CN109181186A - A kind of biodegradable hydrophobicity PVA resin composite materials - Google Patents
A kind of biodegradable hydrophobicity PVA resin composite materials Download PDFInfo
- Publication number
- CN109181186A CN109181186A CN201811339843.9A CN201811339843A CN109181186A CN 109181186 A CN109181186 A CN 109181186A CN 201811339843 A CN201811339843 A CN 201811339843A CN 109181186 A CN109181186 A CN 109181186A
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- CN
- China
- Prior art keywords
- pva
- composite materials
- resin composite
- pva resin
- hydrophobicity
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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- 239000000463 material Substances 0.000 title claims abstract description 100
- 239000000805 composite resin Substances 0.000 title claims abstract description 55
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910010272 inorganic material Inorganic materials 0.000 claims abstract description 27
- 239000011147 inorganic material Substances 0.000 claims abstract description 27
- 239000004014 plasticizer Substances 0.000 claims abstract description 27
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 17
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 17
- 238000006731 degradation reaction Methods 0.000 claims abstract description 12
- 230000015556 catabolic process Effects 0.000 claims abstract description 11
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 10
- 239000011737 fluorine Substances 0.000 claims abstract description 10
- 230000002209 hydrophobic effect Effects 0.000 claims abstract description 10
- 229920002472 Starch Polymers 0.000 claims abstract description 8
- 239000008107 starch Substances 0.000 claims abstract description 8
- 235000019698 starch Nutrition 0.000 claims abstract description 8
- 239000003607 modifier Substances 0.000 claims abstract description 7
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- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 224
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 122
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 51
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 47
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 45
- -1 hydroxyl sulfo group Chemical class 0.000 claims description 26
- 235000011187 glycerol Nutrition 0.000 claims description 20
- 239000002131 composite material Substances 0.000 claims description 16
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 15
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- 239000001301 oxygen Substances 0.000 claims description 11
- 229910052760 oxygen Inorganic materials 0.000 claims description 11
- 229920001223 polyethylene glycol Polymers 0.000 claims description 11
- 229940117986 sulfobetaine Drugs 0.000 claims description 11
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- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 7
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- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical group CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 claims description 6
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- 235000013539 calcium stearate Nutrition 0.000 claims description 4
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 claims description 4
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- VSAWBBYYMBQKIK-UHFFFAOYSA-N 4-[[3,5-bis[(3,5-ditert-butyl-4-hydroxyphenyl)methyl]-2,4,6-trimethylphenyl]methyl]-2,6-ditert-butylphenol Chemical compound CC1=C(CC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)C(C)=C(CC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)C(C)=C1CC1=CC(C(C)(C)C)=C(O)C(C(C)(C)C)=C1 VSAWBBYYMBQKIK-UHFFFAOYSA-N 0.000 claims description 3
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- 239000003513 alkali Substances 0.000 claims description 2
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- QAEDZJGFFMLHHQ-UHFFFAOYSA-N trifluoroacetic anhydride Chemical compound FC(F)(F)C(=O)OC(=O)C(F)(F)F QAEDZJGFFMLHHQ-UHFFFAOYSA-N 0.000 claims 2
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims 1
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- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 6
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- RSWGJHLUYNHPMX-UHFFFAOYSA-N 1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-octahydrophenanthrene-1-carboxylic acid Chemical compound C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 2
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- GDTSJMKGXGJFGQ-UHFFFAOYSA-N 3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound O1B([O-])OB2OB([O-])OB1O2 GDTSJMKGXGJFGQ-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L3/00—Compositions of starch, amylose or amylopectin or of their derivatives or degradation products
- C08L3/02—Starch; Degradation products thereof, e.g. dextrin
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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
- C08L2201/00—Properties
- C08L2201/06—Biodegradable
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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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
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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Abstract
The present invention relates to a kind of biodegradable hydrophobicity PVA resin composite materials, belong to technical field of polymer materials.In order to solve the problems, such as that existing thermal decomposition temperature is low and poor water resistance, a kind of biodegradable hydrophobicity PVA resin composite materials are provided, which includes the parts by weight of following component: PVA:60~80；Hydroxyl sulfo group class degradation of promoter: 1.0~5.0；Fluorine-containing hydrophobic modifier: 0.5~5.0；PVA decomposing inhibitor: 0.5~5.0；Plasticizer: 10~40；Inorganic material: 1.0~30；Antioxidant: 0.5~5.0；Processing aid: 0.1~5.0；Starch: 0~60.The present invention can make melting temperature control at 140 DEG C~250 DEG C, and thermal decomposition temperature is greater than 300 DEG C or more, and temperature of initial decomposition is high；Water solution temperature is controlled at 75 DEG C~100 DEG C, realizes the effect for having both and widening melting temperature and improving water resistance.
Description
Technical field
The present invention relates to a kind of biodegradable hydrophobicity PVA resin composite materials, belong to technical field of polymer materials.
