CN107216586A - A kind of preparation method of polyvinyl alcohol/nano-cellulose/polyethylene composite film - Google Patents
A kind of preparation method of polyvinyl alcohol/nano-cellulose/polyethylene composite film Download PDFInfo
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Abstract
The invention discloses a kind of preparation method of polyvinyl alcohol/nano-cellulose/polyethylene composite film, carry out according to the following steps：Step（1）, the preparation of nano-cellulose whisker suspension；Step（2）, the preparation of polyvinyl alcohol suspension；Step（3）, the preparation of polyvinyl alcohol/nano-cellulose mixed solution；Step（4）, the preparation of polyvinyl alcohol/nano-cellulose/polyethylene composite film.The present invention proposes a kind of preparation method of polyvinyl alcohol/nano-cellulose/polyethylene composite film, it the method increase the interface compatibility of nano-cellulose and polyvinyl alcohol and polyethylene, compared with nano-cellulose film, polyvinyl alcohol/nano-cellulose/polyethylene composite film of preparation has higher tensile strength and heat endurance.
Description
Technical field
The invention belongs to technical field of composite materials, more particularly to a kind of polyvinyl alcohol/nano-cellulose/polyethylene is multiple
Close the preparation method of film.
Background technology
Polyvinyl alcohol is the hydroxyl in important industrial chemicals, polyvinyl alcohol molecule not only containing hydrophily high activity but also contained
Hydrophobic acetyl group, by changing the ratio and space structure of its degree of polymerization, hydroxyl and acetyl group, can send out its performance
Give birth to very big change.Less Volume Changes when polyvinyl alcohol is because with suitable phase transition temperature, high latent heat appearance, solid-liquid phase change
With the premium properties such as excellent heat-resisting, chemically-resistant, it is widely used in the fields such as pharmacy, biological medicine.Therefore, polyvinyl alcohol quilt
It is widely used in adhesive, coating, emulsifying agent, paper conversion auxiliary agent, weaving, film, liquid crystal display, packaging, building, medicine, electricity
The industries such as son, cosmetics, oil exploitation, safety glass, timber processing, agricultural and Metallurgy Industry, with higher interrelationship between industries.
Nano-cellulose（NCC）With more than high accessibility, high-specific surface area, effective active center and its susceptibility height etc.
Advantage, therefore, composite phase-change material is prepared by graft N CC, can be prepared high enthalpy of phase change nano-cellulose base and is combined
Phase-change material, but because nano-cellulose is practically insoluble in common solvent, it is difficult to which directly grafting polyvinyl alcohol prepares Nanowire
The plain base composite phase-change material of dimension.Therefore prior art is solved because nano-cellulose is practically insoluble in common solvent, it is difficult to directly connect
The problem of branch polyvinyl alcohol prepares nano-cellulose base composite phase-change material is an importance of research staff's research.
The content of the invention
Present invention seek to address that prior art is practically insoluble in common solvent because of nano-cellulose, it is difficult to directly be grafted poly- second
The problem of enol prepares nano-cellulose base composite phase-change material, and a kind of polyvinyl alcohol/nano-cellulose/poly- second is provided
The preparation method of alkene composite membrane.
A kind of preparation method of polyvinyl alcohol/nano-cellulose/polyethylene composite film, is carried out according to the following steps：
Step（1）, the preparation of nano-cellulose whisker suspension：
Take nano-cellulose is scattered to be added in sulfuric acid solution, the acidolysis 2-4h under conditions of temperature is 50-60 DEG C obtains nanometer
Cellulose suspension, 15- is centrifuged under conditions of rotating speed is 5000-8000r/min by obtained nano-cellulose suspension
Take upper strata to hold liquid after 25min, centrifugation, shaken using obtaining nano-cellulose dispersion liquid after magnetic stirrer, then with ultrasonic wave
Dynamic instrument obtains nano-cellulose whisker with 12000-14000rmp sound and vibration 4-8min, with 4500-5500rmp separation 25-30min and hanged
Supernatant liquid；
Step（2）, the preparation of polyvinyl alcohol suspension：
Take polyvinyl alcohol and deionized water to add in flask, carry out magnetic agitation 20-40min, it is cold under 85-95 DEG C of water bath condition
Solidifying backflow, until after polyvinyl alcohol is completely dissolved, take 0.06-0.09mm sieves to carry out being filtrated to get the poly- second that concentration is 10wt%
Enolate solution；
Step（3）, the preparation of polyvinyl alcohol/nano-cellulose mixed solution：
Take the poly-vinyl alcohol solution that concentration is 10wt% in flask, add nano-cellulose whisker suspension, flask is placed in super
In acoustic wave vibrations instrument, after ultrasonic activation 20-40min, vigorous mechanical agitation is carried out, polyethylene is obtained after being uniformly mixed
Alcohol/nano-cellulose mixed solution；
Step（4）, the preparation of polyvinyl alcohol/nano-cellulose/polyethylene composite film：
By step（3）Obtained mixed solution uses Buchner funnel and polyethylene filter paper, after filtering, by obtained wet film and
One piece of filter paper is removed, and is positioned between two metallic plates, is dried 23-26h in 75-85 DEG C of temperature, is obtained polyvinyl alcohol/Nanowire
Tie up element/polyethylene composite film.
