CN106007654A - Basalt fiber composite cellulose multifunctional aerogel material and preparation method thereof - Google Patents
Basalt fiber composite cellulose multifunctional aerogel material and preparation method thereof Download PDFInfo
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- CN106007654A CN106007654A CN201610349057.1A CN201610349057A CN106007654A CN 106007654 A CN106007654 A CN 106007654A CN 201610349057 A CN201610349057 A CN 201610349057A CN 106007654 A CN106007654 A CN 106007654A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B30/00—Compositions for artificial stone, not containing binders
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
Abstract
The invention relates to the field of composite materials, particularly a basalt fiber composite cellulose multifunctional aerogel material and a preparation method thereof. The basalt fiber composite cellulose multifunctional aerogel material comprises wood fibers used as a substrate phase and basalt fibers used as a reinforcement phase, wherein the wood fibers and basalt fibers form the composite aerogel structure. The preparation method of the material improves the mechanical strength, flame retardancy and aging resistance of the existing cellulose aerogel, widens the use and processing range of the cellulose aerogel, and greatly enhances the safety and service life in the use process. Meanwhile, the material can not change the original heat-insulating property and oil absorbency of the cellulose aerogel.
Description
Technical field
The present invention relates to field of compound material, particularly relate to a kind of basalt fibre compound cellulose Multifunctional, air gel material
Material and preparation method thereof.
Background technology
Aeroge is also called xerogel.Aeroge refers to, when major part solvent sloughed by gel, make content liquid ratio in gel
Solids content much less, or in the space net structure of gel be full of medium be gas, appearance is the material of solid, shaped.Typical case
Aeroge such as gelatin, arabic gum, silica gel, hair, fingernail etc..Aeroge also has the character of gel, i.e. has expansion, touches
Change effect, synaeresis.Meanwhile, aeroge also has the features such as nano level loose structure and high porosity, is current known
One of solid material that density is minimum.
Owing to the disperse medium of aerogel material is gas, and as the solid phase of gel network skeleton, and network
Gap structure is Nano grade, and this continuous three-dimensional manometer network structure makes it have the performance of uniqueness, such as high porosity, height
Specific surface area, low heat conduction coefficient, low-k, low optical index, the low velocity of sound etc..
Cellulose aerogels, has surmounted silica aerogel and polymer base aeroge, is possessing traditional aerogel property (high hole
Gap rate, high-specific surface area etc.) while incorporated self excellent properties, such as good biocompatibility and degradability,
Heat-insulation and heat-preservation, crude oil the field such as are sewed and are had great application prospect and raw material easily obtains.Such as application number
CN201510997563.7, application title " a kind of graphene oxide/nano-cellulose aerogel and its preparation method and application "
In disclose a kind of graphene oxide/nano-cellulose aerogel and its preparation method and application, belong to aerogel material technology
Field.This aeroge is prepared from by the method comprised the following steps: 1) is scattered in hydrochloric acid by nano-cellulose and makes nanometer
Cellulose dispersion liquid;2) by graphene oxide dispersion and step 1) mixing of gained nano-cellulose dispersion liquid, 170~190
Carry out hydro-thermal reaction at DEG C, obtain hydrogel;3) by step 2) gained hydrogel carries out lyophilization, to obtain final product.The present invention provides
Graphene oxide/nano-cellulose aerogel, with nano-cellulose and graphene oxide as raw material, prepared by hydro-thermal reaction
Hydrogel, further by lyophilization, obtains final products.Compared with graphite oxide aerogel, this aeroge Pyrogentisinic Acid
The removal effect of phenol in aqueous solution is more preferable, can be used for organic dye molecule or the removal of other impurity in sewage, it is achieved sewage
High-efficient purification.
But cellulose aerogels is due to own material, there are some defects, such as mechanical strength the best, durable
Property is general, it is impossible to fire-retardant etc..So needing a kind of novel material, at the base of the existing advantageous property of cellulose-binding aeroge
Preferable mechanical strength and fire resistance it is provided simultaneously with on plinth.
