CN106432783A - Cellulose/organic silicon/dopamine flame-retardant thermal-insulating aerogel and preparation method thereof - Google Patents
Cellulose/organic silicon/dopamine flame-retardant thermal-insulating aerogel and preparation method thereof Download PDFInfo
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- 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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- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
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- 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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Abstract
The invention relates to cellulose/organic silicon/dopamine flame-retardant thermal-insulating aerogel and a preparation method thereof. The dopamine accounts for 5-20wt% of the mass of the aerogel; the mass ratio of organic silicon to the cellulose is (0.5:1)-(3:1); and the cellulose is cellulose micron wires or cellulose nano wires. The preparation method comprises the following steps: adding the organic silicon into a cellulose micron/nano suspension, stirring, adding the dopamine, adjusting the pH value to be 8-9, and stirring so as to obtain a suspension; and putting the suspension into liquid nitrogen for freezing so as to obtain frozen gel, performing freeze-drying, and baking, thereby obtaining the cellulose/organic silicon/dopamine flame-retardant thermal-insulating aerogel. In addition to excellent flame retardancy and thermal insulation, the cellulose/organic silicon/dopamine flame-retardant thermal-insulating aerogel provided by the invention is further good in mechanical property, is capable of meeting requirements of ecological environment protection, and moreover has good application prospects in fields such as thermal-insulating materials of buildings and pipelines, and thermal-insulating coverall fillers.
Description
Technical field
The invention belongs to aeroge and preparation field thereof, particularly to a kind of cellulose/organosilicon/dopamine anti-flaming thermal-insulation
Aeroge and preparation method thereof.
Background technology
Aeroge is gel through supercritical drying or freeze-drying the liquid gas that it is internal replaced and
A kind of three-dimensional porous material generating.This material has that density is little, specific surface area is big and the advantage such as thermal conductivity factor is little, by extensively
It is applied to heat-barrier material, active matter carrier and inductor etc..Traditional aeroge be inorganic aerogels with silicon as representative with
And the organic aerogel as representative is studied widely by people with resorcin/formaldehyde and melamine/formaldehyde.Cellulose
Aeroge as newborn third generation material, is possessing that tradition is inorganic and is incorporating the excellent of cellulose while organic aerogel
Performance, such as abundance, degradable and biocompatibility, have huge latent in following heat-barrier material and bio-medical
Power, and cellulose aerogels can be used to prepare carbon aerogels through pyrolysis and leads for environmental protection and electrochemical energy storage etc.
Territory.
Cellulose is utilized to prepare the research of aeroge, the in recent years extensive concern by researchers for raw material, mainly
Realized the preparation of cellulose aerogels by two approach：One be cellulose through NaOH/urea liquid at low temperature bar
After dissolving under part, then obtain aeroge through the regeneration generation last freeze-drying of cellulose aquagel of weak acid solution；Two is cellulose
Fiber is transformed into the nanowire suspended liquid of cellulose through mechanical stripping or by TEMPO/NaBr/NaClO mechanical stripping again, then
Obtain cellulose aerogels through freezing and freeze-drying.But the fire resistance of cellulose aerogels and mechanical performance are poor.
Silane generates silicone hydroxyl through hydrolysis and carrys out reinforcing fiber element with the hydroxyl of cellulose surface by hydrogen bond and chemical bond interaction
The rigidity of fiber.Therefore may utilize the mechanical performance that silane carrys out reinforcing fiber cellulose fiber.Silicon is conventional in flame-proof treatment simultaneously
A kind of environmentally friendly fire retardant, can be improved the heat endurance of cellulose aerogels by introducing silane.
Dopamine is paid close attention to widely due to its bio-compatible, nontoxic and strong adhesion property.Nearest researcher sends out
The catechol of existing dopamine has very strong radical-scavenging ability.So radical-scavenging ability and the silicon of dopamine can be used
The performance of the catalytic cellulose carbonization of alkane combines, and improves the fire resistance of cellulose aerogels.
Content of the invention
The technical problem to be solved is to provide a kind of cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge
And preparation method thereof, the cellulose that the method nature is widely present is raw material, utilizes organosilicon and dopamine modified fibre
Usually improve its mechanical performance and fire resistance；The aeroge obtaining has good mechanical properties, lower thermal conductivity and excellent resistance
Combustion performance, possesses good application prospect in fields such as building, the heat-barrier material of pipeline and proximity suit fillers.
A kind of cellulose/organosilicon/dopamine anti-flaming thermal-insulation the aeroge of the present invention, the consumption of described dopamine accounts for airsetting
The 5-20wt% of colloid amount, organosilicon is 0.5 with the mass ratio of cellulose:1-3:1；Wherein, cellulose is cellulose micro wire
Or cellulose nano wire.
