CN108276588A - A kind of preparation method of aramid nano-fiber water-dispersed/nano-cellulose compound system and ultraviolet shielded type transparent membrane - Google Patents
A kind of preparation method of aramid nano-fiber water-dispersed/nano-cellulose compound system and ultraviolet shielded type transparent membrane Download PDFInfo
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- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
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Abstract
The invention discloses the preparation methods of a kind of aramid nano-fiber water-dispersed/nano-cellulose compound system and ultraviolet shielded type transparent membrane, first passage addition has the aramid nano-fiber of excellent thermodynamic stability energy, uv-shielding capacity on a small quantity, by nano-cellulose and aramid nano-fiber by high shear and redisperse skill uniformly mix with dispersion, by ultrasound degassing, be filtered by vacuum, low temperature drying and etc. obtain the ultraviolet shielded nanofiber laminated film with certain transparency.The present invention uses natural plant fibre for base stock, reduces production cost, the problems such as efficiently solving toxic, difficult to degrade present in ultraviolet shielded material at this stage.The thermodynamic property of composite material and excellent uv-shielding capacity are significantly improved using synthesis aramid nano-fiber simultaneously.Preparation process of the present invention is simple, of low cost, has excellent performance and degradable green, has broad application prospects.
Description
Technical field
The invention belongs to technical field of composite materials, and in particular to a kind of aramid nano-fiber/nano-cellulose water-dispersed
The preparation method of compound system and ultraviolet shielded type transparent membrane.
Background technology
With the movable aggravation of mankind's modern industrialization, the ozone layer of 99% ultraviolet light in air is can absorb by serious
Ground destroys.Excessive ultraviolet radiation not only results in high-molecular organic material on the earth and degradation and aging occurs, more serious
Skin cancer can also be suffered from by being mankind itself.
It is endangered caused by ultraviolet radioactive to reduce to the greatest extent, ultraviolet shielded material becomes research hotspot in recent years.According to
Shielding principle, ultraviolet shielded material can be divided into ultraviolet reflectance agent and ultraviolet absorber.Currently, ultraviolet reflectance agent is applied than wide
Be with high index (nanometer) inorganic, metal oxide such as zinc oxide, (nanometer) titanium dioxide and silica etc.；
Ultraviolet absorber is mainly the chromophoric group for having the absorbing wavelength being connected on aromatic derivant to be less than 400nm on molecular structure
Or the organic compound of auxochrome group such as benzophenone, benzotriazole and oxanilide etc..It is ultraviolet under action of ultraviolet radiation
Reflection-type shielding material light and heat stability, catalytic activity is high, but there is difficult dispersion, and the low and ultraviolet shielded wave band of transparency is narrow
The problem of.In addition, aging and degradation occur for the dispersate crossed where high catalytic activity also results in it, further make material itself
Service life is reduced, uv-shielding capacity is damaged.In contrast, UV absorption type shielding material shield effectiveness is high, the transparency is good, still
Part has toxicity and resistance to light thermal property is poor, this is also the current major reason for hindering the development of UV absorption type shielding material.
Therefore, seek a kind of green transparent, resistance to photo-thermal, compel in eyebrow in ultraviolet all band all ultraviolet shielded materials with high shield effectiveness
Eyelash.
Cellulose is that one kind passing through linear natural height made of β -1-4 glycosidic bonds are connected with each other by D- glucopyranose units
Molecular material has the characteristics that feed distribution wide, degradable green, reproducible.In recent years, it is pushed in the high speed of nanotechnology
Under, nano-cellulose constructs primitive as a kind of important nanometer, because with big L/D ratio, high-specific surface area, high surface
It is widely used in the Material Fields such as transparent membrane, Flexible Displays and heat-insulation and heat-preservation with excellent mechanical property.Based on nanometer ruler
Very little specific nano effect and its molecular structure feature, although pure nano-cellulose thin-film material is presented under natural visible light
High transparency, however in practical applications, nano-cellulose leads to final thin-film material to the high susceptibility of ambient humidity
Mechanical property is far below theoretical performance.In addition, nano-cellulose absorbed in sunlight ultraviolet band it is less, this strongly limits
The possibility that nano-cellulose is applied in the ultraviolet shielded material of high transparency.
Aramid nano-fiber (a diameter of 5-30nm) is that a kind of high-performance relatively new in recent years synthesizes nanometer primitive material
Material.The lateral hydrogen bond and model ylid bloom action power broken in ring macroscopic view aramid fiber molecular structure, aramid nano-fiber are oriented by alkali solution technique
Inherit macroscopical aramid fiber major part structure and performance (molecular structure and chemical constitution, mechanical property and thermal stability).
It is different from macroscopical aramid fiber, aramid nano-fiber has big L/D ratio and high-specific surface area, the abundant active group in surface
Mix laying a good foundation with crosslinking with other polar materials for aramid nano-fiber.In addition, aramid fiber belongs to aromatic series
One of derivative is connected with the amido bond that abundant absorbing wavelength is less than 400nm on molecular structure, can be in ultraviolet all band area
Show excellent uv-shielding capacity.Therefore, aramid nano-fiber, as a kind of novel transparent ultraviolet absorber ultraviolet
Shielding material has a wide range of applications in field.
Invention content
The purpose of the present invention is to provide a kind of aramid nano-fiber water-dispersed/nano-cellulose compound system and ultraviolet screens
The preparation method for covering type transparent membrane, to overcome the problems of the above-mentioned prior art, present invention efficiently solves at this stage
Transparency present in ultraviolet shielded material is low, difficult dispersion, ultraviolet band absorption bands are narrow, toxic technical barrier difficult to degrade.
