CN105173383B - Polycaprolactone MULTILAYER COMPOSITE degradable packaging film - Google Patents
Polycaprolactone MULTILAYER COMPOSITE degradable packaging film Download PDFInfo
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- CN105173383B CN105173383B CN201510484442.2A CN201510484442A CN105173383B CN 105173383 B CN105173383 B CN 105173383B CN 201510484442 A CN201510484442 A CN 201510484442A CN 105173383 B CN105173383 B CN 105173383B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W90/00—Enabling technologies or technologies with a potential or indirect contribution to greenhouse gas [GHG] emissions mitigation
- Y02W90/10—Bio-packaging, e.g. packing containers made from renewable resources or bio-plastics
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Abstract
The present invention relates to degradation material technical field and packing technique fields.The present invention provides a kind of polycaprolactone MULTILAYER COMPOSITE degradable packaging film, the packaging film is made of four layers or four layers or more resin layers, its structure includes the outer layer containing biodegradable component, and the internal layer including biodegradable component being covered on one of outer layer；Any one resin layer of the packaging film is the blend of single polycaprolactone material or polycaprolactone and the different proportion of other resin materials；And each resin layer of the packaging film is from the center to outer layer, polycaprolactone content with gradient profile incremental variations, also successively decreased variation with gradient profile by melting temperature.Packaging film of the present invention has good heat resistance, thermal contraction performance, flexibility and mechanical property using a kind of completely new structure and mode, can be widely applied to packaging field.
Description
Technical field
The present invention relates to degradation material technical field and packing technique field, more particularly to it is a kind of by four layers or four layers with
The polycaprolactone biodegradable package film of upper resin layer composition.
Background technique
Under the big situation that environmental problem is serious, petroleum resources are short, biodegradable plastic has obtained extensive concern.Its
In, polycaprolactone is one of the hot topic of research and development.The raw material of polycaprolactone industry is can be degraded with regenerated biomaterial
Final product be also all water and carbon dioxide, can with complete biodegradable, be most competitive Biodegradable material it
One.
The film product of polycaprolactone and copolymerization product has broad application prospects in packaging field.However, oneself will be gathered
Interior ester film is applied to packaging field, and there is also many technical problems.For example, the ester bond of polycaprolactone and unstable,
In processing and forming, it is easy to happen thermal decomposition or ester exchange reaction.The product of polycaprolactone one-component because its performance limitation,
It can no longer meet the particular/special requirement of use, processing performance and appearance of product etc..Traditional application method is by polycaprolactone
Binary blend is formed with other monomers, wherein the content of polycaprolactone is 10~90%, and polyester forms continuous phase or co-continuous
Phase, but the tear resistance for the blend produced in this way is very poor.The monofilm of polycaprolactone polyol composition is usually non-
It is often crisp, lack flexibility, erosion-resisting characteristics and thermal stability also need to improve.
Seek polycaprolactone is compound with other materials, and by designing reasonable its flexibility of process improving, mechanical property
The factors such as energy, are polycaprolactone membranes in the only way that packaging field is further exploited market.Japanese Patent Laid-Open number
2004-109000 describes a kind of polyester and glass transition temperature (Tg) it is 0 DEG C or the multilayer of lower group aliphatic resin composition
Film, however these film heat resistances are poor, cause percent thermal shrinkage obviously high.
It can be seen that there is also above-mentioned multiple technologies problems for current polycaprolactone degradable packaging film.And the present invention mentions
A kind of polycaprolactone MULTILAYER COMPOSITE degradable packaging film is supplied, which is answered by polycaprolactone and other different resins
It closes, change of gradient is presented in every layer of melting temperature, improves adhesive property between layers, there is excellent flexibility,
And stable mechanical property, it is highly suitable for the use of packaging field.
Summary of the invention
In view of the above technical problems existing in the prior art, the present invention provides a kind of polycaprolactone MULTILAYER COMPOSITE is degradable
Packaging film, which has good degradable characteristic, while can satisfy packaging material again to heat resistance, mechanics
The requirement of performance, processing performance and appearance.The technical solution adopted by the present invention is as described below.
The present invention provides a kind of structures and performance to stablize, and the degradable packet of polycaprolactone MULTILAYER COMPOSITE with flexibility
Film is filled, the polycaprolactone MULTILAYER COMPOSITE degradable packaging film is made of four layers or four layers or more resin layers, as shown in Figure 1.
Including:
(1) include biodegradable component outer layer；With
(2) internal layer including biodegradable component being covered on one of outer layer.
" internal layer " means that two main surface in a kind of multilayered structure is all directly adhered to another layer of the structure
On any layer." outer layer ", which is meant in a kind of multilayered structure, to be had and only one surface adhesion is into the structure on another layer
Any layer.
Any one resin layer of the packaging film is single polycaprolactone material or polycaprolactone and other resin materials
The blend of different proportion；And each resin layer of the packaging film, from the center to outer layer, polycaprolactone content is with gradient profile
Incremental variations, melting temperature are also successively decreased variation with gradient profile.