Summary of the invention
It is an object of the invention to provide a kind of basalt fibre compound cellulose Multifunctional, air gel rubber material, it is intended to solve
The problem that existing cellulose aerogels mechanical strength is little.
The present invention is achieved in that a kind of basalt fibre compound cellulose Multifunctional, air gel rubber material, and its feature exists
In: include as base material phase wood fibre and as strengthen phase basalt fibre, described wood fibre and the described Black Warrior
Rock fiber forms composite aerogel structure.Basalt fibre (CBF) is the one nothing researched and developed through more than 30 years by the former Soviet Union
Organic fiber, is after basalt building stones melt at 1450 DEG C~1500 DEG C, by platinum-rhodium alloy bushing high speed pulling
Continuous fiber, intensity is suitable with high intensity S glass fibre.The color of pure natural basalt fibre is generally brown, and some is like gold
Color.Basalt fibre is a kind of novel inorganic environment-friendly and green high performance fibre material, and it is by silicon dioxide, aluminium oxide, oxidation
The basalt building stones of the oxide compositions such as calcium, magnesium oxide, ferrum oxide and titanium dioxide, after high-temperature fusion, are quickly drawn by bushing
System.Basalt fibre, basalt continuous fiber not only intensity is high, but also has electric insulation, corrosion-resistant, high temperature resistant etc.
Multiple excellent properties.Temperature tolerance is higher than all of organic fiber, and has noninflammability, without advantages such as thermal contraction phenomenons.It is a kind of
The outstanding material that can be used for being combined.Additionally, the garbage that the production technology of basalt fibre determines generation is few, dirty to environment
Contaminate little, and can degrade the most in the environment after product abandonment, without any harm, thus be a kind of genuine green, environmental protection
Material.
Cellulose fiber peacekeeping basalt fibre is not the most combined with each other by prior art and forms the note of composite aerogel
Carry.Basalt fibre is that aeroge provides high temperature resistant and high definition performance, will not reduce after adding basalt fibre simultaneously
The heat-proof quality of cellulose aerogels script and oil absorbency.
The further technical scheme of the present invention is: length 0.1-10 mm of described wood fibre.The length of wood fibre
The bulk properties of described basalt fibre compound cellulose Multifunctional, air gel rubber material there is considerable influence.
The further technical scheme of the present invention is: a length of 0.1-20 mm of described basalt fibre.Basalt fibre
Length has decisive influence to the mechanical property of described basalt fibre compound cellulose Multifunctional, air gel rubber material.
Another object of the present invention is to provide a kind of basalt fibre compound cellulose Multifunctional, air gel rubber material to prepare
Method, it is characterised in that: comprise the following steps:
A. substrate solution preparation process, lignocellulose is scattered in solvent acquisition base material by described substrate solution preparation process system
Solution;
B. hydrogel preparation process, described substrate solution and basalt fibre are compounded to form water by described hydrogel preparation process system
Gel;
C. freezing gel preparation process, described freezing gel preparation process system will obtain freezing gel after described hydrogel freezing,
Cryogenic temperature is-10 ~-30 DEG C, and cooling time is 0.5-30 h;
D. aeroge preparation process, described aeroge preparation process system will obtain aeroge after described freezing gel lyophilization,
Cryodesiccated condenser temperature is-50 ~-70 DEG C, and vacuum is 10-1000 Pa, and drying time is 0.5-50 h.
The further technical scheme of the present invention is: described step B include following step by step:
B1. mixed solution preparation process, it is molten that described basalt fibre is added described base material by described mixed solution preparation process system
In liquid, obtain mixed solution;
B2. hydrogel solution preparation process, described hydrogel solution preparation process ties up to add in described mixed solution dispersant
Hydrogel solution is obtained with water-repelling agent;
B3. by described hydrogel solution by ultrasonic or mechanical agitation is dispersed and forms hydrogel, the most churned mechanically
Frequency is 500-5000 rpm, and mixing time is 0.5-20 h.