Background technique
Polyvinyl alcohol is the known polymer with very excellent high barrier of one kind, still, due to its fusing point base
Close to even higher than thermal decomposition temperature in sheet, make it unsuitable for being thermoformed, especially the polyethylene of degree of hydrolysis about 99%
Alcohol homopolymer can not be thermoformed completely.Further say, since PVA is polyhydroxy structure, there are it is intermolecular with
Intramolecular strong hydrogen bonding active force, so that melting temperature is very close with decomposition temperature, 220 DEG C of fusing point or so of PVA, thermal decomposition temperature
235 DEG C or so of degree, and rising makes thermal decomposition temperature begin to decompose at 160 DEG C, therefore can not process, and makes to be difficult to pass through heat when processing
Modeling processing, especially room temperature water-insoluble PVA product of the alcoholysis degree greater than 95% are more difficult to process.In order to improve the property of PVA material
Can, it is existing also to have many modified PVA composite materials.
It is mainly to make plasticizer using a large amount of water to improve as existing, it is steady although melt processing temperature can be reduced
Qualitative difference, product to widen temperature very poor and be unable to reach effective application.For another example Chinese patent application (publication number:
CN102234405A) and (publication number: CN102241862A) discloses water-fast PVA composition and its fusion preparation method, they
Common feature is small molecule plasticizer alcohols, amides and macromolecule plasticising, such as polylactic acid, polyester, polyurethane.Although
They can be improved the water resistance of material, but still there is a problem of being granulated easy but blown film hardly possible, mainly cannot be effective
Prevent PVA melt-processed cross-linking reaction.
For another example Chinese patent application (publication number: CN102321325A) is then modified by adding calcium chloride/lithium chloride
Improve plasticizing capacity, however, the water imbibition of the material system is very strong, difficulty of processing is big, while it is discarded after easily cause soil salt
Environment is polluted in alkalization.There is water-resistant polyvinyl alcohol as Chinese patent application (publication number: CN106700362A) discloses one kind
Whole degrading film and preparation method thereof makees crosslinking agent by using borides such as borax and is modified, and still, is difficult to grasp
The degree of cross linking, and be also only that by granulation and be easy, but the problem of blown film hardly possible.
For disadvantages mentioned above, and at present, PVA melt-processed does each based article above all how to widen thermal decomposition temperature
And raising water resistance makes the beneficial characteristics for playing PVA material, and it is very slow how to improve PVA product degradation speed, and is degrading
Easy polycondensation influences the problem of disintegration rate in the process.
Summary of the invention
The present invention is directed to the above defect existing in the prior art, and it is multiple to provide a kind of biodegradable hydrophobicity PVA resin
Condensation material solves the problems, such as it is how to realize the performance widened thermal decomposition temperature and improve water resistance.
The purpose of the present invention is what is be achieved by the following technical programs, a kind of biodegradable hydrophobicity PVA resin
Composite material, which is characterized in that the composite material includes the parts by weight of following component:
PVA:60~80；Hydroxyl sulfo group class degradation of promoter: 1.0~5.0；Fluorine-containing hydrophobic modifier: 0.5~5.0；PVA points
Solution inhibitor: 0.5~5.0；Plasticizer: 10~40；Inorganic material: 1.0~30；Antioxidant: 0.5~5.0；Processing aid: 0.1
~5.0；Starch: 0~60.
The present invention by being added hydroxyl sulfo group class degradation of promoter, fluorine-containing hydrophobic modifier, PVA decomposing inhibitor in the material
And plasticizer, it can effectively improve the performance of material, effective to improve thermal decomposition temperature and its water solution temperature, heat is widened in realization
Decomposition temperature and the temperature of initial decomposition for improving thermal decomposition, effectively avoid secondary operation xanthochromia, to make its composite wood
The melting temperature of material differs larger with thermal decomposition temperature, squeezes out the effect of processing and to realize and be conducive to fusion plastification conducive to blowing
Film processing etc., so that effective solution PVA material makes melting temperature and divide there are intermolecular with intramolecular strong hydrogen bonding active force
It is close to solve temperature, it is difficult to thermoplastic processing；And the difficult processing of the insoluble PVA product of normal-temperature water using PVA alcoholysis degree greater than 95%
Problem.Further, present invention introduces hydroxyl sulfo group class degradation of promoter can effectively realize that adjusting degradation time and raising collapses
The effect of solution rate, and the fluorine-containing hydrophobic modifier introduced can effectively reduce the hydrophobic properties of the surface of respective material product, have
Conducive to the stabilization of barrier properties for gases, excellent gas barrier property is realized, PVA is carried out by the collective effect of above-mentioned each material
It is modified, effectively improve performance, composite material have melt index (MI) reach 0.5~25g/10min.190 DEG C of .2160g~
5000g, and melting temperature can be improved initial pyrolyzation temperature and make heat in the plasticizing resin of 140 DEG C~250 DEG C ranges
Decomposition temperature is greater than 300 DEG C or more and the control of its water solution temperature can be made at 75 DEG C~95 DEG C, and realization is widened melting temperature and mentioned
The effect of enhanced water resistance and water-resistant stability, while the performance of low gas air penetrability and physical mechanics intensity is had both, so that material is existed
The performance that injection molding or blown film are processed can be more effectively suitable in process, improve the processing performance of material.