Further, step（1）The preparing raw material of the suspension of described nano-cellulose be selected from jute, Japanese cedar,
Eucalyptus pulp, bamboo pulp or stalk；The mass fraction of the sulfuric acid solution is 50%-60%, described nano-cellulose dispersion liquid it is dense
Spend for 0.2%-0.4%, a diameter of 7-8nm of the nano-cellulose whisker of described nano-cellulose whisker suspension, length is
100-200nm。
Further, described in step (3) nano-cellulose whisker suspension and the weight ratio of 10% poly-vinyl alcohol solution
For 1:(25-60).
Further, step（1）The thickness of described polyvinyl alcohol/nano-cellulose/polyethylene composite film is 0.010-
0.020mm。
Beneficial effects of the present invention：（1）Polarity and the parent of nano-cellulose are reduced by modified composite film material
It is aqueous, the interface compatibility of nano-cellulose and polyvinyl alcohol and polyethylene is improved；（2）With nano-cellulose film phase
Compare, the tensile strength of polyvinyl alcohol/nano-cellulose/polyethylene composite film can improve 25%-33%；（3）Prepared by the present invention
Polyvinyl alcohol/nano-cellulose/polyethylene composite film is without thermal decomposition below 160 DEG C, and phase transformation enthalpy may be up to 134.6J/g,
Compared with existing graft copolymerization composite phase-change material enthalpy of phase change is generally below 100J/g, 34.6% is at least improved, therefore composite membrane
Heat endurance is greatly improved.
Embodiment
With reference to specific embodiment, the present invention is furture elucidated,
Embodiment 1
A kind of preparation method of polyvinyl alcohol/nano-cellulose/polyethylene composite film, is carried out according to the following steps：
Step（1）, the preparation of the outstanding whisker supernatant liquid of nano-cellulose：
Take nano-cellulose is scattered to be added in the sulfuric acid solution that mass fraction is 50%, the acidolysis under conditions of temperature is 50 DEG C
2h, obtains nano-cellulose suspension, rotating speed be 5000r/min under conditions of by obtained nano-cellulose suspension from
Take upper strata to hold liquid after heart 15min, centrifugation, disperseed using the nano-cellulose that concentration is 0.2wt% is obtained after magnetic stirrer
Liquid, then nano-cellulose whisker is obtained with 4500rmp separation 25min and hanged with 12000rmp sound and vibration 4min with ultrasonic activation instrument
Supernatant liquid, a diameter of 7-8nm of the nano-cellulose whisker of described nano-cellulose whisker suspension, length is 100-200nm；
Step（2）, the preparation of polyvinyl alcohol suspension：
Take polyvinyl alcohol and deionized water to add in flask, carry out magnetic agitation 20min, condensed back under 85 DEG C of water bath conditions
Stream, until after polyvinyl alcohol is completely dissolved, take 0.06mm sieves to carry out being filtrated to get the poly-vinyl alcohol solution that concentration is 10wt%；
Step（3）, the preparation of polyvinyl alcohol/nano-cellulose mixed solution：
Take the poly-vinyl alcohol solution that concentration is 10wt% in flask, add nano-cellulose whisker suspension, described Nanowire
The weight ratio of the plain whisker suspension of dimension and poly-vinyl alcohol solution is 1:25, flask is placed in vibration of ultrasonic wave instrument, ultrasonic wave shakes
After dynamic 20min, vigorous mechanical agitation is carried out, polyvinyl alcohol/nano-cellulose mixed solution is obtained after being uniformly mixed；
Step（4）, the preparation of polyvinyl alcohol/nano-cellulose/polyethylene composite film：
By step（3）Obtained mixed solution uses Buchner funnel and polyethylene filter paper, after filtering, by obtained wet film and
One piece of filter paper is removed, and is positioned between two metallic plates, and 23h is dried in 75 DEG C of temperature, obtains the polyethylene that thickness is 0.010mm
Alcohol/nano-cellulose/polyethylene composite film.