In order to achieve the above objectives, the present invention adopts the following technical scheme that：
A kind of preparation method of aramid nano-fiber water-dispersed/nano-cellulose compound system, includes the following steps：
(1) para-aramid fiber X, potassium hydroxide, dimethyl sulfoxide (DMSO) are placed in container, are dispersed with stirring, is scattered in
Aramid nano-fiber dispersion liquid A under KOH/DMSO systems；
(2) the aramid nano-fiber dispersion liquid A being scattered under KOH/DMSO systems obtained in step (1) is carried out dilute
It releases, obtains evenly dispersed aramid nano-fiber dispersion liquid B；
(3) deionized water is added in nano-cellulose Y and is stirred dispersion, obtained evenly dispersed nano-cellulose and suspend
Liquid C；
(4) the nano-cellulose suspension C that will be obtained in step (3), under the high shear forces that stirring generates, Xiang Qigao
The aramid nano-fiber dispersion liquid B obtained in pressure injecting step (2), obtains being scattered in KOH/DMSO/H2Virtue in O mixed systems
Synthetic fibre nanofiber/nano-cellulose dispersion liquid D；
(5) it is scattered in KOH/DMSO/H by what is obtained in step (4)2Aramid nano-fiber/Nanowire in O mixed systems
Element dispersion liquid D is tieed up by vacuum filtration, obtains mixing nanofiber E；
(6) the mixing nanofiber E obtained in step (5) is washed repeatedly by absolute ethyl alcohol and deionized water, is obtained
Colloidal mixing nanofiber F；
(7) the colloidal mixing nanofiber F obtained in step (6) is scattered in deionized water again under stirring
In, obtain aramid nano-fiber water-dispersed/nano-cellulose compound system.
Further, para-aramid fiber X, potassium hydroxide and dimethyl sulfoxide (DMSO) ratio are 1g in step (1)：1.5g：
500ml, the para-aramid fiber X are p-aramid fiber yarn fibers, p-aramid fiber chopped strand, para-aramid pulp fiber
With one kind in p-aramid fiber fibrid.
Further, in step (2) using DMSO to the aramid nano-fiber dispersion liquid A that is scattered under KOH/DMSO systems
It is diluted, a concentration of 0.1mg/mL of obtained aramid nano-fiber dispersion liquid B.
Further, the mass concentration of nano-cellulose suspension C is 1% in step (3), the nano-cellulose Y
For the nanocrystal cellulose obtained by chemical oxidation treatment, the processing of chemical pretreatment conjunction with mechanical or chemical sour water solution.
Further, the injection of step (4) mesohigh is to utilize stainless steel high-pressure spray pump, and jet pressure is 5~15MPa,
Effluxvelocity is 0.2~2.0mL/s；What step (4) obtained is scattered in KOH/DMSO/H2Aramid fiber Nanowire in O mixed systems
The mass ratio of aramid nano-fiber and nano-cellulose is (1~8) in dimension/nano-cellulose dispersion liquid D：100.
Further, the filter membrane that vacuum filtration uses in step (5) is 500 mesh nylon leaching film；Washing nothing in step (6)
The volume of water-ethanol and the ratio for mixing nanofiber E mass are 1mL:5mg~1mL:2mg；The washing deionized water with it is mixed
The mass ratio for closing nanofiber E is 10:1~5:1.
Further, the dispersion concentrations of colloid mixing nanofiber F in deionized water are 0.5~5mg/ in step (7)
mL。
Further, stirring refers to being stirred 5~8 days at a temperature of 30~60 DEG C under air-proof condition in step (1)；Step
Suddenly mix rotating speed is 1000rpm, mixing time 12h in (3) step, and speed of agitator is 600~3000rpm in step (4)；Step
(7) agitation revolution is 500~2500rpm, 30~180min of mixing time in.
It is a kind of transparent using above-mentioned aramid nano-fiber water-dispersed/nano-cellulose compound system prepares ultraviolet shielded type
The method of film, includes the following steps：
Step 1：Ultrasound degassing：Aramid nano-fiber water-dispersed/nano-cellulose compound system is placed in ultrasonic cleaning machine
Middle ultrasound degassing process；
Step 2：Vacuum filtration：The aramid nano-fiber that step 1 is obtained/nano-cellulose compound system is in recirculated water
Aramid nano-fiber/nano-cellulose compounded wet film, forming quality a concentration of 0.02% are obtained under the swabbing action of power vacuum pump
~0.06%；
Step 3：Squeeze drying：Aramid nano-fiber/nano-cellulose compounded wet film that step 2 obtains is placed in squeezing
Machine squeezes and is dried to obtain ultraviolet shielded type transparent membrane.
Further, the ultrasonic degassing process time is 10~20min in step 1；Vacuum filter pressure described in step 2
For 0.5~1MPa, the suction filtration time is 2~10min, and filter membrane is 500 mesh nylon leaching films；Condition is squeezed in step 3 is：Squeezing pressure
0.2~1.0MPa of power squeezes 3~20min of time；Drying condition is：Drying temperature：70 DEG C, 48~75h of drying time.
Compared with prior art, the present invention has technique effect beneficial below：
The aramid nano-fiber that the present invention uses has excellent mechanical property and thermal stability, the aramid fiber Nanowire of preparation
The characteristic that film has high-strength, high transparency, ultraviolet shielded effect good is tieed up, preparation process is simple, nanofiber purity is high, draw ratio
Greatly.The present invention is using a small amount of aramid nano-fiber as ultraviolet absorber, hydrogen bond crosslinks agent and the nano-cellulose haveing excellent performance
High efficiency composition is carried out to prepare a kind of not high to ambient humidity sensibility while there is excellent mechanical property and thermal stability
Transparent ultraviolet shielded type laminated film.
