CN106432783B - A kind of cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge and preparation method thereof - Google Patents
A kind of cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge and preparation method thereof Download PDFInfo
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- CN106432783B CN106432783B CN201610836204.8A CN201610836204A CN106432783B CN 106432783 B CN106432783 B CN 106432783B CN 201610836204 A CN201610836204 A CN 201610836204A CN 106432783 B CN106432783 B CN 106432783B
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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
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/24—Crosslinking, e.g. vulcanising, of macromolecules
- C08J3/246—Intercrosslinking of at least two polymers
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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
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L1/00—Compositions of cellulose, modified cellulose or cellulose derivatives
- C08L1/02—Cellulose; Modified cellulose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- 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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- 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
- C08J2301/02—Cellulose; Modified cellulose
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2203/00—Applications
- C08L2203/14—Applications used for foams
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
Abstract
The present invention relates to a kind of cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge and preparation method thereof, the dosage of the dopamine accounts for the 5-20wt% of aeroge quality, and the mass ratio of organosilicon and cellulose is 0.5:1-3:1；Wherein, cellulose is cellulose micro wire or cellulose nano wire.Preparation method, comprising: organosilicon is added in cellulose micrometer/nanometer suspension, is stirred, dopamine is then added, adjusts pH to 8~9, stirring obtains suspension；Suspension is placed in liquid nitrogen and is freezed, the gel freezed is freeze-dried, and is baked, is obtained cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge.Anti-flaming thermal-insulation aeroge of the invention also has good mechanical performance other than having excellent fire-retardancy and heat insulating properties energy；Meet the requirement of ecological, environmental protective, and has good application prospect in fields such as building, the heat-barrier material of pipeline and proximity suit fillers.
Description
Technical field
The invention belongs to aeroge and its preparation field, in particular to a kind of cellulose/organosilicon/dopamine anti-flaming thermal-insulation
Aeroge and preparation method thereof.
Background technique
Aeroge is gel by supercritical drying or freeze-drying its internal liquid is replaced with gas and
The three-dimensional porous material of one kind of generation.The material has many advantages, such as that small density, large specific surface area and thermal coefficient are small, extensive
Applied to heat-barrier material, active matter carrier and inductor etc..Traditional aeroge be using silicon as the inorganic aerogels of representative with
And it is widely studied by people using resorcin/formaldehyde and melamine/formaldehyde as the organic aerogel of representative.Cellulose
Aeroge has incorporated the excellent of cellulose while having inorganic tradition and organic aerogel as newborn third generation material
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 for the neck such as environmental protection and electrochemical energy storage by pyrolysis
Domain.
The research for preparing aeroge using cellulose is raw material, in recent years by the extensive concern of researchers, mainly
The preparation of cellulose aerogels is realized by two approach: first is that cellulose is by sodium hydroxide/urea liquid in low temperature item
It dissolves under part and then is finally freeze-dried through weak acid solution regeneration generation cellulose aquagel and obtain aeroge；Second is that cellulose
Fiber is by mechanical stripping or mechanical stripping is transformed into the nanowire suspended liquid of cellulose again by TEMPO/NaBr/NaClO, then
By freezing and freeze-drying obtains cellulose aerogels.But the fire resistance of cellulose aerogels and mechanical performance are poor.
Silane is interacted by the hydroxyl that hydrolysis generates silicone hydroxyl and cellulose surface by hydrogen bond and chemical bond come reinforcing fiber element
The rigidity of fiber.It therefore can be using silane come the mechanical performance of reinforcing fiber cellulose fiber.Silicon is common in flame-proof treatment simultaneously
A kind of environmentally friendly fire retardant can improve the thermal stability of cellulose aerogels by introducing silane.
Dopamine is received extensive attention due to its bio-compatible, nontoxic and strong adhesion property.Nearest researcher's hair
The catechol of existing dopamine has very strong radical-scavenging ability.So the radical-scavenging ability and silicon of dopamine can be used
The performance of the catalytic cellulose carbonization of alkane combines, to improve the fire resistance of cellulose aerogels.