Described organosilicon is γ-aminopropyl triethoxysilane KH-550, γ-(2,3-epoxy the third oxygen) propyl group trimethoxy
At least one in base silane KH-560 and vinyltrimethoxy silane KH-171.
Described cellulose is wood pulp cellulose, bamboo cellulose, cotton cellulose, the one in carboxy-modified cellulose.
A diameter of 30-100nm of described cellulose micro wire, a length of 0.5-1mm；A diameter of 1-of cellulose nano wire
100nm, a length of 100 to 500 nanometers.
A kind of preparation method of the cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge of the present invention, including：
(1) joining organosilicon in cellulose micrometer/nanometer suspension, stirring, being subsequently adding dopamine, regulation pH is extremely
8～9, stirring, obtain suspension；Wherein, organosilicon and the mass ratio of cellulose are 0.5:1-3:1；
(2) suspension in step (1) is placed in liquid nitrogen freezing, obtains the gel of frost, freeze-drying, bakee,
To cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge；Wherein, the consumption of dopamine accounts for the 5-20wt% of aeroge quality.
In described step (1), the solid content of cellulose micrometer/nanometer suspension is 0.7-1.6wt%.
In described step (1), the time of stirring is 20～30h；Preferably 24h.
Regulation pH three (methylol) aminomethane-hydrochloric acid Tris-HCl buffer solution regulation in described step (1).
In described step (1), pH is 8.5.
Time freezing in liquid nitrogen in described step (2) is 3～10min；The cryodesiccated time is 24～48h.
The temperature bakeing in described step (2) is 80～120 DEG C, and the time of baking is 20～35min；Preferably 30min.
Beneficial effect
The present invention is to utilize self hydrolytic polymerization of organosilicon and the autoxidation of dopamine to be aggregated in identical pH condition
Under, and the product after the two polymerization can pass through hydrogen bond with the hydroxyl of cellulose surface or chemical bond interacts and cellulose
Fiber combines, and also improves the mechanical performance of cellulose aerogels while improving cellulose aerogels fire resistance；Gas
The loose structure of gel gives its low thermal conductivity, thus has good heat-proof quality.
Brief description
Fig. 1 is compression stress strain curve (a) and compression strength (b) of the cellulose aerogels of different component；Wherein CA
Referring to pure cellulose aeroge, CA/Si refers to the composite aerogel of cellulose fibre element and organosilicon, CA/Si/Dopa.1, CA/Si/
Dopa.2, CA/Si/Dopa.3 refer to the cellulose containing 5wt%, 10wt% and 20wt% dopamine, organosilicon and DOPA respectively
Amine composite aerogel；(three numerical value corresponding embodiment the 1st, embodiments 2 respectively and and embodiment 3, according to embodiment is given hydrochloric acid
The quality of dopamine, is then calculated the content of dopamine in composite aerogel)
Fig. 2 is the thermal conductivity factor of the cellulose aerogels of different component；
Fig. 3 be different component cellulose aerogels burning before and after the digital photograph of (in corresponding diagram up and down)；From left to right
It is followed successively by CA, CA/Si, CA/Si/Dopa.1, CA/Si/Dopa.2, CA/Si/Dopa.3；
Fig. 4 is the preparation flow figure of cellulose/organosilicon in the present invention/dopamine anti-flaming thermal-insulation aeroge.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention is expanded on further.Should be understood that these embodiments are merely to illustrate the present invention
Rather than restriction the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, people in the art
The present invention can be made various changes or modifications by member, and these equivalent form of values fall within the application appended claims equally and limited
Scope.
Embodiment 1
(1) modification of cellulose micron (nanometer) line suspension
Weigh the wood pulp cellulose micro wire suspension that 10g mass fraction is 1.4% to be placed in 50ml beaker, in room temperature
Under conditions of magnetic agitation, 0.14g KH550 is added dropwise in above-mentioned suspension, adds 17.1mg (5wt%) Dopamine hydrochloride
And by the pH value of Tris-HCl buffer solution regulation suspension to 8.5；Keep 24h is stirred at room temperature.
(2) cellulose aerogels is prepared
Suspension is simultaneously positioned in liquid nitrogen freezing 8min, after freezing terminates by the rotor that takes out in step (1) in suspension
The gel of frost is placed into lyophilized preparation and is dried (about 36h), obtain cellulose aerogels, then by cellulose aerogels
Be placed in 110 DEG C of baking ovens be dried 30min to improve the degree of cross linking of silane, obtain cellulose/organosilicon/dopamine anti-flaming thermal-insulation
Aeroge.
Embodiment 2
(1) modification of cellulose micron (nanometer) line suspension
Weigh the wood pulp cellulose micro wire suspension that 10g mass fraction is 1.4% to be placed in 50ml beaker, in room temperature
Under conditions of magnetic agitation, 0.14g KH550 is added dropwise in above-mentioned suspension, adds 31.1mg (10wt%) hydrochloric acid DOPA
Amine simultaneously regulates the pH value of suspension to 8.5 with Tris-HCl buffer solution；Keep 24h is stirred at room temperature.