In order to realize uniformly mix and disperseing for aramid nano-fiber and nano-cellulose, high speed shear and redisperse are utilized
Technology, the medium for two kinds being scattered in different solvents system first passes through hydrogen bond and model ylid bloom action power is effectively crosslinked, so
ANF/NCF blending agents are scattered in again in purely inorganic system, no according to exchange of solvent principle during redisperse afterwards
Influence of the solvation (DMSO) to nano-cellulose is only greatly reduced, is also stored, again for the steady in a long-term of blending agent
Using and other have the mixing of inorganic system to provide important technical support with dispersion the later stage.
The present invention is carried out two kinds of nanometer elementary materials with different performance using simple and effective nanometer hybrid technology
It is compound to prepare a kind of ultraviolet shielded type transparent material of green, breach traditional natural plant fibre and synthetic fibers compatibility
Difference, difficult compound bottleneck, provide a kind of new thinking and method to prepare nano-cellulose base high-performance composite material, promote
Multifunctional application of the nano-cellulose in modernization field.
Description of the drawings
Fig. 1 is the techniqueflow schematic diagram of the present invention；
Fig. 2 is the pure NFC figures prepared by the present invention；
Fig. 3 is the ANF/NFC laminated film figures that the ANF additive amounts prepared by the present invention are 1%；
Fig. 4 is that the ultraviolet-visible light of the pure nano-cellulose film of comparative example and embodiment 1-5ANF/NFC laminated films is saturating
Penetrate spectrogram.
Specific implementation mode
Embodiments of the present invention are described in further detail below：
A kind of preparation method of aramid nano-fiber water-dispersed/nano-cellulose compound system, includes the following steps：
(1) para-aramid fiber X, potassium hydroxide, dimethyl sulfoxide (DMSO) are placed in container, are dispersed with stirring, is scattered in
Aramid nano-fiber dispersion liquid A under KOH/DMSO systems；
Wherein, para-aramid fiber X, KOH and DMSO ratios are 1g：1.5g：500mL；The stirring refers to sealing
Under the conditions of, it is stirred 5~8 days at a temperature of 30~60 DEG C；The para-aramid fiber X is p-aramid fiber yarn fibers, contraposition
One kind in aramid short fiber, para-aramid pulp fiber and p-aramid fiber fibrid；
(2) aramid nano-fiber being scattered under KOH/DMSO systems obtained in step (1) is diluted processing, obtained
To evenly dispersed aramid nano-fiber dispersion liquid B；
Wherein, use diluent for DMSO, the volumetric concentration of aramid nano-fiber dispersion liquid is 0.1mg/mL after dilution；
(3) deionized water is added in nano-cellulose Y and is stirred dispersion, obtained evenly dispersed nano-cellulose and suspend
Liquid C；
Wherein, nano-cellulose suspension quality a concentration of 1%, mixing speed 1000rpm, mixing time 12h, institute
The nano-cellulose Y stated is by chemical oxidation (TEMPO oxidations) processing, the processing of chemical pretreatment conjunction with mechanical and chemical sour water
One kind in the nanocrystal cellulose that solution obtains；
(4) the nano-cellulose suspension that will be obtained in step (3), under the high shear forces that stirring generates, Xiang Qigao
The aramid nano-fiber dispersion liquid obtained in pressure injecting step (2), obtains being scattered in KOH/DMSO/H2Virtue in O mixed systems
Synthetic fibre nanofiber/nano-cellulose dispersion liquid D；
Wherein, high shear speed of agitator is 600~3000rpm；The high-pressure injection is to utilize stainless steel high-pressure jet
Pump, jet pressure are 5~15MPa, and effluxvelocity is 0.2~2.0mL/s；The aramid nano-fiber and nano-cellulose
Mass ratio is 1~8:100；
(5) it is scattered in KOH/DMSO/H by what is obtained in step (4)2Aramid nano-fiber/Nanowire in O mixed systems
The plain dispersion liquid of dimension obtains mixing nanofiber E by vacuum filtration；
Wherein, the filter membrane used is filtered by vacuum as 500 mesh nylon leaching films；
(6) the mixing nanofiber obtained in step (5) is washed repeatedly by absolute ethyl alcohol and deionized water, obtains glue
Body shape mixing nanofiber F；
Wherein, the ratio of the volume of washing absolute ethyl alcohol and mixing nanofiber quality is 1mL:5mg~1mL:2mg is washed
It is 3~5 times to wash number；The washing deionized water is 10 with the mass ratio for mixing nanofiber:1~5:1；
(7) the colloidal mixing nanofiber obtained in step (6) is scattered in deionized water again under stirring
In, obtain aramid nano-fiber water-dispersed/nano-cellulose compound system：
Wherein, the dispersion concentration of colloid mixing nanofiber in deionized water is 0.5~5mg/mL；The agitation revolution
For 500~2500rpm, 30~180min of mixing time.
