides (TEMPO) is weighed, 1.0g sodium bromide is dissolved into 80ml steaming
In distilled water, it is added drop-wise in cotton linter dropwise；The liquor natrii hypochloritis that 51.3g mass fraction is 14.5% is weighed, is added drop-wise to dropwise
In cotton linter, mechanical stirring, is adjusted with the sodium hydroxide solution that mass fraction is 0.5% during reaction and keeps reactant at room temperature
The pH value of system is 10.0, after the pH value in reaction system does not change, 50ml dehydrated alcohol is added and terminates reaction.It will reaction
It suspension centrifugation washing 3 times, is placed in bruisher and smashs 30min to pieces, dialyse 5 days, obtain the cellulose nanometer that surface has carboxyl
Fento.
The preparation of carbon quantum dot used in embodiment:
0.1g anhydrous citric acid is weighed, 0.945g polyethyleneimine is dissolved into 30ml distilled water, and above-mentioned solution is shifted
Into 50ml hydrothermal reaction kettle, at 180 DEG C, reacts 20 hours, acquired solution is dialysed 3 days after reaction, obtains surface
Amination carbon quantum dot.
Embodiment 1
The amination carbon quantum solution 100ml that mass fraction is 0.1% is prepared, 8mgN- hydroxysuccinimidyl is added in the solution
Acid imide (NHS) and 10mg 1- (3- dimethylamino-propyl) -3- ethyl-carbodiimide hydrochloride (EDC), by above-mentioned solution point four
Part is added in four 25ml vials；Take four 15mm (diameter) × 17mm (height) cylindrical fibre element nanometer fento airsetting
Glue is sequentially placed in vial, at room temperature, vial is placed in constant-temperature table and rocks reaction for 24 hours.After reaction, will
Aeroge takes out, and the cleaning solution unstressed configuration effect repeatedly washed through distilled water obtains fluorescence using freeze-drying process 48h and receives
Rice cellulose composite aerogel.
Embodiment 2
Present embodiment unlike the first embodiment in step 1 mass fraction of amination carbon quantum dot solution than adjustment
It is 0.2%, other steps and parameter are consistent with embodiment 1.
Embodiment 3
Present embodiment unlike the first embodiment in step 1 mass fraction of amination carbon quantum dot solution than adjustment
It is 0.5%, other steps and parameter are consistent with embodiment 2.
Embodiment 4
Present embodiment unlike the first embodiment in step 1 mass fraction of amination carbon quantum dot solution than adjustment
It is 1.0%, other steps and parameter are consistent with embodiment 3.
Comparative example
A kind of cellulose nanometer fento prepares aerogel material, is prepared via a method which to obtain:
Distilled water 100ml is taken, 8mg n-hydroxysuccinimide (NHS) and 10mg 1- (3- diformazan ammonia are added in the solution
Base propyl) -3- ethyl-carbodiimide hydrochloride (EDC), above-mentioned solution point is added in four 25ml vials for four parts；Take four
A 15mm (diameter) × 17mm (height) cylindrical fibre element nanometer fento aeroge is sequentially placed in vial, in room temperature
Under, vial is placed in constant-temperature table and rocks reaction for 24 hours.After reaction, aeroge is taken out, is repeatedly washed through distilled water
Cleaning solution unstressed configuration effect, obtain composite fluorescence aeroge by freeze-drying process 48h.
The fluorescence aeroge for taking carbon quantum dot solution, cellulose nanometer fento suspension obtained by the present invention, embodiment 4 to prepare
The suspension being dispersed in water, by the comparison in the case where natural light and wavelength are 365nm ultraviolet light it can be seen that, carbon quantum dot and point
It dissipates fluorescence aeroge in water and all shows good fluorescent effect in the case where wavelength is 365nm ultraviolet light, and cellulose nanometer
Fento wavelength is unstressed configuration effect under 365nm ultraviolet light.Illustrate successfully to be grafted carbon quantum dot on cellulose nanometer fento, and
Fluorescent effect is good.
Example 1,2,3,4 and the aeroge of comparative example preparation are right in the case where natural light and wavelength are 365nm ultraviolet light
Than that can obtain, aeroge prepared by the comparative example 1 unstressed configuration effect under ultraviolet light, and airsetting prepared by embodiment 1,2,3,4
Glue has good fluorescent effect, and with the increase of carbon quantum dot solution concentration, the fluorescent effect of aeroge also enhances therewith.
Claims (4)
1. a kind of preparation method of fluorescent nano-fiber element composite aerogel, it is characterised in that the following steps are included:
1) using cotton linter as raw material, carboxyl the preparation of cellulose nanometer fento: is had using the method preparation surface of TEMPO oxidation
Cellulose nanometer fento；
2) preparation of carbon quantum dot: with citric acid, polyethyleneimine is raw material, prepares surface amination carbon using hydrothermal synthesis method
Quantum dot；
3) preparation of composite aerogel: use freeze-drying method preparation using step 1 gained cellulose nanometer fento as skeleton
Aeroge is added in step 2 gained surface amination carbon quantum dot solution, utilizes n-hydroxysuccinimide and 1- (3- bis-
Methylaminopropyl) -3- ethyl-carbodiimide hydrochloride be catalyst carbon quantum dot be chemically grafted to cellulose nanometer fento
On surface, after reaction, after repeatedly washing, freeze-drying obtains fluorescent nano-fiber element composite aerogel again.