The further technical scheme of the present invention is: described step B include following step by step:
B1. skeleton preparation process, the roving of basalt fibre, fiber felt or fiber cloth are compiled by described skeleton preparation process system
It is made for skeleton framework;
B2. hydrogel solution preparation process, described hydrogel solution preparation process ties up to add dispersant in described base material and dredge
Water preparation obtains hydrogel solution;
B3. described skeleton framework and described hydrogel solution are compounded to form hydrogel.
The further technical scheme of the present invention is: the content of described basalt fibre is described basalt fibre composite fibre
The 5-50% of element Multifunctional, air gel rubber material.Basalt fibre content is to the described multi-functional airsetting of basalt fibre compound cellulose
The mechanical property of glue material has considerable influence.
The further technical scheme of the present invention is: solvent described in step A is sodium hydroxide, deionized water, carbamide, sulfur
In urea, polyvinyl alcohol, Lithium hydrate one or more.
Preferably, described solvent is the mixed liquor of sodium hydroxide and deionized water, sodium hydroxide quality in described mixed liquor
Accounting 5-15 %.
The further technical scheme of the present invention is: lignocellulose described in step A also need to before disperseing through
Clean and dry run.
The invention has the beneficial effects as follows: the invention discloses a kind of basalt fibre compound cellulose Multifunctional, air gel material
Material and preparation method thereof, this material improves the mechanical strength of existing cellulose aerogels, anti-flammability and ageing resistace, increases
The use of cellulose aerogels and the range of work, substantially increase the safety during use and service life;Meanwhile, originally
Material can't change the original heat-proof quality of cellulose aerogels and oil absorbency.
Detailed description of the invention
Contrast specific embodiment one
Cellulose fibre is joined in appropriate solution, addition dispersant, water-repelling agent and cross-linking agent, mechanical agitation 3h,
3000rpm, at a temperature of 80 DEG C, forms gel mixed solution.Under-20 DEG C of low temperature, freezing 3 hours, arrange condenser temperature-60
DEG C, suction, to 50Pa, then starts lyophilization 30h, freeze temperature 50 DEG C.
The cellulose aerogels prepared, heat conductivity is 0.017W/ (m K), and hot strength is 10MPa;Run into naked light,
Within 3 seconds, light;200 DEG C of degradations 72 hours, subsiding occurs in structure;Saturated oil suction is 112 times of deadweight.
Specific embodiment one.
It is that sodium hydroxide and deionized water are mixed as solution for standby by 5:95 in mass ratio.10:90 in mass ratio is by profound
Military rock chopped strand and cellulose fibre join in solution, addition dispersant, water-repelling agent and cross-linking agent, mechanical agitation 3h,
3000rpm, at a temperature of 80 DEG C, forms gel mixed solution.Under-20 DEG C of low temperature, freezing 3 hours, arrange condenser temperature-60
DEG C, suction, to 50Pa, then starts lyophilization 30h, freeze temperature 50 DEG C.
Basalt-the cellulose aerogels prepared, heat conductivity is 0.015W/ (m K), and hot strength is 30MPa;
It is difficult to light, under alcohol burner, after about 1 minute, just starts burning;Degradation 72 hours, size appearance is without significant change;Full
With 101 times that oil suction is deadweight.
Specific embodiment two.
Joining in solution by 30:70 in mass ratio by basalt chopped fiber and cellulose fibre, other conditions are with real
Execute example 1.
Basalt-the cellulose aerogels prepared, heat conductivity is 0.016W/ (m K), and hot strength is 47MPa;
Being difficult to light, under alcohol burner, after contact aeroge, after 3 minutes, just starting point combustion gas gel, degradation 72 hours, outside size
See without significant change;Saturated oil suction is 81 times of deadweight.
Specific embodiment three.
Joining in solution by 50:50 in mass ratio by basalt chopped fiber and cellulose fibre, other conditions are with real
Execute example 1.