It is a kind of that ultraviolet shielded type transparent membrane is prepared using aramid nano-fiber water-dispersed/nano-cellulose compound system
Method includes the following steps：
Step 1：Ultrasound degassing：Aramid nano-fiber water-dispersed/nano-cellulose compound system is placed in ultrasonic cleaning machine
Middle ultrasound degassing process 10-20min；
Step 2：Vacuum filtration：The aramid nano-fiber that step 1 is obtained/nano-cellulose compound system is in recirculated water
Aramid nano-fiber/nano-cellulose compounded wet film, forming quality a concentration of 0.02% are obtained under the swabbing action of power vacuum pump
~0.06%, the suction filtration condition is：Suction filtration pressure is 0.5~1MPa, and the suction filtration time is 2~10min, and filter membrane is 500 mesh Buddhist nuns
Imperial filter membrane；
Step 3：Squeeze drying：Aramid nano-fiber/nano-cellulose composite fibre wet film that step 2 obtains is placed in
Squeezer squeezes and is dried to obtain ultraviolet shielded type aramid nano-fiber/nano-cellulose transparent membrane；The squeezing condition is：
0.2~1.0MPa of squeeze pressure squeezes 3~20min of time；The drying condition is：Drying temperature：70 DEG C, drying time 48
~75h.
The present invention uses natural plant fibre for base stock, reduces production cost, efficiently solves ultraviolet at this stage
The problems such as toxic, difficult to degrade present in shielding material.Composite material is significantly improved using synthesis aramid nano-fiber simultaneously
Thermodynamic property and excellent uv-shielding capacity.Composite material prepared by the present invention is given birth to current Conventional UV shielding material
Production is compared, and preparation process is simple, of low cost, is had excellent performance and degradable green, is had broad application prospects.In addition, this
Used high speed shear and redisperse technology are invented to there is the uniform mixing of inorganic system to provide important technology with dispersion
It uses for reference and supports.
The present invention is described in further detail with reference to embodiment：
Comparative example
Step 1：12h is stirred under the action of being 1000rpm by the nano-cellulose low whipping speed that mass concentration is 1%,
Obtain evenly dispersed nano-cellulose suspension；
Step 2：The nano-cellulose suspension that step 1 is obtained is by ultrasound degassing 10min, then in vacuum pressure
The pure NCF wet films of forming quality a concentration of 0.06% are obtained to filter 2min under conditions of 0.5MPa；
Step 3：The wet film that step 2 obtains is squeezed into 3min under the conditions of squeeze pressure is 0.2MPa；
Step 4：Dry 48h at the wet film that step 3 is obtained is 70 DEG C in drying temperature, obtains pure NCF films, such as
Shown in Fig. 2.
At room temperature, it is detected using the ultraviolet-visible spectrophotometer laminated film obtained to this implementation.Inspection
It surveys the result shows that (Fig. 4), ANF/NFC laminated films especially 300-800nm in entire ultraviolet-visible optical band have higher
Transmissivity (up to 90%), cannot preferably meet wanting for the high uv-shielding capacity of material although being presented high transparency feature
It asks.
Embodiment 1
(1) 1g p-aramid fibers yarn fibers, 1.5g potassium hydroxide and 500ml dimethyl sulfoxide (DMSO)s are placed in container, close
It under the conditions of envelope, is stirred 8 days at a temperature of 30 DEG C, obtains the aramid nano-fiber dispersion liquid A being scattered under KOH/DMSO systems；
(2) aramid nano-fiber being scattered under KOH/DMSO systems obtained in step (1) is diluted with DMSO,
Obtain the aramid nano-fiber dispersion liquid B that equal volumetric concentration is 0.1mg/mL；
(3) work that deionized water low whipping speed is 1000rpm is added in the nano-cellulose for obtaining chemical sour water solution
With lower stirring 12h, the nano-cellulose suspension C that evenly dispersed mass concentration is 1% is obtained；
(4) the nano-cellulose suspension C that will be obtained in step (3), under the action of speed of agitator is 600rpm, Xiang Qi
The mass ratio of the aramid nano-fiber dispersion liquid obtained in high-pressure injection step (2), aramid nano-fiber and nano-cellulose is
1:100, jet pressure 5MPa, effluxvelocity 0.2ml/s obtain being scattered in KOH/DMSO/H2Aramid fiber in O mixed systems
Nanofiber/nano-cellulose dispersion liquid D；
(5) it is scattered in KOH/DMSO/H by what is obtained in step (4)2Aramid nano-fiber/Nanowire in O mixed systems
The plain dispersion liquid of dimension is filtered by vacuum by the nylon leaching film of 500 mesh, obtains aramid nano-fiber/nano-cellulose composite fibre E；
(6) the mixing nanofiber obtained in step (5) is washed 3 repeatedly respectively by absolute ethyl alcohol and deionized water
Secondary, the ratio of the volume of absolute ethyl alcohol needed for washing and mixing nanofiber quality is 1ml every time:5mg, required deionized water with it is mixed
The mass ratio for closing nanofiber is 5:1, obtain colloidal mixing nanofiber F；
(7) the colloidal mixing nanofiber obtained in step (6) is stirred under the stirring action of 500rpm
30min, dispersion concentration are controlled in 0.5mg/ml, obtain aramid nano-fiber water-dispersed/nano-cellulose compound system G：
It is a kind of in the present embodiment to utilize the aramid nano-fiber water-dispersed/nano-cellulose complex prepared by the above method
System prepares the preparation method of ultraviolet shielded type nano-cellulose based transparent film, including following preparation process：
Step 1：Ultrasound degassing：Dispersion aramid nano-fiber/nano-cellulose compound system of above-mentioned preparation is placed in super
Ultrasonic degassing process 12min in sound washer；
Step 2：Vacuum filtration：The aramid nano-fiber that step 1 is obtained/nano-cellulose compound system is filtering pressure
Power filters 3min under the conditions of being 0.6MPa, obtains aramid nano-fiber/nano-cellulose compounded wet film, forming quality is a concentration of
0.05%；
Step 3：Squeeze drying：Aramid nano-fiber/nano-cellulose compounded wet film that step 2 obtains is placed in squeezing
Machine is squeezed and is dried, and squeezing condition is：Squeeze pressure 0.2MPa squeezes time 7min；Drying condition is：Drying temperature：70 DEG C,
Drying time 55h.