Step（1）The preparing raw material of the suspension of described nano-cellulose is selected from jute.
Embodiment 2
A kind of preparation method of polyvinyl alcohol/nano-cellulose/polyethylene composite film, is carried out according to the following steps：
Step（1）, the preparation of nano-cellulose whisker suspension：
Take nano-cellulose is scattered to be added in the sulfuric acid solution that mass fraction is 60%, the acidolysis under conditions of temperature is 60 DEG C
4h, obtains nano-cellulose suspension, rotating speed be 8000r/min under conditions of by obtained nano-cellulose suspension from
Take upper strata to hold liquid after heart 25min, centrifugation, disperseed using the nano-cellulose that concentration is 0.4wt% is obtained after magnetic stirrer
Liquid, then nano-cellulose whisker is obtained with 5500rmp separation 30min and hanged with 14000rmp sound and vibration 8min with ultrasonic activation instrument
Supernatant liquid, a diameter of 7-8nm of the nano-cellulose whisker of described nano-cellulose whisker suspension, length is 100-200nm；
Step（2）, the preparation of polyvinyl alcohol suspension：
Take polyvinyl alcohol and deionized water to add in flask, carry out magnetic agitation 35min, condensed back under 95 DEG C of water bath conditions
Stream, until after polyvinyl alcohol is completely dissolved, take 0.09mm sieves to carry out being filtrated to get the poly-vinyl alcohol solution that concentration is 10wt%；
Step（3）, the preparation of polyvinyl alcohol/nano-cellulose mixed solution：
Take the poly-vinyl alcohol solution that concentration is 10wt% in flask, add nano-cellulose whisker suspension, described Nanowire
The weight ratio of the plain whisker suspension of dimension and poly-vinyl alcohol solution is 1:60, flask is placed in vibration of ultrasonic wave instrument, ultrasonic wave shakes
After dynamic 40min, vigorous mechanical agitation is carried out, polyvinyl alcohol/nano-cellulose mixed solution is obtained after being uniformly mixed；
Step（4）, the preparation of polyvinyl alcohol/nano-cellulose/polyethylene composite film：
By step（3）Obtained mixed solution uses Buchner funnel and polyethylene filter paper, after filtering, by obtained wet film and
One piece of filter paper is removed, and is positioned between two metallic plates, and 26h is dried in 85 DEG C of temperature, obtains the polyethylene that thickness is 0.020mm
Alcohol/nano-cellulose/polyethylene composite film.
Step（1）The preparing raw material of the suspension of described nano-cellulose is selected from jute.