Summary of the invention
Technical problem to be solved by the invention is to provide a kind of cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroges
And preparation method thereof, this method is raw material with the cellulose that nature is widely present, and utilizes organosilicon and dopamine modified fibre
Usually improve its mechanical performance and flame retardant property；Obtained aeroge has good mechanical properties, lower thermal conductivity and excellent resistance
Performance is fired, has 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 aeroge of the invention, the dosage of the dopamine account for airsetting
The mass ratio of the 5-20wt% of colloid amount, organosilicon and cellulose is 0.5:1-3:1；Wherein, cellulose is cellulose micro wire
Or cellulose nano wire.
The organosilicon is γ-aminopropyl triethoxysilane KH-550, γ-(the third oxygen of 2,3- epoxy) propyl trimethoxy
At least one of base silane KH-560 and vinyltrimethoxysilane KH-171.
The cellulose is one of wood pulp cellulose, bamboo cellulose, cotton cellulose, carboxy-modified cellulose.
The diameter of the cellulose micro wire is 30-100nm, length 0.5-1mm；The diameter of cellulose nano wire is 1-
100nm, length are 100 to 500 nanometers.
A kind of cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge preparation method of the invention, comprising:
(1) organosilicon is added in cellulose micrometer/nanometer suspension, stirs, be then added dopamine, adjust pH to
8~9, stirring obtains suspension；Wherein, the mass ratio of organosilicon and cellulose is 0.5:1-3:1；
(2) suspension in step (1) is placed in liquid nitrogen the gel for freezing, being freezed, be freeze-dried, baked, obtain
To cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge；Wherein, the dosage of dopamine accounts for the 5-20wt% of aeroge quality.
The solid content of cellulose micrometer/nanometer suspension is 0.7-1.6wt% in the step (1).
The time stirred in the step (1) is 20~30h；It is preferred that for 24 hours.
PH is adjusted in the step (1) to be adjusted with three (methylol) aminomethanes-hydrochloric acid Tris-HCl buffer.
PH is 8.5 in the step (1).
The time freezed in liquid nitrogen in the step (2) is 3~10min；The time of freeze-drying is 24~48h.
The temperature baked in the step (2) is 80~120 DEG C, and the time of baking is 20~35min；It is preferred that 30min.
Beneficial effect
The present invention is to be aggregated in identical pH condition using itself hydrolytic polymerization of organosilicon and the autoxidation of dopamine
Under, and the product after the two polymerization can pass through hydrogen bond or chemical bond interaction and cellulose with the hydroxyl of cellulose surface
Fiber combines, and also improves the mechanical performance of cellulose aerogels while improving cellulose aerogels flame retardant property；Gas
The porous structure of gel assigns its low thermal conductivity, to possess good heat-proof quality.
Detailed description of the invention
Fig. 1 is the compression stress strain curve (a) and compression strength (b) of the cellulose aerogels of different component；Wherein CA
Refer to that pure cellulose aeroge, CA/Si refer to the composite aerogel of cellulose fibre element and organosilicon, CA/Si/Dopa.1, CA/Si/
Dopa.2, CA/Si/Dopa.3 respectively refer to the cellulose containing 5wt%, 10wt% and 20wt% dopamine, organosilicon and DOPA
Amine composite aerogel；(three numerical value respectively correspond embodiment 1, embodiment 2 and with embodiment 3, according to providing hydrochloric acid in embodiment
Then the content of dopamine in composite aerogel is calculated in the quality of dopamine)
Fig. 2 is the thermal coefficient of the cellulose aerogels of different component；
Fig. 3 is the digital photograph of the cellulose aerogels burning front and back (in corresponding diagram up and down) of different component；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 cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge preparation flow figure in the present invention.
Specific embodiment
Present invention will be further explained below with reference to specific examples.It should be understood that these embodiments are merely to illustrate the present invention
Rather than it limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, those skilled in the art
Member can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Range.
Embodiment 1
(1) modification of cellulose micron (nanometer) line suspension
It weighs the wood pulp cellulose micro wire suspension that 10g mass fraction is 1.4% to be placed into 50ml beaker, in room temperature
0.14g KH550 is added dropwise in above-mentioned suspension under conditions of magnetic agitation, adds 17.1mg (5wt%) Dopamine hydrochloride
And the pH value of suspension is adjusted to 8.5 with Tris-HCl buffer；Holding is stirred at room temperature for 24 hours.