2. the preparation method of fluorescent nano-fiber element composite aerogel as described in claim 1, it is characterised in that described in step 1
TEMPO oxidation method the following steps are included:
Cotton linter is weighed to react at room temperature 12 hours with the sodium hydroxide solution of 2wt% 1:40 in mass ratio；Resulting suspension
Liquid is dried using Buchner funnel filtering and washing to neutrality；By the cotton linter and tetramethyl piperidine nitrogen oxides after drying
It reacts with the ratio that sodium bromide and sodium hypochlorite are 100:1.6:10:7.5 in mass ratio, is used during reaction at room temperature
It is 10.0 that the sodium hydroxide solution of 0.5wt%, which adjusts solution ph, and reaction is whole to the unchanged rear a certain amount of ethyl alcohol of addition of pH value
It only reacts, after multiple centrifuge washing, dialysis obtains the cellulose nanometer fento suspension that surface has carboxyl.
3. the preparation method of fluorescent nano-fiber element composite aerogel as described in claim 1, it is characterised in that water described in step 2
Thermal synthesis method the following steps are included:
It weighs citric acid and is reacted 20 hours for 180 DEG C in hydrothermal reaction kettle with polyethyleneimine 1:10 in mass ratio；Reaction is produced
Object dialysis treatment, obtains carbon quantum dot.
4. the preparation method of fluorescent nano-fiber element composite aerogel as described in claim 1, it is with mass fraction in step 3
1%~1.5% step 1 gained cellulose nanometer fento prepares aeroge using freeze-drying；Again by gained aeroge
It is placed into the step 2 gained carbon quantum dot solution that mass fraction is 0.1%, appropriate n-hydroxysuccinimide and 1- is added
(3- dimethylamino-propyl) -3- ethyl-carbodiimide hydrochloride catalysis reaction, after reacting 24 hours at room temperature, through multiple water
It washes, freeze-drying obtains fluorescent nano-fiber element composite aerogel again.
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Cited By (8)
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| CN113318070A (en) * | 2021-05-25 | 2021-08-31 | 上海交通大学 | Injectable hydrogel and preparation and application thereof |
| CN113600154A (en) * | 2021-09-13 | 2021-11-05 | 石河子大学 | 3D network structure cellulose-based hydrogel and preparation method and application thereof |
| CN113929971A (en) * | 2021-10-11 | 2022-01-14 | 武汉工程大学 | Solid-phase blending inorganic filler and preparation method and application thereof |
| CN114921241A (en) * | 2022-04-14 | 2022-08-19 | 新疆农业大学 | Preparation method and application of manganese-containing complex cellulose-based fluorescent functional material |
| CN114931907A (en) * | 2022-04-11 | 2022-08-23 | 武汉工程大学 | MXene, conductive polymer and plant cellulose composite aerogel and preparation method and application thereof |
| CN115108822A (en) * | 2022-07-14 | 2022-09-27 | 南京工业大学 | Photo-thermal regulation ceramic nanofiber reinforced ZnAl 2 O 4 :Eu 3+ Method for producing aerogels |
| CN115584626A (en) * | 2022-09-30 | 2023-01-10 | 武汉工程大学 | Carbon dot modified fluorescent fiber and preparation method thereof |
| CN115625948A (en) * | 2022-09-30 | 2023-01-20 | 武汉工程大学 | Carbon dot modified fluorescent fiber composite anti-counterfeiting film material and preparation method thereof |
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| CN113318070A (en) * | 2021-05-25 | 2021-08-31 | 上海交通大学 | Injectable hydrogel and preparation and application thereof |
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| CN114931907A (en) * | 2022-04-11 | 2022-08-23 | 武汉工程大学 | MXene, conductive polymer and plant cellulose composite aerogel and preparation method and application thereof |
| CN114921241A (en) * | 2022-04-14 | 2022-08-19 | 新疆农业大学 | Preparation method and application of manganese-containing complex cellulose-based fluorescent functional material |
| CN115108822A (en) * | 2022-07-14 | 2022-09-27 | 南京工业大学 | Photo-thermal regulation ceramic nanofiber reinforced ZnAl 2 O 4 :Eu 3+ Method for producing aerogels |
| CN115584626A (en) * | 2022-09-30 | 2023-01-10 | 武汉工程大学 | Carbon dot modified fluorescent fiber and preparation method thereof |
| CN115625948A (en) * | 2022-09-30 | 2023-01-20 | 武汉工程大学 | Carbon dot modified fluorescent fiber composite anti-counterfeiting film material and preparation method thereof |
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Application publication date: 20190111 |