CN106007654B - A kind of basalt fibre compound cellulose Multifunctional, air gel rubber material and preparation method thereof - Google Patents
A kind of basalt fibre compound cellulose Multifunctional, air gel rubber material and preparation method thereof Download PDFInfo
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- CN106007654B CN106007654B CN201610349057.1A CN201610349057A CN106007654B CN 106007654 B CN106007654 B CN 106007654B CN 201610349057 A CN201610349057 A CN 201610349057A CN 106007654 B CN106007654 B CN 106007654B
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- basalt fibre
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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
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Abstract
The present invention relates to field of compound material, more particularly to a kind of basalt fibre compound cellulose Multifunctional, air gel rubber material and preparation method thereof；Basalt fibre including the wood fibre as base material phase and as enhancing phase, the wood fibre and the basalt fibre form composite aerogel structure；The invention discloses a kind of basalt fibre compound cellulose Multifunctional, air gel rubber material and preparation method thereof, this material improves mechanical strength, anti-flammability and the ageing resistace of existing cellulose aerogels, use and the range of work of cellulose aerogels are added, substantially increases the security during use and service life；Meanwhile this material can't change the original heat-proof quality of cellulose aerogels and oil absorbency.
Description
Technical field
The present invention relates to field of compound material, more particularly to a kind of basalt fibre compound cellulose Multifunctional, air gel material
Material and preparation method thereof.
Background technology
Aeroge is also known as xerogel.Aeroge refers to when gel sloughs most of solvent, make content liquid ratio in gel
Solids content much less, or the medium being full of in the space net structure of gel are gas, and appearance is in the material of solid-like.Typical case
Aeroge such as gelatin, Arabic gum, silica gel, hair, nail etc..Aeroge also has the property of gel, that is, have expansion, touch
Change effect, synaeresis.Meanwhile aeroge also has the characteristics that nano level loose structure and high porosity, is current known
One of minimum solid material of density.
Because the decentralized 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, and such as high porosity is high
Specific surface area, low heat conduction coefficient, low-k, low optical index, in a low voice speed etc..
Cellulose aerogels, surmount silica aerogel and polymer matrix aeroge, possess traditional aerogel property（Gao Kong
Gap rate, high-specific surface area etc.）While incorporated the excellent properties of itself, such as good biocompatibility and degradability,
Heat-insulation and heat-preservation, crude oil sew etc. that field has great application prospect and raw material easily obtain.Such as application number
CN201510997563.7, apply for 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.The aeroge is prepared by the method comprised the following steps：1) nano-cellulose is scattered in hydrochloric acid and nanometer is made
Cellulose dispersion liquid；2) nano-cellulose dispersion liquid obtained by graphene oxide dispersion and step 1) is mixed, 170~190
Hydro-thermal reaction is carried out at DEG C, obtains hydrogel；3) hydrogel obtained by step 2) is freeze-dried, produced.The present invention provides
Graphene oxide/nano-cellulose aerogel, using nano-cellulose and graphene oxide as raw material, prepared by hydro-thermal reaction
Hydrogel, further by freeze-drying, obtain final products.Compared with graphite oxide aerogel, aeroge Pyrogentisinic Acid
The removal effect of phenol in aqueous solution is more preferable, available for the removal of organic dye molecule in sewage or other impurities, realizes sewage
High-efficient purification.
But cellulose aerogels are due to own material, some defects be present, such as mechanical strength is not good enough, it is durable
Property is general, it is impossible to fire-retardant etc..So a kind of new material is needed, in the base of the existing advantageous property of cellulose-binding aeroge
Preferable mechanical strength and fire resistance are provided simultaneously with plinth.
The content 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 solves
The problem of existing cellulose aerogels mechanical strength is small.
What the present invention was realized in：A kind of basalt fibre compound cellulose Multifunctional, air gel rubber material, its feature exist
In：Basalt fibre including the wood fibre as base material phase and as enhancing phase, the wood fibre and the Black Warrior
Rock fiber forms composite aerogel structure.Basalt fibre（CBF）It is a kind of nothing for passing through research and development in more than 30 years by the former Soviet Union
Machine fiber is basalt building stones after 1450 DEG C~1500 DEG C meltings, is formed by platinum-rhodium alloy bushing high speed pulling
Continuous fiber, intensity are suitable with high intensity S glass fibres.The color of pure natural basalt fibre is generally brown, and some are like gold
Color.Basalt fibre is a kind of novel inorganic environment-friendly and green high performance fibre material, and it is by silica, aluminum oxide, oxidation
The basalt building stones of the oxides such as calcium, magnesia, iron oxide and titanium dioxide composition are quickly drawn after high-temperature fusion by bushing
What system formed.Basalt fibre, not only intensity is high for basalt continuous fiber, but also with electric insulation, corrosion-resistant, high temperature resistant etc.