At room temperature, it is examined using the ultraviolet-visible spectrophotometer laminated film (Fig. 3) obtained to this implementation
It surveys.Testing result shows (Fig. 4), ANF/NFC laminated films in visible-range when ANF additive amounts are 1%, although
Transparency is declined slightly, but still maintains higher transmitance (up to 88%), however compares purer NCF, and composite membrane exists
Ultra-violet (UV) band 200nm-400nm wave bands are through rate and significantly decline (down to 5%), further illustrate the addition of a small amount of ANF
Significantly improve the uv-shielding capacity of NCF films.
Embodiment 2
(1) 1.0g p-aramid fibers chopped strand, 1.5g potassium hydroxide and 500ml dimethyl sulfoxide (DMSO)s are placed in container,
It under air-proof condition, is stirred 7 days at a temperature of 40 DEG C, obtains the aramid nano-fiber dispersion liquid A being scattered under KOH/DMSO systems；
(2) aramid nano-fiber being scattered under KOH/DMSO systems obtained in step (1) is diluted with DMSO,
Obtain the aramid nano-fiber dispersion liquid B that equal volumetric concentration is 0.1mg/mL；
(3) deionized water low whipping speed is added in the nano-cellulose that chemical pretreatment conjunction with mechanical is handled is
12h is stirred under the action of 1000rpm, obtains the nano-cellulose suspension C that evenly dispersed mass concentration is 1%；
(4) the nano-cellulose suspension C that will be obtained in step (3), under the action of speed of agitator is 1000rpm, to
The aramid nano-fiber dispersion liquid obtained in its high-pressure injection step (2), the mass ratio of aramid nano-fiber and nano-cellulose
It is 3:100, jet pressure 7MPa, effluxvelocity 0.5ml/s obtain being scattered in KOH/DMSO/H2Virtue in O mixed systems
Synthetic fibre nanofiber/nano-cellulose dispersion liquid D；
(5) it is scattered in KOH/DMSO/H by what is obtained in step (4)2Aramid nano-fiber/Nanowire in O mixed systems
The plain dispersion liquid of dimension is filtered by vacuum by the nylon leaching film of 500 mesh, obtains aramid nano-fiber/nano-cellulose composite fibre E；
(6) the mixing nanofiber obtained in step (5) is washed 4 repeatedly respectively by absolute ethyl alcohol and deionized water
Secondary, the ratio of the volume of absolute ethyl alcohol needed for washing and mixing nanofiber quality is 1ml every time:2mg, required deionized water with it is mixed
The mass ratio for closing nanofiber is 10:1, obtain colloidal mixing nanofiber F；
(7) the colloidal mixing nanofiber obtained in step (6) is being disperseed again under the stirring action of 1000rpm
In deionized water, 60min is stirred, dispersion concentration is controlled in 1mg/ml, obtains aramid nano-fiber/nano-cellulose water-dispersed
Compound system G：
It is a kind of in the present embodiment to utilize the aramid nano-fiber water-dispersed/nano-cellulose complex prepared by the above method
System prepares the preparation method of ultraviolet shielded type nano-cellulose based transparent film, including following preparation process：
Step 1：Ultrasound degassing：Aramid nano-fiber water-dispersed/nano-cellulose compound system of above-mentioned preparation is placed in
Ultrasonic degassing process 14min in ultrasonic cleaning machine；
Step 2：Vacuum filtration：The aramid nano-fiber that step 1 is obtained/nano-cellulose compound system is filtering pressure
Power filters 4min under the conditions of being 0.7MPa, obtains aramid nano-fiber/nano-cellulose compounded wet film, forming quality is a concentration of
0.04%；
Step 3：Squeeze drying：Aramid nano-fiber/nano-cellulose compounded wet film that step 2 obtains is placed in squeezing
Machine is squeezed and is dried, and squeezing condition is：Squeeze pressure 0.4MPa squeezes time 10min；Drying condition is：Drying temperature：70
DEG C, drying time 60h.
At room temperature, it is detected using the ultraviolet-visible spectrophotometer laminated film obtained to this implementation.Inspection
Survey the result shows that (Fig. 4), ANF/NFC laminated films in visible-range when ANF additive amounts are 3%, although transmission
Rate is still on a declining curve in visible region, but maximum transmission rate is still up to 80%；In addition, ultra-violet (UV) band especially
Transmitance is down to 2% in 250nm-380nm wave bands, uv-shielding capacity compared with ANF additive amounts be 1% ANF/NCF composite membranes more
It is apparent.