In above-mentioned biodegradable hydrophobicity PVA resin composite materials, preferably, hydroxyl sulfo group class degradation promotes
Agent is selected from lauryl hydroxyl sulfo betaine, and one in dodecyl hydroxyl sulfo betaine and Coco-Hydroxysultaine
Kind is several.The degradation speed that PVA material can more effectively be improved avoids easily occurring polycondensation in degradation process and influencing to be disintegrated
Property, realize the effect for improving whole disintegration rate.
In above-mentioned biodegradable hydrophobicity PVA resin composite materials, preferably, the fluorine-containing hydrophobic modifier choosing
From 17 fluorine decyl trimethyl oxysilane, fluorine-containing 13 oxygroup triethoxysilane, perfluoro capryl triethoxysilane and three
One or more of fluoroacetic acid acid anhydride.The improvement gas barrier property and lower water absorption rate of material can more effectively be improved,
Make whole gas permeation rate < 100cm3/cm2* 24H*0.1Mpa makes to be more advantageous to have both and be processed by injection molding or blown film
Performance.
In above-mentioned biodegradable hydrophobicity PVA resin composite materials, preferably, the PVA decomposing inhibitor selects
From 1- butyl -3- methylimidazole tetraborate, 1- butyl -3- methylimidazole villaumite and 1- vinyl -3- ethyl imidazol(e) borate
One or more of.The decomposition of PVA can effectively be inhibited and improve the resistance to water solubility of material, make that there is high water resistance stability
Effect, can effectively solve the problem that can only solve to be easy to injection molding and difficult asking suitable for blown film present in existing modified PVA material
Topic can be such that this composite material is integrally more advantageous to and be suitable for injection molding and blown film processing, improve processability.
In above-mentioned biodegradable hydrophobicity PVA resin composite materials, preferably, the plasticizer is selected from polyalcohol
Class material.By using polyol masses, it can make each ingredient in material that there is better synergistic effect, to make composite material
Tensile strength performance with higher and elongation at break on the whole realize excellent physical and mechanical property.As further
It is preferred that the polyalcohols material be selected from ethylene glycol, polyethylene glycol, glycerol, polyglycereol, propylene glycol, polypropylene glycol, a glycol,
One or more of diethylene glycol (DEG), triethylene glycol, acetic anhydride glyceride, two acetoglycerides and triacetyl glycerine.As optimal
Choosing, the polyalcohols material be a variety of mixed modes, such as using ethylene glycol, polyethylene glycol, glycerol, polyglycereol, propylene glycol,
Polypropylene glycol, a glycol, diethylene glycol (DEG) and triethylene glycol mixture；Or use an acetoglyceride, two acetoglycerides and three
The mixture of acetoglyceride；Or using the mixed of propylene oxide and pentaerythrite, 1,4-butanediol, glycerine and D-sorbite
Close object.The strength character of material can more effectively be increased using above-mentioned compounding mode, and can more effectively guarantee material
Compatibility makes have preferable melting temperature and preferable thermal decomposition temperature, more effectively realizes fusion plastification processing and blown film
Processing, is conducive to industrialized production.
In above-mentioned biodegradable hydrophobicity PVA resin composite materials, preferably, the inorganic material is selected from golden red
One or more of stone-type titanium dioxide, anatase titanium dioxide, talcum powder, calcium carbonate, silica and magnesium hydroxide.Energy
The strength character of material is enough effectively increased, and there is preferable compatibility, the particle of inorganic material is preferably made to be greater than 2500 here
Mesh is conducive to improve its mixing uniformity, further guarantee performance, here preferably with rutile titanium dioxide, sharp
The mixture of titanium-type titanium dioxide and talcum powder, and make their weight ratio 4:4:1.8, silicon can be added during mixing
Alkane coupling agent such as Silane coupling reagent KH-570, can effectively increase the compatibility of inorganic material, make to be more advantageous to uniform dispersion
Into above-mentioned material, realizes and increase mechanical property and improvement material property.
In above-mentioned biodegradable hydrophobicity PVA resin composite materials, preferably, the processing aid is selected from tristearin
One or more of sour zinc, calcium stearate, magnesium stearate, oleamide and methyl methacrylate.Purpose is to improve
The processing performance of material makes to be more advantageous to machine-shaping, guarantees the effect of material property.
In above-mentioned biodegradable hydrophobicity PVA resin composite materials, preferably, the antioxidant is selected from antioxidant
1010, one of irgasfos 168, antioxidant 300, antioxidant 330, antioxidant triphenyl phosphite and tris(nonyl phenyl) phosphate or
It is several.Purpose is the antioxygenic property in order to improve material, improves its anti-aging performance, guarantees the service life of material and whole
Body performance.
In above-mentioned biodegradable hydrophobicity PVA resin composite materials, preferably, the degree of polymerization of the PVA is
600~2600；The alcoholysis degree of the PVA is 88~99.9%.