A variety of excellent properties.Temperature tolerance is higher than all organic fibers, and has the advantages that noninflammability, without thermal contraction phenomenon.It is a kind of
Outstanding can be used for compound material.In addition, the production technology of basalt fibre determines that caused discarded object is few, it is dirty to environment
Contaminate small, and directly can in the environment be degraded after product abandonment, without any harm, thus be a kind of qualified green, environmental protection
Material.
Also cellulose fiber peacekeeping basalt fibre is not combined with each other to form the note of composite aerogel in the prior art
Carry.Basalt fibre provides high temperature resistant and high definition performance for aeroge, while will not be reduced after basalt fibre is added
The heat-proof quality and oil absorbency of cellulose aerogels script.
The present invention further technical scheme be：The mm of length 0.1-10 of the wood fibre.The length of wood fibre
There is considerable influence to the bulk properties of the basalt fibre compound cellulose Multifunctional, air gel rubber material.
The present invention further technical scheme be：The length of the basalt fibre is 0.1-20 mm.Basalt fibre
Length has decisive influence to the mechanical property of the 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, lignocellulosic is scattered in solvent by the substrate solution preparation process system to be obtained
Substrate solution；
B. hydrogel preparation process, the hydrogel preparation process system is by the substrate solution and basalt fibre complex
Into hydrogel；
C. freezing gel preparation process, it is solidifying that the freezing gel preparation process system obtains freezing after the hydrogel is freezed
Glue, cryogenic temperature are -10 ~ -30 DEG C, and cooling time is 0.5-30 h；
D. aeroge preparation process, the aeroge preparation process system obtain airsetting after the freezing gel is freeze-dried
Glue, the condenser temperature of freeze-drying is -50 ~ -70 DEG C, and vacuum is 10-1000 Pa, and drying time is 0.5-50 h.
The present invention further technical scheme be：The step B include it is following step by step：
The basalt fibre is added the base by B1. mixed solution preparation process, the mixed solution preparation process system
In material solution, mixed solution is obtained；
B2. hydrogel solution preparation process, the hydrogel solution preparation process, which ties up to add in the mixed solution, divides
Powder and water-repelling agent obtain hydrogel solution；
B3. the hydrogel solution is dispersed and form hydrogel by ultrasound or mechanical agitation, wherein machinery stirs
The frequency mixed is 500-5000 rpm, and mixing time is 0.5-20 h.
The present invention further technical scheme be：The step B include it is following step by step：
B1. skeleton preparation process, the skeleton preparation process system is by the roving, fibrofelt or fiber of basalt fibre
Cloth establishment turns into skeleton framework；
B2. hydrogel solution preparation process, the hydrogel solution preparation process, which is tied up in the base material, adds dispersant
Hydrogel solution is obtained with water-repelling agent；
B3. the skeleton framework and the hydrogel solution are compounded to form hydrogel.
The present invention further technical scheme be：The content of the basalt fibre is the basalt fibre composite fibre
The 5-50% of plain Multifunctional, air gel rubber material.Basalt fibre content is to the multi-functional airsetting of basalt fibre compound cellulose
The mechanical property of glue material has considerable influence.
The present invention further technical scheme be：Solvent described in step A is sodium hydroxide, deionized water, urea, sulphur
It is one or more of in urea, polyvinyl alcohol, lithium hydroxide.
Preferably, the solvent is the mixed liquor of sodium hydroxide and deionized water, sodium hydroxide quality in the mixed liquor
The % of accounting 5-15.
The present invention further technical scheme be：Lignocellulosic described in step A carry out it is scattered before also need to by
Cleaning and drying process.
The beneficial effects of the invention are as follows：The invention discloses a kind of basalt fibre compound cellulose Multifunctional, air gel material
Material and preparation method thereof, this material improves mechanical strength, anti-flammability and the ageing resistace of existing cellulose aerogels, increase
The use of cellulose aerogels and the range of work, substantially increase the security during use and service life；Meanwhile this
Material can't change the original heat-proof quality of cellulose aerogels and oil absorbency.
Embodiment
Contrast specific embodiment one
Cellulose fibre is added in appropriate solution, addition dispersant, water-repelling agent and crosslinking agent, mechanical agitation 3h,
3000rpm, at a temperature of 80 DEG C, form gel mixed solution.Freezed 3 hours under -20 DEG C of low temperature, condenser temperature -60 is set
DEG C, suction to 50Pa, then start to be freeze-dried 30h, 50 DEG C of freeze temperature.