Basalt-the cellulose aerogels prepared, heat conductivity is 0.018W/ (m K), and hot strength is 67
MPa;Being difficult to light, under alcohol burner, after contact aeroge, self-extinguishment, degradation 72 hours, size appearance is without significant change;Full
With 76 times that oil suction is deadweight.
Specific embodiment four.
It is that sodium hydroxide and deionized water are mixed, as solution for standby by 10:90 in mass ratio.Cellulose fibre is added
In solution, add dispersant, water-repelling agent and cross-linking agent, mechanical agitation 3h, 3000rpm, at a temperature of 80 DEG C, form gel
Mixed solution, places one layer of basalt fiber cloth respectively with top bottom sample tray.Freezing 3 hours under-20 DEG C of low temperature,
Arranging condenser temperature-60 DEG C, suction, to 50Pa, then starts lyophilization 30h, freeze temperature 50 DEG C.
Basalt-the cellulose aerogels prepared, heat conductivity is 0.016W/ (m K), and hot strength is 110MPa;
Cannot light;Degradation 72 hours, size appearance is without significant change;Saturated oil suction is 98 times of deadweight.
Specific embodiment five
It is that sodium hydroxide and deionized water are mixed, as solution for standby by 15:85 in mass ratio.Cellulose fibre is joined molten
In liquid, add dispersant, water-repelling agent and cross-linking agent, mechanical agitation 3h, 3000rpm, at a temperature of 80 DEG C, form gel mixing
Solution, places one layer of 0.5mm thickness basalt fiber cloth respectively with top and centre bottom sample tray.At-20 DEG C of low temperature
Lower freezing 3 hours, arranging condenser temperature-60 DEG C, suction, to 50Pa, then starts lyophilization 30h, freeze temperature 50
℃。
Basalt-the cellulose aerogels prepared, heat conductivity is 0.020W/ (m K), and hot strength is
120MPa;Cannot light;Degradation 72 hours, size appearance is without significant change;Saturated oil suction is 95 times of deadweight.
The invention discloses a kind of basalt fibre compound cellulose Multifunctional, air gel rubber material and preparation method thereof, this material
Material improves the mechanical strength of existing cellulose aerogels, anti-flammability and ageing resistace, adds making of cellulose aerogels
With and the range of work, substantially increase the safety during use and service life;Meanwhile, this material can't change fiber
The element original heat-proof quality of aeroge and oil absorbency.
The foregoing is only presently preferred embodiments of the present invention, not in order to limit the present invention, all essences in the present invention
Any amendment, equivalent and the improvement etc. made within god and principle, should be included within the scope of the present invention.
Claims (10)
1. a basalt fibre compound cellulose Multifunctional, air gel rubber material, it is characterised in that: include as base material phase
Wood fibre and the basalt fibre as enhancing phase, described wood fibre and described basalt fibre form composite aerogel knot
Structure.
It is the most according to claim 1, it is characterised in that: length 0.1-10 mm of described wood fibre.
It is the most according to claim 1, it is characterised in that: a length of 0.1-20 mm of described basalt fibre.
4. arbitrary described basalt fibre compound cellulose Multifunctional, air gel rubber material preparation side in claim 1-3
Method, it is characterised in that: comprise the following steps:
A. substrate solution preparation process, lignocellulose is scattered in solvent acquisition base material by described substrate solution preparation process system
Solution;
B. hydrogel preparation process, described substrate solution and basalt fibre are compounded to form water by described hydrogel preparation process system
Gel;
C. freezing gel preparation process, described freezing gel preparation process system will obtain freezing gel after described hydrogel freezing,
Cryogenic temperature is-10 ~-30 DEG C, and cooling time is 0.5-30 h;
D. aeroge preparation process, described aeroge preparation process system will obtain aeroge after described freezing gel lyophilization,
Cryodesiccated condenser temperature is-50 ~-70 DEG C, and vacuum is 10-1000 Pa, and drying time is 0.5-50 h.