In conclusion compared with prior art, the present invention having the advantage that
1. combining each raw material by using hydroxyl sulfo group class degradation of promoter, fluorine-containing hydrophobic modifier and PVA decomposing inhibitor
Common synergistic effect, can effectively improve the entirety of material, can make melting temperature control in 140 DEG C~250 DEG C ranges
Plasticizing resin, and thermal decomposition temperature is greater than 300 DEG C or more, and temperature of initial decomposition is high, keeps temperature difference larger, is more advantageous to
Fusion plastification processing, improves machinability, and the control of its water solution temperature can be made at 75 DEG C~100 DEG C, and realization can have both
Realize the effect widened melting temperature and improve water resistance.
2. by using composite elasticizer can more effective physical mechanics strength character, make with high tensile strength properties
With the effect of elongation at break.
3. biodegradable hydrophobicity PVA resin composite materials of the invention have melt index (MI) reach 0.5~
The performance of 25g/10min.190 DEG C of .2160g~5000g and higher thermal decomposition temperature and gas air penetrability, make material more can
It is enough to be processed suitable for injection molding or blown film, overall gas transmitance < 100cm3/cm2*24H*0.1Mpa。
Specific embodiment
Below by specific embodiment, the technical solutions of the present invention will be further described, but the present invention is simultaneously
It is not limited to these embodiments.
Embodiment 1
Biodegradable hydrophobicity PVA resin composite materials in the present embodiment include the parts by weight of following component:
PVA:69.3, and PVA is the compound of PVA0599 and PVA2099, the mass ratio of PVA0599:PVA2099 is 3:
7；Lauryl hydroxyl sulfo betaine: 5.0；17 fluorine decyl trimethyl oxysilane: 0.8；1- vinyl -3- ethyl imidazol(e) boron
Hydrochlorate: 1.2；Plasticizer: 18；Inorganic material: 3.0；Antioxidant 1010: 0.5, antioxidant triphenyl phosphite: 0.5；Stearic acid
Zinc: 0.4；
Above-mentioned plasticizer is glycerol, Natrulon H-10 and ethylene glycol mix and form composite elasticizer, and glycerol: polyglycereol-
10: the weight ratio of glycol glycerin is 2:2:1, and 0.01~0.05% phosphoric acid can be added in mixing or sulfuric acid makees catalyst
Corresponding composite elasticizer is formed after being heated to 60 DEG C of mixings cooling in 30~60 minutes, by being pre-mixed, can be increased
Its performance being plasticized；
The mixture of above-mentioned inorganic material rutile titania stone-type titanium dioxide, rutile titanium dioxide and talcum powder, and they
Weight ratio be 4.0:4.0:1.8, when mixing, the Silane coupling reagent KH-570 of 2 parts by weight can be added, can be improved inorganic material
Compatibility, have better reinforcing effect.
Above-mentioned biodegradable hydrophobicity PVA resin composite materials can obtain by the following method:
According to the consumption proportion of above-mentioned each raw material, by above-mentioned raw materials put into high mixer and control temperature 40~120
DEG C cond heat side stir process 35min below, it is then cooled to room temperature, after placing 24 hours, then put into twin-screw
It is granulated in pelletizer, temperature controls 140~220 DEG C, obtains corresponding biodegradable hydrophobicity PVA resin composite materials grain
Son.Further, when in use, obtained biodegradable hydrophobicity PVA resin composite materials particle is put into injection molding machine
Note bottle is carried out, is obtained PVA bottles corresponding.Carry out corresponding performance test, the results showed that, PVA bottles of water solution temperatures 75~100 of gained
DEG C, PVA bottles of thickness 0.2mm, tensile strength > 35Mpa (23 DEG C of .50%RH. tensile speeds are 100mm/min), elongation at break
124%, oxygen transmission rate < 48cm3/m2* 24H*0.1Mpa, bottle surface water imbibition 23.5%, the melting temperature of material is 140 DEG C~
250 DEG C, 274 DEG C of initial pyrolyzation temperature, the fluorinated hydrophobic modifying agent of polyvinyl alcohol and its fluorinated hydrophobic for studying polyvinyl alcohol
Modifying agent and its research thermal decomposition temperature reach 300 DEG C or more, it is seen then that melting temperature differs increase with thermal decomposition temperature, realizes
Thermal decomposition temperature is widened, the effect of temperature of initial decomposition is improved.
Embodiment 2
Biodegradable hydrophobicity PVA resin composite materials in the present embodiment include the parts by weight of following component:
PVA:68, and PVA is the compound of PVA1299 and PVA1799, the mass ratio of PVA1299:PVA1799 is 3:7；
Coco-Hydroxysultaine: 1.0；Perfluoro capryl Ethoxysilane: 1.2；1- butyl -3- methylimidazole borate: 1.0；
Plasticizer: 20；Inorganic material: 5.0；Antioxidant 1010: 0.5, antioxidant 300: 0.5, antioxidant triphenyl phosphite: 0.5；Firmly
Resin acid zinc: 0.4, oleamide: 0.3.
