CN108485140A - A kind of barrier flame retardant type polyvinyl alcohol composite material and preparation method thereof - Google Patents
A kind of barrier flame retardant type polyvinyl alcohol composite material and preparation method thereof Download PDFInfo
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- CN108485140A CN108485140A CN201810364907.4A CN201810364907A CN108485140A CN 108485140 A CN108485140 A CN 108485140A CN 201810364907 A CN201810364907 A CN 201810364907A CN 108485140 A CN108485140 A CN 108485140A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L29/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal or ketal radical; Compositions of hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Compositions of derivatives of such polymers
- C08L29/02—Homopolymers or copolymers of unsaturated alcohols
- C08L29/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/32—Phosphorus-containing compounds
- C08K2003/321—Phosphates
- C08K2003/328—Phosphates of heavy metals
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C08L2201/00—Properties
- C08L2201/02—Flame or fire retardant/resistant
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/14—Gas barrier composition
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- C—CHEMISTRY; METALLURGY
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- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/14—Polymer mixtures characterised by other features containing polymeric additives characterised by shape
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Abstract
The invention discloses a kind of fire-retardant isolation-type polyvinyl alcohol composite materials, are made up of intercalation solution composite algorithm of raw material components polyvinyl alcohol, graphene oxide, α basic zirconium phosphates and sulfonated phosphazene microballoon.Specific preparation process is as follows：S1, by graphene oxide, α basic zirconium phosphates and sulfonated phosphazene microballoon ultrasonic disperse in water, obtain mixture system；S2, polyvinyl alcohol is dissolved in hot water, obtains polyvinyl alcohol water solution；Mixture system made from S1 is added in polyvinyl alcohol water solution, 5 10h are stirred, polyvinyl alcohol/sulfonated phosphazene/α basic zirconium phosphates/graphene oxide liquid mixture is made；S3, the obtained mixed liquors of step S2 are poured into glass mold, non-isothermal drying obtains polyvinyl alcohol composite material.The polyvinyl alcohol composite material of the present invention has the characteristics that the sulfonated phosphazene microballoon, graphene oxide and α basic zirconium phosphates of different structure by introducing, and so that polyvinyl alcohol material is had preferable barrier property and anti-flammability, and bring the raising of comprehensive performance.
Description
Technical field
The invention belongs to technical field of composite materials, and in particular to a kind of barrier flame retardant type polyvinyl alcohol composite material and its
Preparation method.
Background technology
Polyvinyl alcohol (PVA) is the product of polyvinyl acetate ester hydrolysis, is a kind of tasteless, nontoxic synthesis macromolecule, has
Sheet, cotton-shaped or three kinds of forms of pulverulent solids, molecular structure is more regular, is a kind of semicrystalline polymeric.With PVA's
The difference of structure, alcoholysis degree and the degree of polymerization so that it has diversified property.Such as good barrier property, film forming, biology drop
Xie Xing, dissolubility etc. are widely used in food packaging, washing packaging and chemicals packaging.
However, also the general character with plastic material is readily burned polyvinyl alcohol material, and film polyvinyl alcohol material
High to gas barrier property requirement, pure polyvinyl alcohol cannot reach these performance requirements, greatly limit the material and packing
The use and development of Material Field.In recent years, with the rise of nano material, people ask for barrier properties for gases and anti-flammability
Topic, it is intended to solve by the way that PVA and inorganic nano-particle are composite modified, be introduced needed for the performance realization of nano-particle by regulation and control
Performance can be realized by the following method：Laminar nano particle can be considered the impermeable phase of gas because its compact structure is neat, compared with
The laminar nano particle of big L/D ratio, high dispersive and high-orientation can form labyrinth in a polymer matrix, and gas is logical
It is out-of-date to be permeated along the path more distorted.Meanwhile the movement of the laminar nano particle limitation polymer molecular chain of addition, it reduces
Free volume, to improving the gas barrier property of polymer.In addition, by nano-particle of the addition with special properties,
After it reaches certain content, polymer can have such property, and the pattern by regulating and controlling nano-particle be added, and make
It has multiple performance.But technical research compound with inorganic nano-particle PVA at present is not mature enough, acquisition gathers
It still needs further improvement for the barrier property of vinyl alcohol composite material, but also the inflammable general character with plastic material, limits poly-
The practical application of vinyl material.