(2) cellulose aerogels are prepared
It takes out the rotor in step (1) in suspension and suspension is placed in liquid nitrogen and freeze 8min, after freezing
The gel of frost is placed into lyophilized preparation, (about 36h) is dried, obtain cellulose aerogels, then by cellulose aerogels
It is placed into 110 DEG C of baking ovens and dries 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
It weighs the wood pulp cellulose micro wire suspension that 10g mass fraction is 1.4% to be placed into 50ml beaker, in room temperature
0.14g KH550 is added dropwise in above-mentioned suspension under conditions of magnetic agitation, adds 31.1mg (10wt%) hydrochloric acid DOPA
Amine simultaneously adjusts the pH value of suspension to 8.5 with Tris-HCl buffer；Holding is stirred at room temperature for 24 hours.
(2) it takes out the rotor in step (1) in suspension and suspension is placed in liquid nitrogen and freeze 8min, freezing terminates
The gel of frost is placed into lyophilized preparation afterwards, (about 36h) is dried, obtain cellulose aerogels, then by cellulose airsetting
Glue is placed into 110 DEG C of baking ovens dry 30min to improve the degree of cross linking of silane, obtain cellulose/organosilicon/dopamine it is fire-retardant every
Aerogel.
Embodiment 3
(1) modification of cellulose micron (nanometer) line suspension
It weighs the wood pulp cellulose micro wire suspension that 10g mass fraction is 1.4% to be placed into 50ml beaker, in room temperature
0.14g KH550 is added dropwise in above-mentioned suspension under conditions of magnetic agitation, adds 70.0mg (20wt%) hydrochloric acid DOPA
Amine simultaneously adjusts the pH value of suspension to 8.5 with Tris-HCl buffer；Holding is stirred at room temperature for 24 hours.
(2) it takes out the rotor in step (1) in suspension and suspension is placed in liquid nitrogen and freeze 8min, freezing terminates
The gel of frost is placed into lyophilized preparation afterwards, (about 36h) is dried, obtain cellulose aerogels, then by cellulose airsetting
Glue is placed into 110 DEG C of baking ovens dry 30min to improve the degree of cross linking of silane, obtain cellulose/organosilicon/dopamine it is fire-retardant every
Aerogel.
Embodiment 4
(1) modification of cellulose micron (nanometer) line suspension
It weighs the wood pulp cellulose micro wire suspension that 10g mass fraction is 1.4% to be placed into 50ml beaker, in room temperature
0.14g KH560 is added dropwise in above-mentioned suspension under conditions of magnetic agitation, 31.1mg Dopamine hydrochloride is added and is used in combination
Tris-HCl buffer adjusts the pH value of suspension to 8.5；Holding is stirred at room temperature for 24 hours.(2) it takes out in step (1) in suspension
Rotor and suspension be placed in liquid nitrogen freeze 8min, after freezing by the gel of frost be placed into lyophilized preparation into
Row is dry (about 36h), obtains cellulose aerogels, then cellulose aerogels are placed into 110 DEG C of baking ovens dry 30min to mention
The degree of cross linking of high silane obtains cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge.
It is CA/Si/Dopa.1, CA/Si/Dopa.2, CA/Si/ that sample prepared by embodiment 1,2,3, which is once numbered,
Dopa.3.As can be known from Fig. 1, purer cellulose aerogels introduce the mechanical performance of aeroge after organosilicon and dopamine
It improves and intensity is as the increase of the amount of dopamine increases.
See that Fig. 2, the thermal coefficient of aeroge prepared by example 1,2,3 maintain 0.046W/ (m K).
See that Fig. 3, pure cellulose aeroge easily burn, and ashes only a small amount of after burnup are remaining (Fig. 3 a).It introduces
After organosilicon and dopamine, the flame retardant property of cellulose aerogels is significantly improved, when the content of dopamine reaches
When 10wt% (Fig. 3 d), aeroge leave flame can in 3s self-extinguishment.When the amount of dopamine increases to 20wt% (Fig. 3 e),
The composite aerogel leaves flame being capable of horse back self-extinguishment.