Wherein, above-mentioned plasticizer is glycerine, a glycol, diethylene glycol (DEG), triethylene glycol and polyethylene glycol (molecular weight 2000)
The composite elasticizer of mixing and formation, and glycerine: a glycol: diethylene glycol (DEG): triethylene glycol: the weight ratio of polyethylene glycol is 3.0:
1.5:1.5:1.5:2.5, in mixing can be added 0.01~0.05% phosphoric acid or sulfuric acid do catalyst be heated to 60 DEG C it is mixed
Corresponding composite elasticizer is formed after closing stirring cooling in 30~60 minutes, by being pre-mixed, the performance of its plasticising can be increased；
The mixture of above-mentioned inorganic material rutile titania stone-type titanium dioxide, rutile titanium dioxide and talcum powder, and they
Weight ratio be 4.0:4.0:1.8, when mixing, the Silane coupling reagent KH-570 of 2 parts by weight can be added, can be improved inorganic material
Compatibility, have better reinforcing effect.
That the preparation method is the same as that of Example 1 is consistent for above-mentioned biodegradable hydrophobicity PVA resin composite materials specific, here not
It repeats again, further using injection molding in the biodegradable hydrophobicity PVA resin composite materials particle investment injection molding machine
At PVA bottles.
Carry out corresponding performance test, the results showed that, 75~100 DEG C of water solution temperature of PVA bottles of gained, bottle thickness 0.2mm is drawn
Stretch intensity > 46Mpa (23 DEG C, 50%RH. tensile speed 100mm/min), elongation at break 134%, oxygen transmission rate < 21cm3/m2*
24H*0.1Mpa, bottle surface water absorption rate 28.6%, the melting temperature of material are 140 DEG C~250 DEG C, initial pyrolyzation temperature 283
DEG C, thermal decomposition temperature reaches 300 DEG C or more.
Embodiment 3
Biodegradable hydrophobicity PVA resin composite materials in the present embodiment include the parts by weight of following component:
PVA:65, and PVA is the compound of PVA0599 and PVA1799, the mass ratio of PVA0599:PVA1799 is 3:7；
Dodecyl hydroxyl sulfo betaine: 5.0；13 oxygroup triethoxysilanes: 0.8；1- vinyl -3- ethyl imidazol(e) boric acid
Salt: 1.2；Plasticizer: 30；Inorganic material: 4.0；Irgasfos 168: 0.5, antioxidant triphenyl phosphite: 0.5；Zinc stearate:
0.7, methyl methacrylate: 0.2.
Wherein, above-mentioned plasticizer is using corresponding composite elasticizer, i.e. glycerol, Natrulon H-10 and ethylene glycol in embodiment 1
The composite elasticizer of mixing and formation, and glycerol: Natrulon H-10: the weight ratio of glycol glycerin is 2:2:1.
The mixture of above-mentioned inorganic material rutile titania stone-type titanium dioxide, rutile titanium dioxide and talcum powder, and they
Weight ratio be 4.0:4.0:1.8.
That the preparation method is the same as that of Example 1 is consistent for above-mentioned biodegradable hydrophobicity PVA resin composite materials specific, here not
It repeats again, further using injection molding in the biodegradable hydrophobicity PVA resin composite materials particle investment injection molding machine
At PVA bottles.
Carry out corresponding performance test, the results showed that, 75~100 DEG C of water solution temperature of PVA bottles of gained, bottle thickness 0.2mm is drawn
Stretch intensity > 32Mpa (23 DEG C, 50%RH. tensile speed 100mm/min), elongation at break 131%, oxygen transmission rate < 35cm3/m2*
24H*0.1Mpa, bottle surface water absorption rate 19.7%, the melting temperature of material are 140 DEG C~250 DEG C ranges, initial pyrolyzation temperature
>=250 DEG C, thermal decomposition temperature reaches 300 DEG C or more.
Embodiment 4
Biodegradable hydrophobicity PVA resin composite materials in the present embodiment include the parts by weight of following component:
PVA:75, and PVA is the compound of PVA0599 and PVA2499, the mass ratio of PVA0599:PVA2499 is 4:6；
Dodecyl hydroxyl sulfo betaine: 4.0；13 oxygroup triethoxysilanes: 1.0；1- vinyl -3- ethyl imidazol(e) boric acid
Salt: 2.0；Plasticizer: 10；Inorganic material: 3.0；Irgasfos 168: 0.5, antioxidant triphenyl phosphite: 0.5；Zinc stearate:
0.7, methyl methacrylate: 0.3.
Wherein, above-mentioned plasticizer is glycerine, an acetoglyceride, two triacetins from ester, triacetyl glycerine and gathers
The composite elasticizer of ethylene glycol (molecular weight 10000) mixing and formation, and glycerine: an acetoglyceride: two triacetins are certainly
Ester: triacetyl glycerine: the weight ratio of polyethylene glycol is 4.0:1.5:1.5:1.5:2.5,0.01 can be added in mixing~
0.05% phosphoric acid or sulfuric acid does after catalyst is heated to 60 DEG C of mixings cooling in 30~60 minutes and forms corresponding compound increasing
Agent is moulded, by being pre-mixed, the performance of its plasticising can be increased；
Above-mentioned inorganic material is using corresponding inorganic material, i.e. rutile titania stone-type titanium dioxide, rutile-type two in embodiment 1
The mixture of titanium oxide and talcum powder.