The cellulose aerogels prepared, thermal conductivity factor are 0.017W/ (m K), tensile strength 10MPa；Run into naked light,
Light within 3 seconds；200 DEG C of degradations 72 hours, structure collapses；Saturation oil suction is 112 times of deadweight.
Specific embodiment one.
It is 5 in mass ratio：95 mix sodium hydroxide and deionized water as solution for standby.In mass ratio 10:90 will be profound
Military rock chopped strand and cellulose fibre are added in solution, addition dispersant, water-repelling agent and crosslinking agent, mechanical agitation 3h,
3000rpm, at a temperature of 80 DEG C, form gel mixed solution.Freezed 3 hours under -20 DEG C of low temperature, condenser temperature -60 is set
DEG C, suction to 50Pa, then start to be freeze-dried 30h, 50 DEG C of freeze temperature.
Basalt-the cellulose aerogels prepared, thermal conductivity factor are 0.015W/ (m K), tensile strength 30MPa；It is difficult
To light, under alcolhol burner, after about 1 minute, just start to burn；Degradation 72 hours, size appearance is without significant change；Saturation
Oil suction is 101 times of deadweight.
Specific embodiment two.
To in mass ratio 30:70 are added to basalt chopped fiber and cellulose fibre in solution, and other conditions are the same as real
Apply example 1.
Basalt-the cellulose aerogels prepared, thermal conductivity factor are 0.016W/ (m K), tensile strength 47MPa；It is difficult
To light, under alcolhol burner, after contacting aeroge, after 3 minutes, ability starting point combustion gas gel, degradation 72 hours, size appearance
Without significant change；Saturation oil suction is 81 times of deadweight.
Specific embodiment three.
To in mass ratio 50:50 are added to basalt chopped fiber and cellulose fibre in solution, and other conditions are the same as real
Apply example 1.
Basalt-the cellulose aerogels prepared, thermal conductivity factor are 0.018W/ (mK), tensile strength 67
MPa；It is difficult to light, under alcolhol burner, after contacting aeroge, self-extinguishment, degradation 72 hours, size appearance is without significant change；It is full
76 times with oil suction for deadweight.
Specific embodiment four.
It is 10 in mass ratio：90 mix sodium hydroxide and deionized water, as solution for standby.Cellulose fibre is added
Into solution, dispersant, water-repelling agent and crosslinking agent are added, at a temperature of 3h, 3000rpm, 80 DEG C of mechanical agitation, form gel
Mixed solution, one layer of basalt fiber cloth is placed respectively in sample tray bottom and top.Freezed 3 hours under -20 DEG C of low temperature,
- 60 DEG C of condenser temperature is set, suction to 50Pa, then starts to be freeze-dried 30h, 50 DEG C of freeze temperature.
Basalt-the cellulose aerogels prepared, thermal conductivity factor are 0.016W/ (m K), tensile strength 110MPa；
It can not light；Degradation 72 hours, size appearance is without significant change；Saturation oil suction is 98 times of deadweight.
Specific embodiment five
It is 15 in mass ratio：85 mix sodium hydroxide and deionized water, as solution for standby.Cellulose fibre is added
Into solution, dispersant, water-repelling agent and crosslinking agent are added, at a temperature of 3h, 3000rpm, 80 DEG C of mechanical agitation, form gel
Mixed solution, in sample tray bottom and top and middle one layer of 0.5mm thickness basalt fiber cloth of placement respectively.At -20 DEG C
Freezed 3 hours under low temperature, -60 DEG C of condenser temperature is set, suction to 50Pa, then starts to be freeze-dried 30h, freeze temperature
50℃。
Basalt-the cellulose aerogels prepared, thermal conductivity factor are 0.020W/ (mK), and tensile strength is
120MPa；It can not light；Degradation 72 hours, size appearance is without significant change；Saturation 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 mechanical strength, anti-flammability and the ageing resistace of existing cellulose aerogels, adds making for cellulose aerogels
With and the range of work, substantially increase the security during use and service life；Meanwhile this material can't change fiber
The original heat-proof quality of plain aeroge and oil absorbency.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the invention, all essences in the present invention
All any modification, equivalent and improvement made within refreshing and principle etc., should be included in the scope of the protection.