Embodiment 3
A kind of preparation method of polyvinyl alcohol/nano-cellulose/polyethylene composite film, is carried out according to the following steps：
Step（1）, the preparation of nano-cellulose whisker suspension：
Take nano-cellulose is scattered to be added in the sulfuric acid solution that mass fraction is 55%, the acidolysis under conditions of temperature is 55 DEG C
3h, obtains nano-cellulose suspension, rotating speed be 6500r/min under conditions of by obtained nano-cellulose suspension from
Take upper strata to hold liquid after heart 20min, centrifugation, disperseed using the nano-cellulose that concentration is 0.3wt% is obtained after magnetic stirrer
Liquid, then nano-cellulose whisker is obtained with 5000rmp separation 28min and hanged with 13000rmp sound and vibration 6min with ultrasonic activation instrument
Supernatant liquid, a diameter of 7-8nm of the nano-cellulose whisker of described nano-cellulose whisker suspension, length is 100-200nm；
Step（2）, the preparation of polyvinyl alcohol suspension：
Take polyvinyl alcohol and deionized water to add in flask, carry out magnetic agitation 30min, condensed back under 90 DEG C of water bath conditions
Stream, until after polyvinyl alcohol is completely dissolved, take 0.074mm sieves to carry out being filtrated to get the poly-vinyl alcohol solution that concentration is 10wt%；
Step（3）, the preparation of polyvinyl alcohol/nano-cellulose mixed solution：
Take the poly-vinyl alcohol solution that concentration is 10wt% in flask, add nano-cellulose whisker suspension, described Nanowire
The weight ratio of the plain whisker suspension of dimension and poly-vinyl alcohol solution is 1:42, flask is placed in vibration of ultrasonic wave instrument, ultrasonic wave shakes
After dynamic 30min, vigorous mechanical agitation is carried out, polyvinyl alcohol/nano-cellulose mixed solution is obtained after being uniformly mixed；
Step（4）, the preparation of polyvinyl alcohol/nano-cellulose/polyethylene composite film：
By step（3）Obtained mixed solution uses Buchner funnel and polyethylene filter paper, after filtering, by obtained wet film and
One piece of filter paper is removed, and is positioned between two metallic plates, and 24.5h is dried in 80 DEG C of temperature, obtains the poly- second that thickness is 0.015mm
Enol/nano-cellulose/polyethylene composite film.
Step（1）The preparing raw material of the suspension of described nano-cellulose is selected from bamboo pulp.
Embodiment 4
A kind of preparation method of polyvinyl alcohol/nano-cellulose/polyethylene composite film, is carried out according to the following steps：
Step（1）, the preparation of nano-cellulose whisker suspension：
Take nano-cellulose is scattered to be added in the sulfuric acid solution that mass fraction is 55%, the acidolysis under conditions of temperature is 55 DEG C
3h, obtains nano-cellulose suspension, rotating speed be 6500r/min under conditions of by obtained nano-cellulose suspension from
Take upper strata to hold liquid after heart 20min, centrifugation, disperseed using the nano-cellulose that concentration is 0.2wt% is obtained after magnetic stirrer
Liquid, then nano-cellulose whisker is obtained with 5000rmp separation 28min and hanged with 13000rmp sound and vibration 6min with ultrasonic activation instrument
Supernatant liquid, a diameter of 7-8nm of the nano-cellulose whisker of described nano-cellulose whisker suspension, length is 100-200nm；
Step（2）, the preparation of polyvinyl alcohol suspension：
Take polyvinyl alcohol and deionized water to add in flask, carry out magnetic agitation 30min, condensed back under 90 DEG C of water bath conditions
Stream, until after polyvinyl alcohol is completely dissolved, take 0.074mm sieves to carry out being filtrated to get the poly-vinyl alcohol solution that concentration is 10wt%；
Step（3）, the preparation of polyvinyl alcohol/nano-cellulose mixed solution：
Take the poly-vinyl alcohol solution that concentration is 10wt% in flask, add nano-cellulose whisker suspension, described Nanowire
The weight ratio of the plain whisker suspension of dimension and poly-vinyl alcohol solution is 1:60, flask is placed in vibration of ultrasonic wave instrument, ultrasonic wave shakes
After dynamic 30min, vigorous mechanical agitation is carried out, polyvinyl alcohol/nano-cellulose mixed solution is obtained after being uniformly mixed；
Step（4）, the preparation of polyvinyl alcohol/nano-cellulose/polyethylene composite film：
By step（3）Obtained mixed solution uses Buchner funnel and polyethylene filter paper, after filtering, by obtained wet film and
One piece of filter paper is removed, and is positioned between two metallic plates, and 24h is dried in 80 DEG C of temperature, obtains the polyethylene that thickness is 0.020mm
Alcohol/nano-cellulose/polyethylene composite film.
Step（1）The preparing raw material of the suspension of described nano-cellulose is selected from bamboo pulp.