Basalt fibre compound cellulose Multifunctional, air gel rubber material preparation method the most according to claim 4, its feature
Be: described step B include following step by step:
B1. mixed solution preparation process, it is molten that described basalt fibre is added described base material by described mixed solution preparation process system
In liquid, obtain mixed solution;
B2. hydrogel solution preparation process, described hydrogel solution preparation process ties up to add in described mixed solution dispersant
Hydrogel solution is obtained with water-repelling agent;
B3. by described hydrogel solution by ultrasonic or mechanical agitation is dispersed and forms hydrogel, the most churned mechanically
Frequency is 500-5000 rpm, and mixing time is 0.5-20 h.
Basalt fibre compound cellulose Multifunctional, air gel rubber material preparation method the most according to claim 4, its feature
Be: described step B include following step by step:
B1. skeleton preparation process, the roving of basalt fibre, fiber felt or fiber cloth are compiled by described skeleton preparation process system
It is made for skeleton framework;
B2. hydrogel solution preparation process, described hydrogel solution preparation process ties up to add dispersant in described base material and dredge
Water preparation obtains hydrogel solution;
B3. described skeleton framework and described hydrogel solution are compounded to form hydrogel.
Basalt fibre compound cellulose Multifunctional, air gel rubber material preparation method the most according to claim 4, its feature
It is: the content of described basalt fibre is the 5-50% of described basalt fibre compound cellulose Multifunctional, air gel rubber material.
Basalt fibre compound cellulose Multifunctional, air gel rubber material preparation method the most according to claim 4, its feature
It is: solvent described in step A is a kind of or several in sodium hydroxide, deionized water, carbamide, thiourea, polyvinyl alcohol, Lithium hydrate
Kind.
Basalt fibre compound cellulose Multifunctional, air gel rubber material preparation method the most according to claim 8, its feature
It is: described solvent is the mixed liquor of sodium hydroxide and deionized water, sodium hydroxide quality accounting 5-15 in described mixed liquor
%。
Basalt fibre compound cellulose Multifunctional, air gel rubber material preparation method the most according to claim 4, its feature
It is: lignocellulose described in step A also needs to through over cleaning and dry run before disperseing.
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Cited By (4)
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CN106830878A (en) * | 2017-01-18 | 2017-06-13 | 加新科技(深圳)有限公司 | A kind of super-hydrophobicity sial zirconium composite material and preparation method thereof |
CN108939387A (en) * | 2018-08-29 | 2018-12-07 | 佛山皖和新能源科技有限公司 | A kind of preparation method of anticorrosion type gel smother agent material |
CN109174021A (en) * | 2018-08-07 | 2019-01-11 | 济南大学 | A kind of preparation method of hydrophobic ionic liquid modified cellulose aeroge coating solid phase micro-extraction fiber |
CN109174020A (en) * | 2018-08-07 | 2019-01-11 | 济南大学 | A kind of preparation method of poly-dopamine modified lithium cellulose aerogels coating solid phase micro-extraction fiber |
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Cited By (8)
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CN106830878A (en) * | 2017-01-18 | 2017-06-13 | 加新科技(深圳)有限公司 | A kind of super-hydrophobicity sial zirconium composite material and preparation method thereof |
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CN109174021A (en) * | 2018-08-07 | 2019-01-11 | 济南大学 | A kind of preparation method of hydrophobic ionic liquid modified cellulose aeroge coating solid phase micro-extraction fiber |
CN109174020A (en) * | 2018-08-07 | 2019-01-11 | 济南大学 | A kind of preparation method of poly-dopamine modified lithium cellulose aerogels coating solid phase micro-extraction fiber |
CN109174021B (en) * | 2018-08-07 | 2021-07-27 | 济南大学 | Preparation method of hydrophobic ionic liquid modified cellulose aerogel coating solid-phase micro-extraction fiber |
CN109174020B (en) * | 2018-08-07 | 2021-07-27 | 济南大学 | Preparation method of polydopamine modified cellulose aerogel coating solid-phase microextraction fiber |
CN108939387A (en) * | 2018-08-29 | 2018-12-07 | 佛山皖和新能源科技有限公司 | A kind of preparation method of anticorrosion type gel smother agent material |
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