CN107418026A - Composite barrier material and preparation method thereof - Google Patents
Composite barrier material and preparation method thereof Download PDFInfo
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/06—Polyethene
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2323/04—Homopolymers or copolymers of ethene
- C08J2323/06—Polyethene
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2423/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
- C08J2423/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
- C08J2423/04—Homopolymers or copolymers of ethene
- C08J2423/08—Copolymers of ethene
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- C—CHEMISTRY; METALLURGY
- 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
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C—CHEMISTRY; METALLURGY
- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/14—Gas barrier composition
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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
- 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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/062—HDPE
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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
- C08L2207/00—Properties characterising the ingredient of the composition
- C08L2207/06—Properties of polyethylene
- C08L2207/066—LDPE (radical process)
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- Chemical Kinetics & Catalysis (AREA)
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- Polymers & Plastics (AREA)
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Abstract
The application provides a kind of preparation method of composite barrier material, comprises the following steps：After barrier resins, compatilizer, melaminecyanurate, phyllosilicate, coupling agent and lubricant are mixed, melting mixing extruding pelletization, pre- dispensing is obtained；After above-mentioned pre- dispensing, base resin and auxiliary agent are mixed, melting mixing extruding pelletization, composite barrier material is obtained.The preparation method of above-mentioned composite barrier material, there is the characteristics of sclay texture using melaminecyanurate, it is advantageously implemented the stratiform alloying of base resin and barrier resins, can an extrusion molding, equipment and technology is greatly simplified, and it is compound with phyllosilicate, the performance complement of each component material can be reached, while the composite barrier material for making to prepare has high obstructing performance, mechanical property and processing characteristics are also fine.
Description
Technical field
The present invention relates to separated packaging material field, more particularly to a kind of composite barrier material and preparation method thereof.
Background technology
The problems such as small molecule transmitance is high, such as oxygen, vapor, odourant molecules mostly be present in common plastic material packing material
Transmitance it is high, bring great harm to overwhelming majority packaging occasions.And the appearance of separated packaging material, solve above-mentioned ask
Topic.
Traditional separated packaging material is mainly one pack system barrier material, such as polyvinylidene chloride, ethylene-vinyl alcohol are common
Polymers, polyvinyl alcohol, polyester, cyano resin and polyamide etc..Problems with mostly be present in these one pack system barrier materials：（1）
The good poor processability of barrier property；（2）The good barrier property of processing characteristics is poor；（3）Barrier property is good, prepares extremely tired
It is difficult.
In order to solve the above problems, people do a lot of work, and mainly have following three aspects：（1）Improved equipment, use
It is multi-layer co-extruded to solve the problems, such as poor processability with MULTILAYER COMPOSITE, but technique and equipment are all more complicated；（2）Improve barrier material
Molecular structure solve the problems, such as barrier property difference, but cost is higher；（3）Solves barrier with metal or inorganic oxide plated film
The problem of poor performance, but complex process, cost are higher.
The content of the invention
Based on this, it is necessary to the problem of in background technology, there is provided a kind of technique is simple, processing characteristics is good and barrier
The preparation method of composite barrier material that can be good.
The application also provides a kind of composite barrier material prepared using above-mentioned preparation method.
A kind of preparation method of composite barrier material, comprises the following steps：
After barrier resins, compatilizer, melaminecyanurate, phyllosilicate, coupling agent and lubricant are mixed, melting
Extruding pelletization is mixed, obtains pre- dispensing；
After the pre- dispensing, base resin and auxiliary agent are mixed, melting mixing extruding pelletization, the composite barrier material is obtained.
In one of the embodiments, the mass ratio relation between each raw material is as follows：
5 ~ 30 parts of barrier resins；
3 ~ 15 parts of compatilizer；
2 ~ 15 parts of melaminecyanurate；
2 ~ 15 parts of phyllosilicate；
0.1 ~ 1 part of coupling agent；
0.2 ~ 1.5 part of lubricant；
20.5 ~ 87.2 parts of base resin；
0 ~ 2 part of auxiliary agent.
In one of the embodiments, the barrier resins are selected from polyamide, polyester, ethylene-vinyl alcohol copolymer, poly- inclined
At least one of dichloroethylene and cyano resin.
In one of the embodiments, the compatilizer is selected from maleic anhydride grafted polyethylene, acrylic ester grafted poly- second
Alkene, methacrylate grafted polyethylene, ethylene acrylic acid co polymer, ethylene acrylate copolymer, ethylene methacrylic acid
At least one of ester copolymer, ethylene vinyl acetate copolymer, thermoplastic polyurethane and polyacrylate.
In one of the embodiments, layered silicate is selected from the inorganic laminated silicate of clay system and clay system is organic
At least one of modified sheet silicate.