Available: the amount difference of dopamine can significantly affect the flame retardant property of aeroge.
Claims (10)
1. a kind of cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge, which is characterized in that the aeroge be by organosilicon,
It is prepared after dopamine, cellulose suspension mixing, wherein hydrolytic condensation occurs for organosilicon, and it is poly- that autoxidation occurs for dopamine
It closes, cellulose suspension forms porous gel；The dosage of dopamine accounts for the 5-20wt% of aeroge quality, organosilicon and cellulose
Mass ratio be 0.5:1-3:1；Cellulose is cellulose micro wire or cellulose nano wire.
2. a kind of cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge according to claim 1, which is characterized in that institute
Stating organosilicon is γ-aminopropyl triethoxysilane KH-550, γ-(the third oxygen of 2,3- epoxy) propyl trimethoxy silicane KH-
At least one of 560 and vinyltrimethoxysilane KH-171.
3. a kind of cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge according to claim 1, which is characterized in that institute
Stating cellulose is one of wood pulp cellulose, bamboo cellulose, cotton cellulose, carboxy-modified cellulose.
4. a kind of cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge according to claim 1, which is characterized in that institute
The diameter for stating cellulose micro wire is 30-100nm, length 0.5-1mm；The diameter of cellulose nano wire is 1-100nm, length
It is 100 to 500 nanometers.
5. a kind of cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge preparation method, comprising:
(1) organosilicon is added in cellulose micrometer/nanometer suspension, is stirred, dopamine is then added, adjust pH to 8~9,
Stirring, obtains suspension；Wherein, the mass ratio of organosilicon and cellulose is 0.5:1-3:1；
(2) suspension in step (1) is placed in liquid nitrogen the gel for freezing, being freezed, be freeze-dried, baked, obtain fibre
Tie up element/organosilicon/dopamine anti-flaming thermal-insulation aeroge；Wherein, the dosage of dopamine accounts for the 5-20wt% of aeroge quality.
6. a kind of preparation method of cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge according to claim 5,
It is characterized in that, the solid content of cellulose micrometer/nanometer suspension is 0.7-1.6wt% in the step (1).
7. a kind of preparation method of cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge according to claim 5,
It is characterized in that, the time stirred in the step (1) is 20~30h.
8. a kind of preparation method of cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge according to claim 5,
It is characterized in that, pH is adjusted in the step (1) and is adjusted with three (methylol) aminomethanes-hydrochloric acid Tris-HCl buffer.
9. a kind of preparation method of cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge according to claim 5,
It is characterized in that, the time freezed in liquid nitrogen in the step (2) is 3~10min；The time of freeze-drying is 24~48h.
10. a kind of preparation method of cellulose/organosilicon/dopamine anti-flaming thermal-insulation aeroge according to claim 5,
It is characterized in that, the temperature baked in the step (2) is 80~120 DEG C, and the time of baking is 20~35min.
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| 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 |
| CN110534725B (en) * | 2019-09-24 | 2020-10-30 | 浙江农林大学 | Silicon/carbon nano tube/carbon micron line and preparation method and application thereof |
| 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 |
| CN112694638B (en) * | 2020-12-21 | 2021-10-15 | 东华大学 | Flexible flame-retardant aerogel, and preparation method and application thereof |
| 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 |
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| CN105254916A (en) * | 2015-09-30 | 2016-01-20 | 西南交通大学 | Preparation method for oxidized graphene-poly-dopamine composite aerogel |
| CN105566673A (en) * | 2015-12-17 | 2016-05-11 | 中国科学院兰州化学物理研究所 | Preparation method of multifunctional cellulose elastic aerogel |
| CN105664738A (en) * | 2016-04-11 | 2016-06-15 | 江西师范大学 | Graphene oxide-based composite membrane for treating radioactive wastewater |
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| CN105254916A (en) * | 2015-09-30 | 2016-01-20 | 西南交通大学 | Preparation method for oxidized graphene-poly-dopamine composite aerogel |
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