Invention content
Present invention aim to address the technologies of barrier property difference and poor fire existing for existing polyvinyl alcohol composite material
Problem.
To achieve the goals above, the present invention provides a kind of fire-retardant isolation-type polyvinyl alcohol composite materials, by raw material
Component polyvinyl alcohol, graphene oxide, alpha zirconium phosphate and sulfonated phosphazene microballoon are made up of intercalation-solution composite approach.
Preferably, the polyvinyl alcohol composite material passes through intercalation-solution composite approach by the raw material that following weight matches
It is made：60-94 parts of polyvinyl alcohol, 0.5-5 parts of graphene oxide, 0.5-5 parts of alpha zirconium phosphate, 5-30 parts of sulfonated phosphazene microballoon.
Preferably, the draw ratio of the graphene oxide is 500-5000.
Preferably, the draw ratio of the alpha zirconium phosphate is 100-1500.
Preferably, the sulfonated phosphazene microspherulite diameter is 0.01-5.0 μm.
Preferably, sulfonic group quality accounts for the 0.5-9.0% of microballoon gross mass in the sulfonated phosphazene microballoon.
A kind of preparation method of above-mentioned barrier flame retardant type polyvinyl alcohol composite material, includes the following steps：
S1, by 0.5-5 parts by weight graphene oxide, 0.5-5 parts by weight alpha zirconium phosphate and 5-30 parts by weight sulfonated phosphazenes
Microballoon ultrasonic disperse obtains graphene oxide/alpha zirconium phosphate/sulfonated phosphazene microballoon mixing liquid in 5-50 parts by weight water
System；
S2, the polyvinyl alcohol of 60-94 parts by weight is dissolved in the water of 80-95 DEG C of temperature of 70-100 parts by weight, is obtained
Polyvinyl alcohol water solution；Mixture system made from step S1 is added in polyvinyl alcohol water solution, 5-10h is stirred, is made
Polyvinyl alcohol/sulfonated phosphazene/alpha zirconium phosphate/graphene oxide liquid mixture；
S3, the obtained mixed liquors of step S2 are poured into glass mold, non-isothermal drying removal decentralized medium obtains poly- second
Enol/sulfonated phosphazene/alpha zirconium phosphate/graphene oxide composite membrane (PVA/sPPSZ/ α-ZrP/GO), as fire-retardant isolation-type
Polyvinyl alcohol composite material.
Preferably, in the step S3, the obtained mixed liquors of step S2 are poured by glass by the method for casting film-forming
In mold.
Preferably, the non-isothermal drying is divided into two stages, and the first stage is 20-30 DEG C of 2-3 days dry, second-order
Section is 3-5 days dry for 35-45 DEG C.
Preferably, in the step S2, the polyvinyl alcohol of 60-94 parts by weight is added to 70-100 parts by weight temperature
In 80-95 DEG C of hot water, stirring and dissolving 5-10h obtains polyvinyl alcohol water solution.
The invention has the beneficial effects that：
(1) polyvinyl alcohol/sulfonated phosphazene/alpha zirconium phosphate/graphene oxide composite material (PVA/ prepared by the present invention
SPPSZ/ α-ZrP/GO), using the monolithic thickness of the alpha zirconium phosphate and micron level dispersion of the lamellar structure of Nano grade dispersion
The graphene oxide of degree has larger draw ratio, can be uniformly dispersed in aqueous solution, pass through intercalation-solution composite approach
Polyvinyl alcohol to being dissolved in water carries out oxygen obstruction modification；The sulfonated phosphazene microballoon and oxygen with cross-linked structure introduced simultaneously
Graphite alkene and alpha zirconium phosphate constitute the gas infiltration structure of multidimensional, further improve oxygen barrier property.