In one of the embodiments, the coupling agent is selected from organo silane coupling agent, titanate coupling agent and multi-functional
At least one of coupling agent.
In one of the embodiments, the lubricant is selected from higher fatty acids, high-grade aliphatic ester, higher fatty acids acyl
At least one of amine, advanced unsaturated acids acid amides and higher fatty acid salt.
In one of the embodiments, the base resin is polyethylene, and the polyethylene includes polyethylene from high pressure process, low pressure
At least one of polyethylene, linear low density polyethylene (LLDPE), medium density polyethylene and metallocene PE.
In one of the embodiments, the auxiliary agent is selected from least one of colouring agent and antioxidant.
A kind of composite barrier material prepared using above-mentioned preparation method.
The preparation method of above-mentioned composite barrier material, there is the spy of sclay texture using melaminecyanurate
Point, be advantageously implemented the stratiform alloying of base resin and barrier resins, can an extrusion molding, greatly simplify equipment and work
Skill, and it is compound with phyllosilicate, the performance complement of each component material can be reached, the composite barrier material for making to prepare has
While high obstructing performance, mechanical property is also fine with processing characteristics.
Embodiment
In order to facilitate the understanding of the purposes, features and advantages of the present invention, below to the specific reality of the present invention
The mode of applying is described in detail.Many details are elaborated in the following description in order to fully understand the present invention.But
The invention can be embodied in many other ways as described herein, and those skilled in the art can be without prejudice to this hair
Similar improvement is done in the case of bright intension, therefore the present invention is not limited to the specific embodiments disclosed below.
A kind of preparation method of composite barrier material, comprises the following steps：
S110, by barrier resins, compatilizer, melaminecyanurate, phyllosilicate, coupling agent and lubricant mix
Afterwards, melting mixing extruding pelletization, pre- dispensing is obtained.
Wherein, barrier resins are selected from polyamide, polyester, ethylene-vinyl alcohol copolymer（EVOH）, polyvinylidene chloride
（PVDC）And at least one of cyano resin.
Specifically, polyamide includes nylon 6（PA6）, nylon66 fiber（PA66）, NYLON610（PA610）, copolymer nylon 6/66
（PA6/66 copolymers）, at least one of MXD6 etc..
Polyester includes polyethylene terephthalate（PET）, polybutylene terephthalate (PBT)（PBT）, it is poly- to benzene two
Formic acid glycol ester -1,4 cyclohexane dimethanol ester（PETG）, PEN（PEN）At least one of Deng.
Cyano resin is the copolymer based on acrylonitrile.
Wherein, compatilizer is selected from maleic anhydride grafted polyethylene, acrylic ester grafted polyethylene, methacrylate grafting
Polyethylene, ethylene acrylic acid co polymer（EAA）, ethylene acrylate copolymer, ethylene methyl acrylate copolymer（EMA）、
At least one of ethylene vinyl acetate copolymer, thermoplastic polyurethane and polyacrylate.
Phyllosilicate in the inorganic laminated silicate of clay system and clay system organic modified sheet silicate at least
It is a kind of.
Wherein, the inorganic laminated silicate of clay system includes at least one of montmorillonite, bentonite, kaolin etc..It is preferred that
, the mesh of the fineness of phyllosilicate >=500.
Coupling agent is selected from least one of organo silane coupling agent, titanate coupling agent and multi-functional coupling agent.
Wherein, organo silane coupling agent includes the silane coupler containing amino（Such as aminopropyl silane coupling agent）, contain
The silane coupler of epoxy radicals（Such as γ-（Glycidol ether）Propyl trimethoxy silicane coupling agent）Or the silicon containing unsaturated group
Alkane coupling agent（Such as vinyl three（'beta '-methoxy ethyoxyl）It is silane, γ-propyl methacrylate base trimethoxy silane, suitable
Butylmaleimide base propyl-triethoxysilicane）At least one of Deng.
Titanate coupling agent includes the oleoyl epoxide titanate esters of isopropyl three, isopropyl two（Methylacryloyl）Isostearoyl
The different pungent phosphinylidyne epoxide titanate esters of base titanate esters, isopropyl dioleoyl epoxide two, isopropyl three（Dodecyl benzenesulfonyl）Metatitanic acid
Ester, isopropyl three（Dioctylphyrophosphoric acid ester）At least one of titanate esters etc..
Multi-functional coupling agent is multi-functional coupling agent disclosed in application number 2017101443072.Specifically, the multi-functional idol
It is steady by the organotin of the basic coupling agent of 56 ~ 95.5 mass parts, the multifunctional assistant of 3 ~ 30 mass parts, 0.5 ~ 3 mass parts to join agent
The defoamer compounding for determining synergist, the antioxidant of 0.5 ~ 5 mass parts, the lubricant of 0.5 ~ 5 mass parts and 0 ~ 1 mass parts forms.