Further, in polycaprolactone MULTILAYER COMPOSITE degradable packaging film of the present invention, outside the first outer layer and second
Layer contains the polycaprolactone within the scope of 70~95 weight %, preferably 80~90 weight %.The internal layer contains 10~
Polycaprolactone within the scope of 90 weight %, preferably 25~75 weight %.
The degradable packaging film that the present invention states, the component of polycaprolactone is changed with gradient profile in each resin layer, so that respectively
The melting temperature of layer is also changed with gradient profile, reduces the molding temperature difference between layers, in this way when material squeezes out, with temperature
Gradient and stress gradient form transition are spent, the technique requirement of co-extrusion modling processing is met.
In polycaprolactone MULTILAYER COMPOSITE degradable packaging film of the present invention, the overall weight percentage of each component is such as
Under:
The antioxidant can be triphenyl phosphite, phosphorous acetoacetic ester, cetyl pentaerythritol diphosphites
One of it is a variety of；The lubricant is hard amide, zinc stearate, any one in ethylenebisstearamide.
Polycaprolactone MULTILAYER COMPOSITE degradable packaging film of the present invention only passes through the amount for changing different function additive
Or property of the ratio to change each layer and the effect in whole laminated film, such as plasticizer can be added in each internal layer
The amount of tributyl citrate reduces the glass transition temperature of polycaprolactone, increases the flexibility of whole laminated film.
The thickness of polycaprolactone MULTILAYER COMPOSITE degradable packaging film of the present invention is in the range of 50~250 microns.
Any of them two layers of thickness ratio is in the range of 1:1 to 25:1, preferably 4:1 to 7:1.To include fully biodegradable component
An outer layer be reference, when any one layer too thick relative to lower a layer thickness, it will occur crystallinity difference and mechanical property not
Stable phenomenon, and it is any one layer too thick relative to upper a layer thickness when, the heat adhesive strength of the film will be difficult to reach work
Skill requirement.In actual process, weigh hopper real-time monitoring discharge quantity, feedback control extruder extrusion output, to each layer can be passed through
Thickness proportion is controlled.
The invention has the following beneficial effects: 1, during the preparation process reduce between layers due to melting temperature difference
And the molding temperature difference generated, the work for meeting Coextrusion Blow Moulding processing is gradually transitted to using temperature and stress gradient form
Skill requirement, makes composite material have good heat resistance and thermal contraction performance；2, it is mentioned to prepare polycaprolactone multi-layer compound film
A kind of completely new structure and mode are supplied；3 final product toughness are higher, have good flexibility and mechanical property, can be extensive
Applied to packaging field.
Detailed description of the invention
In order to will become apparent to the following present invention, below in the description of embodiment, embodiment and reference will be passed through
The mode that attached drawing combines is described, in which:
Fig. 1 is the polycaprolactone MULTILAYER COMPOSITE degradable packaging film schematic diagram；
Fig. 2 is four layers of composite degradable packaging film schematic diagram of polycaprolactone；
Fig. 3 is five layers of composite degradable packaging film schematic diagram of polycaprolactone；
Fig. 4 is six layers of composite degradable packaging film schematic diagram of polycaprolactone.
Wherein, 1 is the first outer layer, and 2 be the second outer layer, and 3 be internal layer a, and 4 be internal layer b, and 5 be internal layer c, and 6 be internal layer d.
Specific embodiment:
It can further illustrate that the present invention, embodiment are in order to illustrate being not intended to limit the present invention by the following example.
Any those of ordinary skill of this field can understand that these embodiments are not limit the invention in any way, and can do to it
Modification appropriate without prejudice to essence of the invention and deviates the scope of the present invention with data transformation.Table one is each embodiment product
Mechanical property comparative situation.
Embodiment 1
Polycaprolactone MULTILAYER COMPOSITE degradable packaging film described in the present embodiment, as shown in Fig. 2, by four layers of resin layer group
At structure includes the first outer layer 1 and the second outer layer 2 containing biodegradable component, and is covered on one of outer layer
Internal layer a3 and internal layer b4 including biodegradable component.The internal layer is that two main surface is all direct in a kind of multilayered structure
Adhere to any layer on another layer of the structure, the outer layer is to have in a kind of multilayered structure and only one surface adhesion arrives
Any layer in the structure on another layer.
Any one resin layer of the packaging film is single polycaprolactone material or polycaprolactone and other resin materials
The blend of different proportion；And each resin layer of the packaging film, from the center to outer layer, polycaprolactone content is with gradient profile
Incremental variations, melting temperature are also successively decreased variation with gradient profile.Specific preparation method is as described below.