Claims (10)
- A kind of 1. basalt fibre compound cellulose Multifunctional, air gel rubber material preparation method, it is characterised in that：Including following step Suddenly：A. substrate solution preparation process, the substrate solution preparation process system by wood fibre be scattered in solvent obtain base material it is molten Liquid；The substrate solution and basalt fibre are compounded to form water by B. hydrogel preparation process, the hydrogel preparation process system Gel；C. freezing gel preparation process, the freezing gel preparation process system obtain freezing gel after the hydrogel is freezed, Cryogenic temperature is -10 ~ -30 DEG C, and cooling time is 0.5-30 h；D. aeroge preparation process, the aeroge preparation process system obtain aeroge after the freezing gel is freeze-dried, The condenser temperature of freeze-drying is -50 ~ -70 DEG C, and vacuum is 10-1000 Pa, and drying time is 0.5-50 h.
- 2. basalt fibre compound cellulose Multifunctional, air gel rubber material preparation method according to claim 1, its feature It is：The step B include it is following step by step：B1. mixed solution preparation process, the mixed solution preparation process system are molten by the basalt fibre addition base material In liquid, mixed solution is obtained；B2. hydrogel solution preparation process, the hydrogel solution preparation process, which is tied up in the mixed solution, adds dispersant Hydrogel solution is obtained with water-repelling agent；B3. it is the hydrogel solution is dispersed and form hydrogel by ultrasound or mechanical agitation, wherein churned mechanically Frequency is 500-5000 rpm, and mixing time is 0.5-20 h.
- 3. basalt fibre compound cellulose Multifunctional, air gel rubber material preparation method according to claim 1, its feature It is：The step B include it is following step by step：B1. the roving, fibrofelt or fiber cloth of basalt fibre are compiled by skeleton preparation process, the skeleton preparation process system It is made for skeleton framework；B2. hydrogel solution preparation process, the hydrogel solution preparation process, which is tied up in the base material, to be added dispersant and dredges Aqua obtains hydrogel solution；B3. the skeleton framework and the hydrogel solution are compounded to form hydrogel.
- 4. basalt fibre compound cellulose Multifunctional, air gel rubber material preparation method according to claim 1, its feature It is：The content of the basalt fibre is the 5-50% of the basalt fibre compound cellulose Multifunctional, air gel rubber material.
- 5. basalt fibre compound cellulose Multifunctional, air gel rubber material preparation method according to claim 4, its feature It is：Solvent described in step A is a kind of or several in sodium hydroxide, deionized water, urea, thiocarbamide, polyvinyl alcohol, lithium hydroxide Kind.
- 6. basalt fibre compound cellulose Multifunctional, air gel rubber material preparation method according to claim 5, its feature It is：The solvent is the mixed liquor of sodium hydroxide and deionized water, sodium hydroxide quality accounting 5-15 in the mixed liquor %。
- 7. basalt fibre compound cellulose Multifunctional, air gel rubber material preparation method according to claim 1, its feature It is：Wood fibre described in step A is also needed to through over cleaning and drying process before disperse.
- 8. a kind of usage right requires basalt fibre compound cellulose Multifunctional, air made from 1 to 7 any one preparation method Gel rubber material, it is characterised in that：Basalt fibre including the wood fibre as base material phase and as enhancing phase, the wood Matter fiber and the basalt fibre form composite aerogel structure.
- It is 9. according to claim 8, it is characterised in that：The mm of length 0.1-10 of the wood fibre.
- It is 10. according to claim 8, it is characterised in that：The length of the basalt fibre is 0.1-20 mm.
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| CN106830878B (en) * | 2017-01-18 | 2018-04-06 | 加新科技(深圳)有限公司 | A kind of super-hydrophobicity sial zirconium composite material and preparation method thereof |
| CN109174020B (en) * | 2018-08-07 | 2021-07-27 | 济南大学 | Preparation method of polydopamine modified cellulose aerogel coating solid-phase microextraction 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 |
| CN108939387B (en) * | 2018-08-29 | 2021-06-22 | 深圳市骏丰木链网科技股份有限公司 | Preparation method of corrosion-resistant gel extinguishing agent material |
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| CN101880410B (en) * | 2010-07-21 | 2014-08-13 | 武汉大学 | High-strength transparent cellulose material and preparation method thereof |
| US9975270B2 (en) * | 2010-07-30 | 2018-05-22 | Rockwool International A/S | Method for manufacturing an aerogel-containing composite and composite produced by that method |
| CN102443180A (en) * | 2011-09-15 | 2012-05-09 | 复旦大学 | Method for preparing cellulose composite aerogel |
| CN103709435B (en) * | 2013-12-19 | 2016-01-20 | 东北林业大学 | A kind of preparation method of light-weight high-intensity cellulose aerogel |
| CN104945004B (en) * | 2015-06-15 | 2017-11-07 | 利津慈母坊纺织科技有限公司 | A kind of composite of New Regenerated Cellulosic Fibers aeroge and preparation method thereof |
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