(2) suspension is simultaneously positioned in liquid nitrogen freezing 8min by the rotor that takes out in step (1) in suspension, and freezing terminates
After the gel of frost be placed into lyophilized preparation be dried (about 36h), obtain cellulose aerogels, then by cellulose airsetting
Glue is placed in 110 DEG C of baking ovens and is dried 30min improving the degree of cross linking of silane, obtain cellulose/organosilicon/dopamine fire-retardant every
Aerogel.
Embodiment 3
(1) modification of cellulose micron (nanometer) line suspension
Weigh the wood pulp cellulose micro wire suspension that 10g mass fraction is 1.4% to be placed in 50ml beaker, in room temperature
Under conditions of magnetic agitation, 0.14g KH550 is added dropwise in above-mentioned suspension, adds 70.0mg (20wt%) hydrochloric acid DOPA
Amine simultaneously regulates the pH value of suspension to 8.5 with Tris-HCl buffer solution；Keep 24h is stirred at room temperature.
(2) suspension is simultaneously positioned in liquid nitrogen freezing 8min by the rotor that takes out in step (1) in suspension, and freezing terminates
After the gel of frost be placed into lyophilized preparation be dried (about 36h), obtain cellulose aerogels, then by cellulose airsetting
Glue is placed in 110 DEG C of baking ovens and is dried 30min improving the degree of cross linking of silane, obtain cellulose/organosilicon/dopamine fire-retardant every
Aerogel.
Embodiment 4
(1) modification of cellulose micron (nanometer) line suspension
Weigh the wood pulp cellulose micro wire suspension that 10g mass fraction is 1.4% to be placed in 50ml beaker, in room temperature
Under conditions of magnetic agitation, 0.14g KH560 is added dropwise in above-mentioned suspension, adds 31.1mg Dopamine hydrochloride and be used in combination
The pH value of Tris-HCl buffer solution regulation suspension is to 8.5；Keep 24h is stirred at room temperature.(2) in taking-up step (1) in suspension
Rotor and suspension is positioned in liquid nitrogen freezing 8min, the gel of frost is placed into lyophilized preparation after terminating and enters by freezing
Row is dried (about 36h), obtains cellulose aerogels, then is placed into cellulose aerogels in 110 DEG C of baking ovens and is dried 30min and carries
The degree of cross linking of high silane, obtains cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge.
Embodiment the 1st, the 2nd, 3 preparation sample once numbered CA/Si/Dopa.1, CA/Si/Dopa.2, CA/Si/
Dopa.3.As can be known from Fig. 1, purer cellulose aerogels, the mechanical performance of aeroge after introducing organosilicon and dopamine
Improve and the increase of the amount with dopamine for the intensity increases.
See Fig. 2, example the 1st, the 2nd, the thermal conductivity factor of aeroges of 3 preparations maintain 0.046W/ (m K).
Seeing Fig. 3, pure cellulose aeroge easily burns, and ashes residue (Fig. 3 a) only a small amount of after burnup.Introduce
After organosilicon and dopamine, the fire resistance of cellulose aerogels is significantly improved, when the content of dopamine reaches
During 10wt% (Fig. 3 d), aeroge leave flame can in 3s self-extinguishment.When the amount of dopamine increases to 20wt% (Fig. 3 e),
This composite aerogel leaves flame can horse back self-extinguishment.
Available：The amount difference of dopamine can significantly affect the fire resistance of aeroge.
Claims (10)
1. cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge, it is characterised in that the consumption of described dopamine accounts for gas
The 5-20wt% of gel quality, organosilicon is 0.5 with the mass ratio of cellulose:1-3:1；Wherein, cellulose is cellulose micron
Line or cellulose nano wire.
2. a kind of cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge according to claim 1, it is characterised in that institute
Stating organosilicon is γ-aminopropyl triethoxysilane KH-550, γ-(2,3-epoxy the third oxygen) propyl trimethoxy silicane KH-
At least one in 560 and vinyltrimethoxy silane KH-171.
3. a kind of cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge according to claim 1, it is characterised in that institute
Stating cellulose is wood pulp cellulose, bamboo cellulose, cotton cellulose, the one in carboxy-modified cellulose.
4. a kind of cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge according to claim 1, it is characterised in that institute
State a diameter of 30-100nm of cellulose micro wire, a length of 0.5-1mm；A diameter of 1-100nm of cellulose nano wire, length
It is 100 to 500 nanometers.