Embodiment 3
(1) 1.0g para-aramid pulp fiber, 1.5g potassium hydroxide and 500ml dimethyl sulfoxide (DMSO)s are placed in container,
It under air-proof condition, is stirred 6 days at a temperature of 50 DEG C, obtains the aramid nano-fiber dispersion liquid A being scattered under KOH/DMSO systems；
(2) aramid nano-fiber being scattered under KOH/DMSO systems obtained in step (1) is diluted with DMSO,
Obtain the aramid nano-fiber dispersion liquid B that equal volumetric concentration is 0.1mg/mL；
(3) deionized water low whipping speed is added as under the action of 1000rpm in the nano-cellulose for aoxidizing TEMPO
12h is stirred, the nano-cellulose suspension C that evenly dispersed mass concentration is 1% is obtained；
(4) the nano-cellulose suspension C that will be obtained in step (3), under the action of speed of agitator is 1600rpm, to
The aramid nano-fiber dispersion liquid obtained in its high-pressure injection step (2), the mass ratio of aramid nano-fiber and nano-cellulose
It is 5:100, jet pressure 10MPa, effluxvelocity 1ml/s obtain being scattered in KOH/DMSO/H2Virtue in O mixed systems
Synthetic fibre nanofiber/nano-cellulose dispersion liquid D；
(5) it is scattered in KOH/DMSO/H by what is obtained in step (4)2Aramid nano-fiber/Nanowire in O mixed systems
The plain dispersion liquid of dimension is filtered by vacuum by the nylon leaching film of 500 mesh, obtains aramid nano-fiber/nano-cellulose composite fibre E；
(6) the mixing nanofiber obtained in step (5) is washed 3 repeatedly respectively by absolute ethyl alcohol and deionized water
Secondary, the ratio of the volume of absolute ethyl alcohol needed for washing and mixing nanofiber quality is 1ml every time:2mg, required deionized water with it is mixed
The mass ratio for closing nanofiber is 10:1, obtain colloidal mixing nanofiber F；
(7) the colloidal mixing nanofiber obtained in step (6) is being disperseed again under the stirring action of 1500rpm
In deionized water, 100min is stirred, dispersion concentration is controlled in 2.5mg/ml, obtains aramid nano-fiber/Nanowire water-dispersed
The plain compound system G of dimension：
It is a kind of in the present embodiment to utilize the aramid nano-fiber water-dispersed/nano-cellulose complex prepared by the above method
System prepares the preparation method of ultraviolet shielded type nano-cellulose based transparent film, including following preparation process：
Step 1：Ultrasound degassing：Aramid nano-fiber water-dispersed/nano-cellulose compound system of above-mentioned preparation is placed in
Ultrasonic degassing process 16min in ultrasonic cleaning machine；
Step 2：Vacuum filtration：The aramid nano-fiber that step 1 is obtained/nano-cellulose compound system is filtering pressure
Power filters 6min under the conditions of being 0.8MPa, obtains aramid nano-fiber/nano-cellulose compounded wet film, forming quality is a concentration of
0.03%；
Step 3：Squeeze drying：Aramid nano-fiber/nano-cellulose compounded wet film that step 2 obtains is placed in squeezing
Machine is squeezed and is dried, and squeezing condition is：Squeeze pressure 0.6MPa squeezes time 14min；Drying condition is：Drying temperature：70
DEG C, drying time 65h.
At room temperature, it is detected using the ultraviolet-visible spectrophotometer laminated film obtained to this implementation.Inspection
It surveys the result shows that (Fig. 4), when ANF additive amounts are 5%, ANF/NFC laminated films max transmissive in visible-range
Rate is still positively retained at 75% or so, and changes in ultra-violet (UV) band transmissivity smaller, while ultraviolet shielded wave band is to visible wavelength
Direction increases about 15nm.
Embodiment 4
(1) 1.0g p-aramid fibers fibrid, 1.5g potassium hydroxide and 500ml dimethyl sulfoxide (DMSO)s are placed in container,
Under air-proof condition, is stirred 5.5 days at a temperature of 55 DEG C, obtain the aramid nano-fiber dispersion liquid being scattered under KOH/DMSO systems
A；
(2) aramid nano-fiber being scattered under KOH/DMSO systems obtained in step (1) is diluted with DMSO,
Obtain the aramid nano-fiber dispersion liquid B that equal volumetric concentration is 0.1mg/mL；
(3) deionized water low whipping speed is added in the nano-cellulose that chemical pretreatment conjunction with mechanical is handled is
12h is stirred under the action of 1000rpm, obtains the nano-cellulose suspension C that evenly dispersed mass concentration is 1%；
(4) the nano-cellulose suspension C that will be obtained in step (3), under the action of speed of agitator is 2400rpm, to
The aramid nano-fiber dispersion liquid obtained in its high-pressure injection step (2), the mass ratio of aramid nano-fiber and nano-cellulose
It is 6.5:100, jet pressure 13MPa, effluxvelocity 1.5ml/s obtain being scattered in KOH/DMSO/H2In O mixed systems
Aramid nano-fiber/nano-cellulose dispersion liquid D；
(5) it is scattered in KOH/DMSO/H by what is obtained in step (4)2Aramid nano-fiber/Nanowire in O mixed systems
The plain dispersion liquid of dimension is filtered by vacuum by the nylon leaching film of 500 mesh, obtains aramid nano-fiber/nano-cellulose composite fibre E；
(6) the mixing nanofiber obtained in step (5) is washed 4 repeatedly respectively by absolute ethyl alcohol and deionized water
Secondary, the ratio of the volume of absolute ethyl alcohol needed for washing and mixing nanofiber quality is 1ml every time:2mg, required deionized water with it is mixed
The mass ratio for closing nanofiber is 10:1, obtain colloidal mixing nanofiber F；
(7) the colloidal mixing nanofiber obtained in step (6) is being disperseed again under the stirring action of 2000rpm
In deionized water, 140min is stirred, dispersion concentration is controlled in 1.5mg/ml, obtains aramid nano-fiber/Nanowire water-dispersed
The plain compound system G of dimension：
It is a kind of in the present embodiment to utilize the aramid nano-fiber water-dispersed/nano-cellulose complex prepared by the above method
System prepares the preparation method of ultraviolet shielded type nano-cellulose based transparent film, including following preparation process：
Step 1：Ultrasound degassing：Aramid nano-fiber water-dispersed/nano-cellulose compound system of above-mentioned preparation is placed in
Ultrasonic degassing process 18min in ultrasonic cleaning machine；
Step 2：Vacuum filtration：The aramid nano-fiber that step 1 is obtained/nano-cellulose compound system is filtering pressure
Power filters 8min under the conditions of being 0.9MPa, obtains aramid nano-fiber/nano-cellulose compounded wet film, forming quality is a concentration of
0.02%；
Step 3：Squeeze drying：Aramid nano-fiber/nano-cellulose compounded wet film that step 2 obtains is placed in squeezing
Machine is squeezed and is dried, and squeezing condition is：Squeeze pressure 0.8MPa squeezes time 17min；Drying condition is：Drying temperature：70
DEG C, drying time 70h.