(2) exist because containing in a large amount of N, P element and alpha zirconium phosphate molecular structure in sulfonated phosphazene molecular structure
The P element of certain content so that polyvinyl alcohol/sulfonated phosphazene/alpha zirconium phosphate/graphene oxide composite material has both barrier anti-flammability
Energy；Not only solved the problems, such as that prior art preparation polyvinyl alcohol material oxygen-barrier property was bad, but also to solve plastic material inflammable
The problem of.
(3) comprehensive performances such as mechanical property, hot property of polyvinyl alcohol composite material also further increase.
(4) decentralized medium is water in polyvinyl alcohol composite material preparation process, nontoxic and pollution-free, and ecological, environmental protective meets
Instantly environment-friendly materials development trend；And preparation process is simple, and it is of low cost, it is easy to industrialized production；With prodigious practical valence
Value and promotional value.
Description of the drawings
The oxygen of polyvinyl alcohol composite material prepared by Fig. 1, embodiment 1 and the pure polyvinyl alcohol material of comparative example 1 permeates
Coefficient figure.
The heat release speed of polyvinyl alcohol composite material prepared by Fig. 2, embodiment 1 and the pure polyvinyl alcohol material of comparative example 1
Rate (HRR) figure.
The life cigarette rate of polyvinyl alcohol composite material and the pure polyvinyl alcohol material of comparative example 1 prepared by Fig. 3, embodiment 1
(SPR) figure.
Specific implementation mode
Hereinafter, preferred embodiments of the present invention will be described with reference to the accompanying drawings, it should be understood that preferred reality described herein
Apply example only for the purpose of illustrating and explaining the present invention and is not intended to limit the present invention.
Embodiment 1
A kind of preparation method of barrier flame retardant type polyvinyl alcohol composite material, includes the following steps：
Step S1, the α-phosphorus for being 200 by graphene oxide that 0.7 parts by weight draw ratio is 500,0.5 parts by weight draw ratio
Sour zirconium and 5 parts by weight grain sizes are that the sulfonated phosphazene microballoon that 1 μm of sulfonation degree is 5% is added in 10 parts by weight water, and 100 kHz are super
Sound disperses, and ultrasonic time 60min obtains sulfonated phosphazene/alpha zirconium phosphate/graphene oxide liquid mixture system；Wherein, sulfonation degree
Refer to that sulfonic group quality accounts for the 5% of microballoon gross mass in the sulfonated phosphazene microballoon for 5%；
Step S2, by the polyvinyl alcohol of 94 parts by weight be added 95 DEG C of 75 parts by weight temperature deionized water, stirring and dissolving 5h,
Obtain polyvinyl alcohol water solution；Then by sulfonated phosphazene/alpha zirconium phosphate/graphene oxide liquid mixture system made from step S1
Be added in polyvinyl alcohol water solution, in 1000rpm magnetic agitation 5h, be made polyvinyl alcohol/sulfonated phosphazene/alpha zirconium phosphate/
Graphene oxide liquid mixture；
Step S3, polyvinyl alcohol/sulfonated phosphazene/alpha zirconium phosphate/graphene oxide liquid mixture prepared by step S2 is fallen
Enter in glass mold, first 2 days dry at 25 DEG C, then at 35 DEG C, drying obtains having barrier flame retardant property in 5 days to remove moisture
Polyvinyl alcohol composite material (PVA/sPPSZ/ α-ZrP/GO).