Wherein, multifunctional assistant is formed by multi-functional compounds with the reaction of the compound containing basic coupling agent centerbody.
Lubricant is selected from higher fatty acids, high-grade aliphatic ester, higher fatty acid amides（Such as behenamide, ethylene
Bis-stearamides etc.）, advanced unsaturated acids acid amides（Such as oleamide, erucyl amide etc.）And in higher fatty acid salt at least
It is a kind of.
Specifically, barrier resins, compatilizer, melaminecyanurate, phyllosilicate, coupling agent and lubricant mix
After even, with high shear screw rod melting mixing extruding pelletization, pre- dispensing is obtained.
S120, after mixing above-mentioned pre- dispensing, base resin and auxiliary agent, melting mixing extruding pelletization, obtain compound barrier
Material.
Wherein, base resin is polyethylene.The polyethylene includes polyethylene from high pressure process（LDPE）, low-pressure polyethylene（HDPE）、
Linear low density polyethylene (LLDPE)（LLDPE）, medium density polyethylene（MDPE）And metallocene PE（Metallocene PE）In at least one
Kind.
Auxiliary agent is colouring agent or antioxidant.
It should be noted that above-mentioned auxiliary agent can also be other typical additives.
Mass ratio relation between above-mentioned each raw material is as follows：
5 ~ 30 parts of barrier resins；
3 ~ 15 parts of compatilizer；
2 ~ 15 parts of melaminecyanurate；
2 ~ 15 parts of phyllosilicate；
0.1 ~ 1 part of coupling agent；
0.2 ~ 1.5 part of lubricant；
20.5 ~ 87.2 parts of base resin；
0 ~ 2 part of auxiliary agent.
Preferably, the mass ratio relation between above-mentioned raw materials is as follows：
5 ~ 20 parts of barrier resins；
3 ~ 10 parts of compatilizer；
3 ~ 10 parts of melaminecyanurate；
3 ~ 10 parts of phyllosilicate；
0.3 ~ 0.6 part of coupling agent；
0.4 ~ 1.3 part of lubricant；
46.9 ~ 84.7 parts of base resin；
0.6 ~ 1.2 part of auxiliary agent.
Specifically, after above-mentioned pre- dispensing, base resin and auxiliary agent mix, with low sheraing screw rod melting mixing extruding pelletization,
Obtain composite barrier material.
The preparation method of above-mentioned composite barrier material, there is the spy of sclay texture using melaminecyanurate
Point, be advantageously implemented the stratiform alloying of base resin and barrier resins, can an extrusion molding, greatly simplify equipment and work
Skill, and it is compound with phyllosilicate, the performance complement of each component material can be reached, the composite barrier material for making to prepare has
While high obstructing performance, mechanical property is also fine with processing characteristics.
It is specific embodiment below.
Embodiment 1
By 16kg PA6/66 copolymers（PA6 segments 75%, PA66 segments 25%）, 10kg PETG, 16kg EVOH, 12kg Malaysias
Anhydride grafted lldpe（Grafting rate 1.1%）, 1kg EAA, 7kg EMA, 6kg melaminecyanurates, 8kg nanometers are covered de-
Soil, the multi-functional silane couplers of 0.4kg（The silane type prepared for the disclosed embodiment 2 of application number 2017101443072 is multi-functional
Coupling agent）, the multi-functional titanate coupling agents of 0.4kg（The metatitanic acid prepared for the disclosed embodiment 1 of application number 2017101443072
Ester type multi-functional coupling agent）After being mixed with 1.6kg erucyl amides, with high shear screw rod melting mixing extruding pelletization, obtain prewired
Material.
By the above-mentioned pre- dispensings of 58.8kg, 60kg HDPE, 15kg LDPE, 15kg LLDPE, 0.9kg titanium dioxides and 0.3kg
After antioxidant 1010 mixes, with low sheraing screw rod melting mixing extruding pelletization, composite barrier material is obtained.
It is 1.5 decimillimeters that composite barrier material prepared by embodiment 1 is blow molded into thickness, a diameter of 40cm cylindrical membrane.Take
The cylindrical membrane of 40cm length packs the dried nylon 6 of 5kg（Moisture content 0.12%）, deposit 6 months after Vacuum Package.
After testing, after depositing 6 months, the Nylon 6 Samples through the encapsulation of above-mentioned cylindrical membrane, moisture content 0.14%, Buddhist nun has been reached
The waterproof and dampproof requirement of the vacuum packaging of dragon 6.
Detected by the sample preparation of plastic tensile detection performance standard, above-mentioned cylindrical membrane tensile break strength is 35MPa, extension at break
Rate is 161%, is occurred before being broken exfoliated.