That the preparation method is the same as that of Example 1 is consistent for above-mentioned biodegradable hydrophobicity PVA resin composite materials specific, here not
It repeats again, is further put into using the composite particles and carry out blown film in inflation film manufacturing machine, obtain corresponding film, film thickness is
0.08mm。
Carry out corresponding performance test, the results showed that, 75~100 DEG C of the water solution temperature of gained PVA film, tensile strength >
20Mpa, elongation at break 121%, oxygen transmission rate < 31cm3/m2* 24H*0.1Mpa, film surface water absorption rate 26.3%, material melt
Melting temperature is 140 DEG C~250 DEG C ranges, and 276 DEG C of initial pyrolyzation temperature, thermal decomposition temperature reaches 300 DEG C or more.
Embodiment 5
Biodegradable hydrophobicity PVA resin composite materials in the present embodiment include the parts by weight of following component:
PVA:80, and PVA is the compound of PVA1299 and PVA2499, the mass ratio of PVA1299:PVA2499 is 3:7；
Coco-Hydroxysultaine: 5.0；Perfluoro capryl triethoxysilane: 1.0；1- butyl -3- methylimidazole villaumite: 4.0；
Plasticizer: 40, plasticizer is polypropylene glycol；Inorganic material rutile titanium dioxide: 5.0；Irgasfos 168: 0.5, antioxidant
Tris(nonyl phenyl) phosphate: 0.5；Calcium stearate: 2.0, methyl methacrylate: 3.0, starch: 10.
That the preparation method is the same as that of Example 1 is consistent for above-mentioned biodegradable hydrophobicity PVA resin composite materials specific, here not
It repeats again, is further put into inflation film manufacturing machine and blown using the biodegradable hydrophobicity PVA resin composite materials particle
Film obtains corresponding film, film thickness 0.08mm.
Carry out corresponding performance test, the results showed that, 80~100 DEG C of the water solution temperature of gained PVA film, tensile strength >
35Mpa, elongation at break 123%, oxygen transmission rate < 28cm3/m2* 24H*0.1Mpa, film surface water absorption rate 18.9%, material melt
Melting temperature is 150 DEG C~250 DEG C ranges, and 284 DEG C of initial pyrolyzation temperature, thermal decomposition temperature reaches 320 DEG C or more.
Embodiment 6
Biodegradable hydrophobicity PVA resin composite materials in the present embodiment include the parts by weight of following component:
PVA:60, and PVA is PVA1299；Coco-Hydroxysultaine: 1.0, lauryl hydroxyl sulfo betaine:
2.0；17 fluorine decyl trimethyl oxysilane: 5.0；1- vinyl -3- ethyl imidazol(e) borate: 5.0；Plasticizer: 10, plasticising
Agent is the mixture of acetic anhydride glyceride, two acetoglycerides and triacetyl glycerine, mass ratio 1:0.5:0.3；Inorganic material
Material talcum powder: 1.0, the partial size of talcum powder is 3000 mesh or so；Irgasfos 168: 0.5, antioxidant tris(nonyl phenyl) phosphate: 0.5；Firmly
Resin acid calcium: 2.0, methyl methacrylate: 3.0, starch: 20.
That the preparation method is the same as that of Example 1 is consistent for above-mentioned biodegradable hydrophobicity PVA resin composite materials specific, here not
It repeats again, is further put into inflation film manufacturing machine and blown using the biodegradable hydrophobicity PVA resin composite materials particle
Film obtains corresponding film, film thickness 0.09mm.
Carry out corresponding performance test, the results showed that, 80~100 DEG C of the water solution temperature of gained PVA film, tensile strength >
38Mpa, elongation at break 118%, oxygen transmission rate < 29cm3/m2* 24H*0.1Mpa, film surface water absorption rate 19.2%, material melt
Melting temperature is 150 DEG C~250 DEG C ranges, and 268 DEG C of initial pyrolyzation temperature, thermal decomposition temperature reaches 320 DEG C or more.
Embodiment 7
Biodegradable hydrophobicity PVA resin composite materials in the present embodiment include the parts by weight of following component:
PVA:70, and PVA is the mixture of PVA0599 and PVA2099, and the mass ratio of the two is 3:6；Cocoyl hydroxyl
Sulfobetaines: 0.5, lauryl hydroxyl sulfo betaine: 0.5；17 fluorine decyl trimethyl oxysilane: 0.5；1- ethylene
Base -3- ethyl imidazol(e) borate: 0.5；Plasticizer: 40, plasticizer is ethylene glycol, polyethylene glycol, glycerol, polyglycereol, propylene glycol
With the mixture of polypropylene glycol, mass ratio 0.5:0.3:0.6:0.5:0.3:0.2；Inorganic material silica: 10, titanium dioxide
The partial size of silicon is 2500 mesh or so；Irgasfos 168: 0.5, calcium stearate: 2.0, methyl methacrylate: 3.0, starch: 40.
That the preparation method is the same as that of Example 1 is consistent for above-mentioned biodegradable hydrophobicity PVA resin composite materials specific, here not
It repeats again, is further put into injection molding machine and infused using the biodegradable hydrophobicity PVA resin composite materials particle
Bottle, obtain it is PVA bottle corresponding, bottle thickness be 0.2mm.