Embodiment 2
A kind of preparation method of barrier flame retardant type polyvinyl alcohol composite material, includes the following steps：
Step S1, by 1 parts by weight draw ratio is 2000 graphene oxides, 1 parts by weight draw ratio is 500 alpha zirconium phosphate and
10 parts by weight grain sizes are that the sulfonated phosphazene microballoon that 0.5 μm of sulfonation degree is 3% is added in 20 parts by weight water, 100 kHz ultrasound
Dispersion, ultrasonic time 30min obtain sulfonated phosphazene/alpha zirconium phosphate/graphene oxide liquid mixture system；Wherein, sulfonation degree is
3% refers to that sulfonic group quality accounts for the 3% of microballoon gross mass in the sulfonated phosphazene microballoon；
Step S2, by the polyvinyl alcohol of 88 parts by weight be added 85 DEG C of 75 parts by weight temperature deionized water, stirring and dissolving 6h,
Obtain polyvinyl alcohol water solution；Then by sulfonated phosphazene/alpha zirconium phosphate/graphene oxide liquid mixture system made from step S1
Be added in polyvinyl alcohol water solution, in 8000rpm magnetic agitation 7h, be made polyvinyl alcohol/sulfonated phosphazene/alpha zirconium phosphate/
Graphene oxide divides mixed liquor；
Step S3, the polyvinyl alcohol/sulfonated phosphazene/alpha zirconium phosphate prepared step S2 by the method for casting film-forming/
Graphene oxide liquid mixture is poured into glass mold, first 3 days dry at 35 DEG C, and then at 40 DEG C, drying is obtained for 5 days with removing moisture
To the polyvinyl alcohol composite material (PVA/sPPSZ/ α-ZrP/GO) with fire-retardant barrier property.
Embodiment 3
Step S1, by 2 parts by weight draw ratios are 3000 graphene oxides, 3 parts by weight draw ratios are 1000 alpha zirconium phosphate
It is that the sulfonated phosphazene microballoon that 2 μm of sulfonation degrees are 9% is added in 25 parts by weight water with 15 parts by weight grain sizes, 100 kHz ultrasound
Dispersion, ultrasonic time 60min obtain sulfonated phosphazene/alpha zirconium phosphate/graphene oxide liquid mixture system.
Step S2, by the polyvinyl alcohol of 60 parts by weight be added 80 DEG C of 90 parts by weight temperature deionized water, stirring and dissolving 6h,
Obtain polyvinyl alcohol water solution；Then by sulfonated phosphazene/alpha zirconium phosphate/graphene oxide liquid mixture system made from step S1
It is added in polyvinyl alcohol water solution, polyvinyl alcohol/sulfonated phosphazene/alpha zirconium phosphate/oxygen is made in 500rpm magnetic agitations 8h
Graphite alkene divides mixed liquor；
Step S3, the polyvinyl alcohol/sulfonated phosphazene/alpha zirconium phosphate prepared step S2 by the method for casting film-forming/
Graphene oxide liquid mixture is poured into glass mold, first 2 days dry at 30 DEG C, then removes moisture within dry 5 days at 40 DEG C, finally
Obtain the polyvinyl alcohol composite material (PVA/sPPSZ/ α-ZrP/GO) with barrier flame retardant property.
Embodiment 4
Step S1, by 5 parts by weight draw ratios are 5000 graphene oxides, 5 parts by weight draw ratios are 1500 alpha zirconium phosphate
It is that the sulfonated phosphazene microballoon that 5 μm of sulfonation degrees are 0.5% is added in 50 parts by weight water with 30 parts by weight grain sizes, 100 kHz are super
Sound disperses, and ultrasonic time 60min obtains sulfonated phosphazene/alpha zirconium phosphate/graphene oxide liquid mixture system.
Step S2, the polyvinyl alcohol of 77 parts by weight is added to the deionized water of 95 DEG C of 100 parts by weight temperature, stirring and dissolving
5h obtains polyvinyl alcohol water solution；Then by sulfonated phosphazene/alpha zirconium phosphate/graphene oxide liquid mixture made from step S1
System is added in polyvinyl alcohol water solution, and polyvinyl alcohol/sulfonated phosphazene/alpha-phosphate is made in 600rpm magnetic agitations 10h
Zirconium/graphene oxide divides mixed liquor；
Step S3, the polyvinyl alcohol/sulfonated phosphazene/alpha zirconium phosphate prepared step S2 by the method for casting film-forming/
Graphene oxide liquid mixture is poured into glass mold, first 3 days dry at 25 DEG C, then removes moisture within dry 5 days at 40 DEG C, finally
Obtain the polyvinyl alcohol composite material (PVA/sPPSZ/ α-ZrP/GO) with barrier flame retardant property.