5. a preparation method for cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge, including：
(1) organosilicon is added in cellulose micrometer/nanometer suspension, stirring, is subsequently adding dopamine, regulate pH to 8～9,
Stirring, obtains suspension；Wherein, organosilicon and the mass ratio of cellulose are 0.5:1-3:1；
(2) suspension in step (1) is placed in liquid nitrogen freezing, obtains the gel of frost, freeze-drying, bakee, obtain fibre
Dimension element/organosilicon/dopamine anti-flaming thermal-insulation aeroge；Wherein, the consumption of dopamine accounts for the 5-20wt% of aeroge quality.
6. the preparation method of a kind of cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge according to claim 5, its
Being characterised by, in described step (1), the solid content of cellulose micrometer/nanometer suspension is 0.7-1.6wt%.
7. the preparation method of a kind of cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge according to claim 5, its
Being characterised by, in described step (1), the time of stirring is 20～30h.
8. the preparation method of a kind of cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge according to claim 5, its
It is characterised by, regulation pH three (methylol) aminomethane-hydrochloric acid Tris-HCl buffer solution regulation in described step (1).
9. the preparation method of a kind of cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge according to claim 5, its
Being characterised by, the time freezing in liquid nitrogen in described step (2) is 3～10min；The cryodesiccated time is 24～48h.
10. the preparation method of a kind of cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge according to claim 5, its
Being characterised by, the temperature bakeing in described step (2) is 80～120 DEG C, and the time of baking is 20～35min.
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Cited By (8)
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| CN108570163A (en) * | 2018-05-15 | 2018-09-25 | 东华大学 | A kind of preparation method of the high-efficiency electromagnetic shielding porous material based on nano-cellulose |
| CN109364834A (en) * | 2018-11-10 | 2019-02-22 | 浙江理工大学 | A kind of tri compound aeroge flame resistant heat insulation material and preparation method thereof by bamboo fiber reinforcement |
| CN110534725A (en) * | 2019-09-24 | 2019-12-03 | 浙江农林大学 | Silicon/carbon nanotube/carbon micro wire and preparation method and application |
| CN112281491A (en) * | 2020-10-30 | 2021-01-29 | 齐鲁工业大学 | Preparation and application of plant fiber-based reinforced carbon fiber network |
| CN112694638A (en) * | 2020-12-21 | 2021-04-23 | 东华大学 | Flexible flame-retardant aerogel, and preparation method and application thereof |
| CN115368621A (en) * | 2021-05-18 | 2022-11-22 | 中国科学院苏州纳米技术与纳米仿生研究所 | Aramid fiber/polydopamine aerogel film, phase-change composite film, preparation method and application |
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| CN108570163A (en) * | 2018-05-15 | 2018-09-25 | 东华大学 | A kind of preparation method of the high-efficiency electromagnetic shielding porous material based on nano-cellulose |
| CN108570163B (en) * | 2018-05-15 | 2021-05-11 | 东华大学 | Preparation method of efficient electromagnetic shielding porous material based on nanocellulose |
| CN109364834A (en) * | 2018-11-10 | 2019-02-22 | 浙江理工大学 | A kind of tri compound aeroge flame resistant heat insulation material and preparation method thereof by bamboo fiber reinforcement |
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| CN110534725A (en) * | 2019-09-24 | 2019-12-03 | 浙江农林大学 | Silicon/carbon nanotube/carbon micro wire and preparation method and application |
| CN112281491A (en) * | 2020-10-30 | 2021-01-29 | 齐鲁工业大学 | Preparation and application of plant fiber-based reinforced carbon fiber network |
| CN112281491B (en) * | 2020-10-30 | 2022-07-22 | 齐鲁工业大学 | Preparation and application of plant fiber-based reinforced carbon fiber network |
| CN112694638A (en) * | 2020-12-21 | 2021-04-23 | 东华大学 | Flexible flame-retardant aerogel, and preparation method and application thereof |
| CN112694638B (en) * | 2020-12-21 | 2021-10-15 | 东华大学 | Flexible flame-retardant aerogel, and preparation method and application thereof |
| CN115368621A (en) * | 2021-05-18 | 2022-11-22 | 中国科学院苏州纳米技术与纳米仿生研究所 | Aramid fiber/polydopamine aerogel film, phase-change composite film, preparation method and application |
| CN115368621B (en) * | 2021-05-18 | 2024-03-15 | 中国科学院苏州纳米技术与纳米仿生研究所 | Aramid fiber/polydopamine aerogel film, phase change composite film, preparation method and application |
| CN115960445A (en) * | 2022-11-25 | 2023-04-14 | 东华大学 | Surface-modified long bamboo fiber reinforced polylactic acid composite board and preparation method thereof |
| CN117736666A (en) * | 2023-11-30 | 2024-03-22 | 南通科顺建筑新材料有限公司 | Biomass flame-retardant heat-insulating self-adhesive waterproof coiled material and preparation method thereof |
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