At room temperature, it is detected using the ultraviolet-visible spectrophotometer laminated film obtained to this implementation.Inspection
It surveys the result shows that (Fig. 4), ANF/NFC laminated films are in visible-range when ANF additive amounts are 6.5%, and maximum is thoroughly
It is only 2% or so to penetrate rate compared with the laminated film that ANF additive amounts are 5% to decline, and in ultraviolet shielded wave band transmitance value and covering
Range does not show too big difference.
Embodiment 5
(1) 1.0g p-aramid fibers chopped strand, 1.5g potassium hydroxide and 500ml dimethyl sulfoxide (DMSO)s are placed in container,
It under air-proof condition, is stirred 5 days at a temperature of 60 DEG C, obtains the aramid nano-fiber dispersion liquid A being scattered under KOH/DMSO systems；
(2) aramid nano-fiber being scattered under KOH/DMSO systems obtained in step (1) is diluted with DMSO,
Obtain the aramid nano-fiber dispersion liquid B that equal volumetric concentration is 0.1mg/mL；
(3) deionized water low whipping speed is added as under the action of 1000rpm in the nano-cellulose for aoxidizing TEMPO
12h is stirred, the nano-cellulose suspension C that evenly dispersed mass concentration is 1% is obtained；
(4) the nano-cellulose suspension C that will be obtained in step (3), under the action of speed of agitator is 3000rpm, to
The aramid nano-fiber dispersion liquid obtained in its high-pressure injection step (2), the mass ratio of aramid nano-fiber and nano-cellulose
It is 8:100, jet pressure 15MPa, effluxvelocity 2ml/s obtain being scattered in KOH/DMSO/H2Virtue in O mixed systems
Synthetic fibre nanofiber/nano-cellulose dispersion liquid D；
(5) it is scattered in KOH/DMSO/H by what is obtained in step (4)2Aramid nano-fiber/Nanowire in O mixed systems
The plain dispersion liquid of dimension is filtered by vacuum by the nylon leaching film of 500 mesh, obtains aramid nano-fiber/nano-cellulose composite fibre E；
(6) the mixing nanofiber obtained in step (5) is washed 4 repeatedly respectively by absolute ethyl alcohol and deionized water
Secondary, the ratio of the volume of absolute ethyl alcohol needed for washing and mixing nanofiber quality is 1ml every time:2mg, required deionized water with it is mixed
The mass ratio for closing nanofiber is 10:1, obtain colloidal mixing nanofiber F；
(7) the colloidal mixing nanofiber obtained in step (6) is being disperseed again under the stirring action of 2500rpm
In deionized water, 180min is stirred, dispersion concentration is controlled in 0.5mg/ml, obtains aramid nano-fiber/Nanowire water-dispersed
The plain compound system G of dimension：
It is a kind of in the present embodiment to mix fibre using the aramid nano-fiber water-dispersed prepared by the above method/nano-cellulose
Dimension prepares the preparation method of ultraviolet shielded type nano-cellulose based transparent film, including following preparation process：
Step 1：Ultrasound degassing：Aramid nano-fiber water-dispersed/nano-cellulose compound system of above-mentioned preparation is placed in
Ultrasonic degassing process 20min in ultrasonic cleaning machine；
Step 2：Vacuum filtration：The aramid nano-fiber that step 1 is obtained/nano-cellulose compound system is filtering pressure
Power filters 10min under the conditions of being 1MPa, obtains aramid nano-fiber/nano-cellulose compounded wet film, forming quality is a concentration of
0.02%；
Step 3：Squeeze drying：Aramid nano-fiber/nano-cellulose compounded wet film that step 2 obtains is placed in squeezing
Machine is squeezed and is dried, and squeezing condition is：Squeeze pressure 1MPa squeezes time 20min；Drying condition is：Drying temperature：70 DEG C,
Drying time 75h.
At room temperature, it is detected using the ultraviolet-visible spectrophotometer laminated film obtained to this implementation.Inspection
Survey the result shows that (Fig. 4), when ANF additive amounts are 8%, ANF/NFC laminated films visible-range internal transmission factor still
Up to 76%, at the same it is most wide in ultraviolet shielded band coverage, and uv-shielding capacity shows best.