Comparative example 1
The polyvinyl alcohol of 5 parts by weight is added in the deionized water of 95 DEG C of 100 parts by weight temperature, stirring and dissolving 5h.It will
Poly-vinyl alcohol solution is poured by the method for casting film-forming in glass mold, first 2 days dry at 25 DEG C, then in 35 DEG C of dryings
It removes moisture within 5 days, finally obtains unmodified pure polyvinyl alcohol material.
Polyvinyl alcohol composite material prepared by embodiment 1 and pure polyvinyl alcohol material prepared by comparative example 1 are subjected to oxygen
The test of the performances such as infiltration coefficient, heat release rate (HRR) and smoke rate (SPR).
Oxygen permeability coefficient is tested：Using Jinan blue streak mechanical ＆ electrical technology corporation VAC-A2 type pressure differential gas permeameters.It is real
It is 40 DEG C to test temperature, relative humidity 0%.Sample to be tested is made to the disk of a diameter of 50mm, is positioned between test chamber up and down
And it clamps；It is filled with certain pressure (0.1MPa) nitrogen to test epicoele, and ensures to form a constant pressure difference in sample both sides；
Under the action of differential pressure gradients, oxygen is permeated from high-pressure side (epicoele) to low-pressure side (cavity of resorption), to obtain oxygen infiltration
Coefficient.
Taper calorimetric (CONE) is tested：Using the cone calorimetry (CONE) of FTT UK corporations according to 5660 standards of ISO
Test the parameters such as heat release rate (HRR), the smoke rate (SPR) of sample to be tested, radiation intensity 35KW/m2, sample size
100mm × 100mm × 0.5mm, sample to be tested are placed on masking foil.
Fig. 1 is the oxygen of polyvinyl alcohol composite material prepared by embodiment 1 and pure polyvinyl alcohol material prepared by comparative example 1
Infiltration coefficient figure.From the figure, it can be seen that the pure polyvinyl alcohol material oxygen permeability coefficient (P of comparative example 1O2) it is 1.890 × 10-16cm3cmcm-2s-1Pa-1；Embodiment 1 prepare polyvinyl alcohol composite material due to add sulfonated phosphazene, alpha zirconium phosphate and
Graphene oxide, oxygen permeability coefficient (PO2) it is 0.425 × 10-16cm3cm cm-2s-1Pa-1, reduce 78%.Fig. 2 and Fig. 3 points
Not Wei embodiment 1 prepare polyvinyl alcohol composite material and comparative example 1 prepare pure polyvinyl alcohol material heat release rate
(HRR) and raw cigarette rate (SPR) figure.As can be seen that the rapid burning after lighting of 1 pure PVA film of comparative example, in 463kW m-2There is peak
The fire-retardant isolation-type polyvinyl alcohol composite material of value, embodiment 1 has delayed a period of time just to start to burn after ignition, peak value
For 319kWm-2.For raw cigarette rate, fire-retardant isolation-type polyvinyl alcohol composite material SPR peak of curve is only 0.09m2s-1, more right
1 pure polyvinyl alcohol material of ratio has preferable smoke suppressing effect.
In conclusion polyvinyl alcohol/sulfonated phosphazene/alpha zirconium phosphate/graphene oxide composite material prepared by the present invention has
High oxygen-barrier property, and meet good flame retardant effect simultaneously on this basis, both solve the polyethylene of the prior art
The bad problem of alcohol material oxygen-barrier property, and solve the problems, such as that plastic material is inflammable.Simultaneously in composite material preparation process
Middle decentralized medium is water, nontoxic and pollution-free, ecological, environmental protective, meets environment-friendly materials development trend instantly.