Carry out corresponding performance test, the results showed that, 80~100 DEG C of the water solution temperature of gained PVA film, tensile strength >
45Mpa, elongation at break 123%, oxygen transmission rate < 31cm3/m2* 24H*0.1Mpa, film surface water absorption rate 22.3%, material melt
Melting temperature is 150 DEG C~250 DEG C ranges, and 276 DEG C of initial pyrolyzation temperature, thermal decomposition temperature reaches 365 DEG C or more.
Embodiment 8
Biodegradable hydrophobicity PVA resin composite materials in the present embodiment include the parts by weight of following component:
PVA:70, and PVA is the mixture of PVA0599 and PVA2099, and the mass ratio of the two is 3:6；Cocoyl hydroxyl
Sulfobetaines: 0.5, lauryl hydroxyl sulfo betaine: 0.5；17 fluorine decyl trimethyl oxysilane: 0.5；1- ethylene
Base -3- ethyl imidazol(e) borate: 0.5；Plasticizer: 40, plasticizer is ethylene glycol, polyethylene glycol, glycerol, polyglycereol, propylene glycol
With the mixture of polypropylene glycol, mass ratio 0.5:0.3:0.6:0.5:0.3:0.2；Inorganic material silica: 10, titanium dioxide
The partial size of silicon is 2500 mesh or so；Antioxidant 1010: 1.0, zinc stearate: 0.1, starch: 60.
That the preparation method is the same as that of Example 1 is consistent for above-mentioned biodegradable hydrophobicity PVA resin composite materials specific, here not
It repeats again, is further put into injection molding machine and infused using the biodegradable hydrophobicity PVA resin composite materials particle
Bottle, obtain it is PVA bottle corresponding, bottle thickness be 0.2mm.
Carry out corresponding performance test, the results showed that, 75~100 DEG C of the water solution temperature of gained PVA film, tensile strength >
48Mpa, elongation at break 119%, oxygen transmission rate < 30cm3/m2* 24H*0.1Mpa, film surface water absorption rate 18.3%, material melt
Melting temperature is 150 DEG C~250 DEG C, and 266 DEG C of initial pyrolyzation temperature, thermal decomposition temperature reaches 318 DEG C or more.
Embodiment 9
Biodegradable hydrophobicity PVA resin composite materials in the present embodiment include the parts by weight of following component:
PVA:72, and the degree of polymerization of PVA is 600, and the alcoholysis degree of PVA is 88%；Lauryl hydroxyl sulfo betaine:
2.0；17 fluorine decyl trimethyl oxysilane: 2.0；1- vinyl -3- ethyl imidazol(e) borate: 1.0；1- butyl -3- methyl
Imidazoles tetraborate: 1.0；Plasticizer: 15；Inorganic material: 8.0；Antioxidant 1010: 1.0, antioxidant 330: 0.5；Stearic acid
Zinc: 1.0, methyl methacrylate: 0.5.
Wherein, above-mentioned plasticizer is glycerine, an acetoglyceride, two triacetins from ester, triacetyl glycerine and gathers
The composite elasticizer of ethylene glycol (molecular weight 10000) mixing and formation, and glycerine: an acetoglyceride: two triacetins are certainly
Ester: triacetyl glycerine: the weight ratio of polyethylene glycol is 4.0:1.5:1.5:1.5:2.5；
Above-mentioned inorganic material is using corresponding inorganic material, i.e. rutile titania stone-type titanium dioxide, rutile-type two in embodiment 1
The mixture of titanium oxide and talcum powder.
That the preparation method is the same as that of Example 1 is consistent for above-mentioned biodegradable hydrophobicity PVA resin composite materials specific, here not
It repeats again, is further put into inflation film manufacturing machine and blown using the biodegradable hydrophobicity PVA resin composite materials particle
Film obtains corresponding film, film thickness 0.08mm.
Carry out corresponding performance test, the results showed that, 75~100 DEG C of the water solution temperature of gained PVA film, tensile strength >
32Mpa, elongation at break 112%, oxygen transmission rate < 32cm3/m2* 24H*0.1Mpa, film surface water absorption rate 21.3%, material melt
Melting temperature is 140 DEG C~250 DEG C ranges, and 256 DEG C of initial pyrolyzation temperature, thermal decomposition temperature reaches 300 DEG C or more.
Embodiment 10
Biodegradable hydrophobicity PVA resin composite materials in the present embodiment include the parts by weight of following component:
PVA:68, and the degree of polymerization of PVA is 2600, and the alcoholysis degree of PVA is 99.9%；Lauryl weight ratio beet
Alkali: 1.0；17 fluorine decyl trimethyl oxysilane: 1.0；1- butyl -3- methylimidazole villaumite: 2.0；Plasticizer: 15；It is inorganic
Material: 30；Antioxidant 300: 1.0, irgasfos 168: 1.5；Zinc stearate: 1.0, oleamide: 0.5, starch: 60.
Wherein, above-mentioned plasticizer is the compound plasticising of ethylene glycol, polyethylene glycol, glycerol and Natrulon H-10 mixing and formation
Agent, and ethylene glycol: polyethylene glycol: glycerol: the weight ratio of Natrulon H-10 is 3.0:2.0:1.5:1.5.