Embodiment 5
A kind of preparation method of polyvinyl alcohol/nano-cellulose/polyethylene composite film, is carried out according to the following steps：
Step（1）, the preparation of nano-cellulose whisker suspension：
Take nano-cellulose is scattered to be added in the sulfuric acid solution that mass fraction is 60%, the acidolysis under conditions of temperature is 50 DEG C
3h, obtains nano-cellulose suspension, rotating speed be 6500r/min under conditions of by obtained nano-cellulose suspension from
Take upper strata to hold liquid after heart 20min, centrifugation, disperseed using the nano-cellulose that concentration is 0.4wt% is obtained after magnetic stirrer
Liquid, then nano-cellulose whisker is obtained with 5000rmp separation 28min and hanged with 13000rmp sound and vibration 6min with ultrasonic activation instrument
Supernatant liquid, a diameter of 7-8nm of the nano-cellulose whisker of described nano-cellulose whisker suspension, length is 100-200nm；
Step（2）, the preparation of polyvinyl alcohol suspension：
Take polyvinyl alcohol and deionized water to add in flask, carry out magnetic agitation 30min, condensed back under 90 DEG C of water bath conditions
Stream, until after polyvinyl alcohol is completely dissolved, take 0.074mm sieves to carry out being filtrated to get the poly-vinyl alcohol solution that concentration is 10wt%；
Step（3）, the preparation of polyvinyl alcohol/nano-cellulose mixed solution：
Take the poly-vinyl alcohol solution that concentration is 10wt% in flask, add nano-cellulose whisker suspension, described Nanowire
The weight ratio of the plain whisker suspension of dimension and poly-vinyl alcohol solution is 1:25, flask is placed in vibration of ultrasonic wave instrument, ultrasonic wave shakes
After dynamic 30min, vigorous mechanical agitation is carried out, polyvinyl alcohol/nano-cellulose mixed solution is obtained after being uniformly mixed；
Step（4）, the preparation of polyvinyl alcohol/nano-cellulose/polyethylene composite film：
By step（3）Obtained mixed solution uses Buchner funnel and polyethylene filter paper, after filtering, by obtained wet film and
One piece of filter paper is removed, and is positioned between two metallic plates, and 25h is dried in 80 DEG C of temperature, obtains the polyethylene that thickness is 0.020mm
Alcohol/nano-cellulose/polyethylene composite film.
Step（1）The preparing raw material of the suspension of described nano-cellulose is selected from bamboo pulp.
Embodiment 6
A kind of preparation method of polyvinyl alcohol/nano-cellulose/polyethylene composite film, is carried out according to the following steps：
Step（1）, the preparation of nano-cellulose whisker suspension：
Take nano-cellulose is scattered to be added in the sulfuric acid solution that mass fraction is 50%, the acidolysis under conditions of temperature is 60 DEG C
3h, obtains nano-cellulose suspension, rotating speed be 7000r/min under conditions of by obtained nano-cellulose suspension from
Take upper strata to hold liquid after heart 20min, centrifugation, disperseed using the nano-cellulose that concentration is 0.3wt% is obtained after magnetic stirrer
Liquid, then nano-cellulose whisker is obtained with 5000rmp separation 28min and hanged with 13000rmp sound and vibration 8min with ultrasonic activation instrument
Supernatant liquid, a diameter of 7-8nm of the nano-cellulose whisker of described nano-cellulose whisker suspension, length is 100-200nm；
Step（2）, the preparation of polyvinyl alcohol suspension：
Take polyvinyl alcohol and deionized water to add in flask, carry out magnetic agitation 30min, condensed back under 90 DEG C of water bath conditions
Stream, until after polyvinyl alcohol is completely dissolved, take 0.074mm sieves to carry out being filtrated to get the poly-vinyl alcohol solution that concentration is 10wt%；
Step（3）, the preparation of polyvinyl alcohol/nano-cellulose mixed solution：
Take the poly-vinyl alcohol solution that concentration is 10wt% in flask, add nano-cellulose whisker suspension, described Nanowire
The weight ratio of the plain whisker suspension of dimension and poly-vinyl alcohol solution is 1:60, flask is placed in vibration of ultrasonic wave instrument, ultrasonic wave shakes
After dynamic 30min, vigorous mechanical agitation is carried out, polyvinyl alcohol/nano-cellulose mixed solution is obtained after being uniformly mixed；
Step（4）, the preparation of polyvinyl alcohol/nano-cellulose/polyethylene composite film：
By step（3）Obtained mixed solution uses Buchner funnel and polyethylene filter paper, after filtering, by obtained wet film and
One piece of filter paper is removed, and is positioned between two metallic plates, and 24h is dried in 80 DEG C of temperature, obtains the polyethylene that thickness is 0.020mm
Alcohol/nano-cellulose/polyethylene composite film.