The above described is only a preferred embodiment of the present invention, be not intended to limit the present invention in any form, though
So the present invention has been disclosed as a preferred embodiment, and however, it is not intended to limit the invention, any technology people for being familiar with this profession
Member, without departing from the scope of the present invention, when the technology contents using the disclosure above make a little change or modification
For the equivalent embodiment of equivalent variations, as long as being the content without departing from technical solution of the present invention, according to the technical essence of the invention
To any simple modification, equivalent change and modification made by above example, in the range of still falling within technical solution of the present invention.
Claims (10)
1. a kind of fire-retardant isolation-type polyvinyl alcohol composite material, which is characterized in that by raw material components polyvinyl alcohol, graphite oxide
Alkene, alpha zirconium phosphate and sulfonated phosphazene microballoon are made up of intercalation-solution composite approach.
2. fire-retardant isolation-type polyvinyl alcohol composite material as described in claim 1, which is characterized in that by following weight proportioning
Raw material is made up of intercalation-solution composite approach：60-94 parts of polyvinyl alcohol, 0.5-5 parts of graphene oxide, alpha zirconium phosphate 0.5-5
Part, 5-30 parts of sulfonated phosphazene microballoon.
3. fire-retardant isolation-type polyvinyl alcohol composite material as claimed in claim 2, which is characterized in that the graphene oxide
Draw ratio is 500-5000.
4. fire-retardant isolation-type polyvinyl alcohol composite material as claimed in claim 3, which is characterized in that the length of the alpha zirconium phosphate
Diameter ratio is 100-1500.
5. fire-retardant isolation-type polyvinyl alcohol composite material as claimed in claim 4, which is characterized in that the sulfonated phosphazene is micro-
Spherolite diameter is 0.01-5.0 μm.
6. fire-retardant isolation-type polyvinyl alcohol composite material as claimed in claim 5, which is characterized in that the sulfonated phosphazene is micro-
Sulfonic group quality accounts for the 0.5-9.0% of microballoon gross mass in ball.
7. a kind of preparation method of barrier flame retardant type polyvinyl alcohol composite material as claimed in any one of claims 1 to 6,
It is characterized in that, includes the following steps：
S1, by 0.5-5 parts by weight graphene oxide, 0.5-5 parts by weight alpha zirconium phosphate and 5-30 parts by weight sulfonated phosphazene microballoons
Ultrasonic disperse obtains graphene oxide/alpha zirconium phosphate/sulfonated phosphazene microballoon mixture system in 5-50 parts by weight water；
S2, the polyvinyl alcohol of 60-94 parts by weight is dissolved in the water of 80-95 DEG C of temperature of 70-100 parts by weight, obtains poly- second
Enol aqueous solution；Mixture system made from step S1 is added in polyvinyl alcohol water solution, 5-10h is stirred, poly- second is made
Enol/sulfonated phosphazene/alpha zirconium phosphate/graphene oxide liquid mixture；
S3, the obtained mixed liquors of step S2 are poured into glass mold, non-isothermal drying removal decentralized medium obtains polyethylene
Alcohol/sulfonated phosphazene/alpha zirconium phosphate/graphene oxide composite membrane, as fire-retardant isolation-type polyvinyl alcohol composite material.
8. the preparation method of barrier flame retardant type polyvinyl alcohol composite material as claimed in claim 7, which is characterized in that the step
In rapid S3, the obtained mixed liquors of step S2 are poured into glass mold by the method for casting film-forming.
9. the preparation method of barrier flame retardant type polyvinyl alcohol composite material as claimed in claim 8, which is characterized in that described non-
Isothermal drying is divided into two stages, and the first stage is 20-30 DEG C 2-3 days dry, and second stage is 35-45 DEG C 3-5 days dry.
10. the preparation method of barrier flame retardant type polyvinyl alcohol composite material as claimed in claim 7, which is characterized in that described
In step S2, the polyvinyl alcohol of 60-94 parts by weight is added in the hot water of 80-95 DEG C of 70-100 parts by weight temperature, stirring is molten
5-10h is solved, polyvinyl alcohol water solution is obtained.
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