Above-mentioned inorganic material is the mixing of rutile titanium dioxide, anatase titanium dioxide, talcum powder and silica
Object, and weight ratio is 1.0:1.2:1.5:2.0.
That the preparation method is the same as that of Example 1 is consistent for above-mentioned biodegradable hydrophobicity PVA resin composite materials specific, here not
It repeats again, is further put into inflation film manufacturing machine and blown using the biodegradable hydrophobicity PVA resin composite materials particle
Film obtains corresponding film, film thickness 0.08mm.
Carry out corresponding performance test, the results showed that, 75~100 DEG C of the water solution temperature of gained PVA film, tensile strength >
35Mpa, elongation at break 118%, oxygen transmission rate < 31cm3/m2* 24H*0.1Mpa, film surface water absorption rate 23.1%, material melt
Melting temperature is 140 DEG C~250 DEG C ranges, and 269 DEG C of initial pyrolyzation temperature, thermal decomposition temperature reaches 300 DEG C or more.
Specific embodiment described in the present invention only illustrate the spirit of the present invention by way of example.The neck of technology belonging to the present invention
The technical staff in domain can make various modifications or additions to the described embodiments or replace by a similar method
In generation, however, it does not deviate from the spirit of the invention or beyond the scope of the appended claims.
It is skilled to this field although present invention has been described in detail and some specific embodiments have been cited
For technical staff, as long as it is obvious for can making various changes or correct without departing from the spirit and scope of the present invention.
Claims (10)
1. a kind of biodegradable hydrophobicity PVA resin composite materials, which is characterized in that the composite material includes following component
Parts by weight:
PVA:60~80；Hydroxyl sulfo group class degradation of promoter: 1.0~5.0；Fluorine-containing hydrophobic modifier: 0.5~5.0；PVA decomposes suppression
Preparation: 0.5~5.0；Plasticizer: 10~40；Inorganic material: 1.0~30；Antioxidant: 0.5~5.0；Processing aid: 0.1~
5.0；Starch: 0~60.
2. biodegradable hydrophobicity PVA resin composite materials according to claim 1, which is characterized in that the hydroxyl sulfo group
Class degradation of promoter is selected from lauryl hydroxyl sulfo betaine, dodecyl hydroxyl sulfo betaine and cocoyl weight ratio sweet tea
One or more of dish alkali.
3. biodegradable hydrophobicity PVA resin composite materials according to claim 1, which is characterized in that described fluorine-containing thin
Water modifying agent is selected from 17 fluorine decyl trimethyl oxysilane, fluorine-containing 13 oxygroup triethoxysilane, three ethoxy of perfluoro capryl
One or more of base silane and trifluoroacetic anhydride.
4. biodegradable hydrophobicity PVA resin composite materials according to claim 1, which is characterized in that the PVA is decomposed
Inhibitor is selected from 1- butyl -3- methylimidazole tetraborate, 1- butyl -3- methylimidazole villaumite and 1- vinyl -3- ethyl miaow
One or more of azoles borate.
5. biodegradable hydrophobicity PVA resin composite materials described in -4 any one according to claim 1, which is characterized in that
The plasticizer is selected from polyalcohols material.
6. biodegradable hydrophobicity PVA resin composite materials according to claim 5, which is characterized in that the polyalcohol
Class material is selected from ethylene glycol, polyethylene glycol, glycerol, polyglycereol, propylene glycol, polypropylene glycol, a glycol, diethylene glycol (DEG), triethylene glycol, vinegar
One or more of acid anhydrides glyceride, two acetoglycerides and triacetyl glycerine.
7. biodegradable hydrophobicity PVA resin composite materials described in -4 any one according to claim 1, which is characterized in that
The inorganic material is selected from rutile titanium dioxide, anatase titanium dioxide, talcum powder, calcium carbonate, silica and hydrogen-oxygen
Change one or more of magnesium.
8. biodegradable hydrophobicity PVA resin composite materials described in -4 any one according to claim 1, which is characterized in that
The processing aid be selected from one of zinc stearate, calcium stearate, magnesium stearate, oleamide and methyl methacrylate or
It is several.
9. biodegradable hydrophobicity PVA resin composite materials described in -4 any one according to claim 1, which is characterized in that
The antioxidant is selected from antioxidant 1010, irgasfos 168, antioxidant 300, antioxidant 330, antioxidant triphenyl phosphite and Asia
One or more of trinonyl phosphate.
10. biodegradable hydrophobicity PVA resin composite materials described in -4 any one according to claim 1, which is characterized in that
The degree of polymerization of the PVA is 600~2600；The alcoholysis degree of the PVA is 88%~99.9%.
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| US20220002518A1 (en) * | 2020-07-06 | 2022-01-06 | Aquapak Polymers Limited | Process and apparatus for manufacture of processable polyvinyl alcohol |
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| CN112194869A (en) * | 2020-08-17 | 2021-01-08 | 福建师范大学泉港石化研究院 | Special PVA material capable of being thermoplastically processed and preparation method thereof |
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