Embodiment 2
By 12kg PVDC, 30kg EVOH, 10kg butyl acrylate grafted polyethylenes（Grafting rate 0.7%）, 10kg EMA, 5kg
Melaminecyanurate, 9kg nano imvites, the multi-functional silane couplers of 0.4kg, 0.4kg isopropyl dioleoyl epoxides
After two different pungent phosphinylidyne epoxide titanate esters and 1.6kg oleamides mix, with high shear screw rod melting mixing extruding pelletization, obtain pre-
Dispensing.
By the above-mentioned pre- dispensings of 58.8kg, 60kg HDPE, 15kg LDPE, 15kg LLDPE, 0.9kg titanium dioxides and 0.3kg
After antioxidant 1010 mixes, with low sheraing screw rod melting mixing extruding pelletization, composite barrier material is obtained.
It is 1.5 decimillimeters that composite barrier material prepared by embodiment 2 is blow molded into thickness, a diameter of 40cm cylindrical membrane.Take
The cylindrical membrane of 40cm length packs the dried nylon 6 of 5kg（Moisture content 0.12%）, deposit 6 months after Vacuum Package.
After testing, after depositing 6 months, the Nylon 6 Samples through the encapsulation of above-mentioned cylindrical membrane, moisture content 0.13%, Buddhist nun has been reached
The waterproof and dampproof requirement of the vacuum packaging of dragon 6.
Detected by the sample preparation of plastic tensile detection performance standard, above-mentioned cylindrical membrane tensile break strength is 33.5MPa, and fracture is stretched
Long rate is 167%, is occurred before being broken exfoliated.
Embodiment described above only expresses the several embodiments of the present invention, and its description is more specific and detailed, but simultaneously
Therefore the limitation to the scope of the claims of the present invention can not be interpreted as.It should be pointed out that for one of ordinary skill in the art
For, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the guarantor of the present invention
Protect scope.Therefore, the protection domain of patent of the present invention should be determined by the appended claims.
Claims (10)
1. a kind of preparation method of composite barrier material, it is characterised in that comprise the following steps：
After barrier resins, compatilizer, melaminecyanurate, phyllosilicate, coupling agent and lubricant are mixed, melting
Extruding pelletization is mixed, obtains pre- dispensing；
After the pre- dispensing, base resin and auxiliary agent are mixed, melting mixing extruding pelletization, the composite barrier material is obtained.
2. the preparation method of composite barrier material according to claim 1, it is characterised in that the mass ratio between each raw material
Example relation is as follows：
5 ~ 30 parts of barrier resins；
3 ~ 15 parts of compatilizer；
2 ~ 15 parts of melaminecyanurate；
2 ~ 15 parts of phyllosilicate；
0.1 ~ 1 part of coupling agent；
0.2 ~ 1.5 part of lubricant；
20.5 ~ 87.2 parts of base resin；
0 ~ 2 part of auxiliary agent.
3. the preparation method of composite barrier material according to claim 1 or 2, it is characterised in that the barrier resins choosing
From at least one of polyamide, polyester, ethylene-vinyl alcohol copolymer, polyvinylidene chloride and cyano resin.
4. the preparation method of composite barrier material according to claim 1 or 2, it is characterised in that the compatilizer is selected from
Maleic anhydride grafted polyethylene, acrylic ester grafted polyethylene, methacrylate grafted polyethylene, ethylene-acrylic acid copolymer
Thing, ethylene acrylate copolymer, ethylene methyl acrylate copolymer, ethylene vinyl acetate copolymer, thermoplastic poly ammonia
At least one of ester and polyacrylate.
5. the preparation method of composite barrier material according to claim 1 or 2, it is characterised in that layered silicate
Selected from least one of the inorganic laminated silicate of clay system and clay system organic modified sheet silicate.
6. the preparation method of composite barrier material according to claim 1 or 2, it is characterised in that the coupling agent is selected from
At least one of organo silane coupling agent, titanate coupling agent and multi-functional coupling agent.
7. the preparation method of composite barrier material according to claim 1 or 2, it is characterised in that the lubricant is selected from
In higher fatty acids, high-grade aliphatic ester, higher fatty acid amides, advanced unsaturated acids acid amides and higher fatty acid salt at least
It is a kind of.
8. the preparation method of composite barrier material according to claim 1 or 2, it is characterised in that the base resin is
Polyethylene, the polyethylene include polyethylene from high pressure process, low-pressure polyethylene, linear low density polyethylene (LLDPE), medium density polyethylene and cyclopentadienyl
At least one of metal polyethylene.
9. the preparation method of composite barrier material according to claim 1 or 2, it is characterised in that the auxiliary agent is selected from
At least one of toner and antioxidant.
10. composite barrier material prepared by a kind of preparation method of composite barrier material using described in claim 1.
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