Claims (10)
1. a kind of preparation method of aramid nano-fiber water-dispersed/nano-cellulose compound system, which is characterized in that including following
Step：
(1) para-aramid fiber X, potassium hydroxide, dimethyl sulfoxide (DMSO) are placed in container, are dispersed with stirring, obtain being scattered in KOH/
Aramid nano-fiber dispersion liquid A under DMSO system；
(2) the aramid nano-fiber dispersion liquid A being scattered under KOH/DMSO systems obtained in step (1) is diluted, is obtained
To evenly dispersed aramid nano-fiber dispersion liquid B；
(3) deionized water is added in nano-cellulose Y and is stirred dispersion, obtain evenly dispersed nano-cellulose suspension C；
(4) the nano-cellulose suspension C that will be obtained in step (3), under the high shear forces that stirring generates, to its high pressure injection
The aramid nano-fiber dispersion liquid B obtained in step (2) is penetrated, obtains being scattered in KOH/DMSO/H2Aramid fiber in O mixed systems is received
Rice fibers/nanofibers element dispersion liquid D；
(5) it is scattered in KOH/DMSO/H by what is obtained in step (4)2Aramid nano-fiber/nano-cellulose in O mixed systems
Dispersion liquid D obtains mixing nanofiber E by vacuum filtration；
(6) the mixing nanofiber E obtained in step (5) is washed repeatedly by absolute ethyl alcohol and deionized water, obtains colloid
Shape mixing nanofiber F；
(7) the colloidal mixing nanofiber F obtained in step (6) is scattered in deionized water again under stirring,
Obtain aramid nano-fiber water-dispersed/nano-cellulose compound system.
2. a kind of preparation method of aramid nano-fiber water-dispersed/nano-cellulose compound system according to claim 1,
It is characterized in that, para-aramid fiber X, potassium hydroxide and dimethyl sulfoxide (DMSO) ratio are 1g in step (1)：1.5g：500ml, institute
The para-aramid fiber X stated is p-aramid fiber yarn fibers, p-aramid fiber chopped strand, para-aramid pulp fiber and contraposition virtue
One kind in synthetic fibre fibrid.
3. a kind of preparation method of aramid nano-fiber water-dispersed/nano-cellulose compound system according to claim 1,
It is characterized in that, dilute to the aramid nano-fiber dispersion liquid A progress being scattered under KOH/DMSO systems using DMSO in step (2)
It releases, a concentration of 0.1mg/mL of obtained aramid nano-fiber dispersion liquid B.
4. a kind of preparation method of aramid nano-fiber water-dispersed/nano-cellulose compound system according to claim 1,
It is characterized in that, the mass concentration of nano-cellulose suspension C is 1% in step (3), the nano-cellulose Y is to pass through
The nanocrystal cellulose that chemical oxidation treatment, the processing of chemical pretreatment conjunction with mechanical or chemical sour water solution obtain.
5. a kind of preparation method of aramid nano-fiber water-dispersed/nano-cellulose compound system according to claim 1,
It is characterized in that, the injection of step (4) mesohigh is to utilize stainless steel high-pressure spray pump, jet pressure is 5~15MPa, jet velocity
Degree is 0.2~2.0mL/s；What step (4) obtained is scattered in KOH/DMSO/H2Aramid nano-fiber/nanometer in O mixed systems
The mass ratio of aramid nano-fiber and nano-cellulose is (1~8) in cellulose dispersion liquid D：100.
6. a kind of preparation method of aramid nano-fiber water-dispersed/nano-cellulose compound system according to claim 1,
It is characterized in that, the filter membrane that vacuum filtration uses in step (5) is 500 mesh nylon leaching film；Washing absolute ethyl alcohol in step (6)
Volume and mix nanofiber E mass ratio be 1mL:5mg~1mL:2mg；The washing deionized water with mix nanometer
The mass ratio of fiber E is 10:1~5:1.
7. a kind of preparation method of aramid nano-fiber water-dispersed/nano-cellulose compound system according to claim 1,
It is characterized in that, the dispersion concentrations of colloid mixing nanofiber F in deionized water are 0.5~5mg/mL in step (7).
8. a kind of preparation method of aramid nano-fiber water-dispersed/nano-cellulose compound system according to claim 1,
It is characterized in that, stirring refers to being stirred 5~8 days at a temperature of 30~60 DEG C under air-proof condition in step (1)；Step (3) step
Mix rotating speed is 1000rpm in rapid, mixing time 12h, and speed of agitator is 600~3000rpm in step (4)；Step is stirred in (7)
It is 500~2500rpm, 30~180min of mixing time to mix revolution.
9. a kind of using claim 1-8 any one of them aramid nano-fiber water-dispersed/nano-cellulose compound system system
The method of standby ultraviolet shielded type transparent membrane, which is characterized in that include the following steps：
Step 1：Ultrasound degassing：Aramid nano-fiber water-dispersed/nano-cellulose compound system is placed in ultrasonic cleaning machine and is surpassed
Sound degassing process；
Step 2：Vacuum filtration：The aramid nano-fiber that step 1 is obtained/nano-cellulose compound system is true in circulation hydraulic
Aramid nano-fiber/nano-cellulose compounded wet film is obtained under the swabbing action of sky pump, forming quality a concentration of 0.02%~
0.06%；
Step 3：Squeeze drying：Aramid nano-fiber/nano-cellulose compounded wet film that step 2 obtains is placed in squeezer pressure
It squeezes and is dried to obtain ultraviolet shielded type transparent membrane.
10. according to claim 9 prepare ultraviolet screen using aramid nano-fiber water-dispersed/nano-cellulose compound system
Cover the method for type transparent membrane, which is characterized in that the ultrasonic degassing process time is 10~20min in step 1；Institute in step 2
It is 0.5~1MPa to state vacuum filter pressure, and the suction filtration time is 2~10min, and filter membrane is 500 mesh nylon leaching films；It is squeezed in step 3
Condition is：0.2~1.0MPa of squeeze pressure squeezes 3~20min of time；Drying condition is：Drying temperature：70 DEG C, drying time
48~75h.
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