Step（1）The preparing raw material of the suspension of described nano-cellulose is selected from bamboo pulp.
In a word, the present invention proposes a kind of preparation method of polyvinyl alcohol/nano-cellulose/polyethylene composite film, the party
Method improves the interface compatibility of nano-cellulose and polyvinyl alcohol and polyethylene, compared with nano-cellulose film, preparation it is poly-
Vinyl alcohol/nano-cellulose/polyethylene composite film has higher tensile strength and heat endurance.
Six embodiments of the present invention are above are only, but the design concept of the present invention is not limited thereto, all profits
The change of unsubstantiality is carried out to the present invention with this design, the behavior for invading the scope of protection of the invention all should be belonged to.In every case it is
Any type of letter made without departing from the content of technical solution of the present invention, the technical spirit according to the present invention to above example
Single modification, equivalent variations and remodeling, still fall within the protection domain of technical solution of the present invention.
Claims (4)
1. a kind of preparation method of polyvinyl alcohol/nano-cellulose/polyethylene composite film, it is characterised in that enter according to the following steps
OK：
Step（1）, the preparation of the outstanding whisker supernatant liquid of nano-cellulose：
Take nano-cellulose is scattered to be added in sulfuric acid solution, the acidolysis 2-4h under conditions of temperature is 50-60 DEG C obtains nanometer
Cellulose suspension, 15- is centrifuged under conditions of rotating speed is 5000-8000r/min by obtained nano-cellulose suspension
Take upper strata to hold liquid after 25min, centrifugation, shaken using obtaining nano-cellulose dispersion liquid after magnetic stirrer, then with ultrasonic wave
Dynamic instrument obtains nano-cellulose whisker with 12000-14000rmp sound and vibration 4-8min, with 4500-5500rmp separation 25-30min and hanged
Supernatant liquid；
Step（2）, the preparation of polyvinyl alcohol suspension：
Take polyvinyl alcohol and deionized water to add in flask, carry out magnetic agitation 20-40min, it is cold under 85-95 DEG C of water bath condition
Solidifying backflow, until after polyvinyl alcohol is completely dissolved, take 0.06-0.09mm sieves to carry out being filtrated to get the poly- second that concentration is 10wt%
Enolate solution；
Step（3）, the preparation of polyvinyl alcohol/nano-cellulose mixed solution：
Take the poly-vinyl alcohol solution that concentration is 10wt% in flask, add nano-cellulose whisker suspension, flask is placed in super
In acoustic wave vibrations instrument, after ultrasonic activation 20-40min, vigorous mechanical agitation is carried out, polyethylene is obtained after being uniformly mixed
Alcohol/nano-cellulose mixed solution；
Step（4）, the preparation of polyvinyl alcohol/nano-cellulose/polyethylene composite film：
By step（3）Obtained mixed solution uses Buchner funnel and polyethylene filter paper, after filtering, by obtained wet film and
One piece of filter paper is removed, and is positioned between two metallic plates, is dried 23-26h in 75-85 DEG C of temperature, is obtained polyvinyl alcohol/Nanowire
Tie up element/polyethylene composite film.
2. the preparation method of polyvinyl alcohol/nano-cellulose/polyethylene composite film as claimed in claim 1, it is characterised in that
Step（1）The preparing raw material of the suspension of described nano-cellulose is selected from jute, Japanese cedar, eucalyptus pulp, bamboo pulp or stalk；
The mass fraction of the sulfuric acid solution is 50%-60%, and the concentration of described nano-cellulose dispersion liquid is 0.2%-0.4%, described
Nano-cellulose whisker suspension nano-cellulose whisker a diameter of 7-8nm, length is 100-200nm.
3. the preparation method of polyvinyl alcohol/nano-cellulose/polyethylene composite film according to claim 1, its feature exists
In the weight ratio of nano-cellulose whisker suspension and 10% poly-vinyl alcohol solution described in step (3) is 1:(25-60).
4. the preparation method of polyvinyl alcohol/nano-cellulose/polyethylene composite film as claimed in claim 1, it is characterised in that
Step（1）The thickness of described polyvinyl alcohol/nano-cellulose/polyethylene composite film is 0.010-0.020mm.
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