It is the polycaprolactone containing 70 weight %, the poly- valerolactone of 4 weight %, 14 weights by 1 masterbatch component of the first outer layer
The tris phosphite of the tributyl citrate, 12 weight % of measuring % puts into double screw extruder.It is by 2 masterbatch component of the second outer layer
Polycaprolactone containing 70 weight %, the poly- valerolactone of 4 weight %, the tributyl citrate of 14 weight %, 12 weight % Asia
Phosphotriester puts into double screw extruder.It is the polycaprolactone containing 10 weight %, 35 weight % by internal layer a3 masterbatch component
Poly- valerolactone, the tributyl citrate of 15 weight %, the polytrimethylene carbonate of 20 weight %, 20 weight % phosphorous acid three
Ester puts into double screw extruder.By internal layer b4 masterbatch component be the polycaprolactone containing 10 weight %, 35 weight % poly- penta in
Ester, the tributyl citrate of 15 weight %, the polytrimethylene carbonate of 20 weight %, the tris phosphite investment of 20 weight %
Double screw extruder.Each master batch converges masterbatch in the cylinder by the concetrated pipe of extrusion die, in the item of streamline flow
Together by die head under part, wherein die head size can be adjusted according to film thickness needs.By up- coiler obtain with a thickness of
50 microns of film.It obtains product properties and is shown in Table 1, show that the polycaprolactone MULTILAYER COMPOSITE degradable package film properties meet one
As packaging material requirement.
The expression formula of the composite package film are as follows: the first outer layer/internal layer a/ internal layer the second outer layer of b/.
Embodiment 2
Polycaprolactone MULTILAYER COMPOSITE degradable packaging film prepared by the present embodiment, as shown in figure 3, by five layers of resin layer group
At structure includes the first outer layer 1 and the second outer layer 2 containing biodegradable component, and is covered on one of outer layer
Three internal layers including biodegradable component, i.e. internal layer a3, internal layer b4 and internal layer c5.
Any one resin layer of the packaging film is single polycaprolactone material or polycaprolactone and other resin materials
The blend of different proportion；And each resin layer of the packaging film, from the center to outer layer, polycaprolactone content is with gradient profile
Incremental variations, melting temperature are also successively decreased variation with gradient profile.
It is the polycaprolactone containing 80 weight %, the poly- valerolactone of 12 weight %, 7 weights by 1 masterbatch component of the first outer layer
The tris phosphite of the tributyl citrate, 1 weight % of measuring % puts into double screw extruder.It is by 2 masterbatch component of the second outer layer
Polycaprolactone containing 80 weight %, the poly- valerolactone of 12 weight %, the tributyl citrate of 7 weight %, the phosphorous of 1 weight %
Sour three esters put into double screw extruder.By internal layer a3 masterbatch component be the polycaprolactone containing 50 weight %, 12 weight % it is poly-
Valerolactone, the tributyl citrate of 15 weight %, the polytrimethylene carbonate of 22 weight %, 1 weight % tris phosphite
Put into double screw extruder.It is the oligomerization of the polycaprolactone containing 25 weight %, 17 weight % in oneself by internal layer b4 masterbatch component
Ester, the tributyl citrate of 20 weight %, caprolactone-ethanol copolymer of 37 weight %, 1 weight % tris phosphite
Put into double screw extruder.By internal layer c5 masterbatch component be the polycaprolactone containing 65 weight %, 17 weight % poly- valerolactone,
The tributyl citrate of 15 weight %, the polytrimethylene carbonate of 2 weight %, 1 weight % tris phosphite put into double spiral shells
Bar extruder.Each master batch converges masterbatch in the cylinder by the concetrated pipe of extrusion die, under conditions of streamline flow
Together by die head, wherein die head size can be adjusted according to film thickness needs.It is obtained by up- coiler micro- with a thickness of 150
The film of rice.It obtains product properties and is shown in Table 1, show that the polycaprolactone MULTILAYER COMPOSITE degradable package film properties meet general packet
Package material requirement.
The expression formula of the composite package film are as follows: the first outer layer/internal layer a/ internal layer b/ internal layer the second outer layer of c/.
Embodiment 3
Polycaprolactone MULTILAYER COMPOSITE degradable packaging film prepared by the present embodiment, as shown in figure 4, by six layers of resin layer group
At structure includes the first outer layer 1 and the second outer layer 2 containing biodegradable component, and is covered on one of outer layer
Four internal layers including biodegradable component, i.e. internal layer a3, internal layer b4, internal layer c5 and internal layer d6.
Any one resin layer of the packaging film is single polycaprolactone material or polycaprolactone and other resin materials
The blend of different proportion；And each resin layer of the packaging film, from the center to outer layer, polycaprolactone content is with gradient profile
Incremental variations, melting temperature are also successively decreased variation with gradient profile.
It is the polycaprolactone containing 95 weight %, the poly- valerolactone of 1 weight %, 2 weight % by 1 masterbatch component of the first outer layer
Tributyl citrate, 2 weight % tris phosphite put into double screw extruder.Second outer layer, 2 masterbatch component is contained
The polycaprolactone of 95 weight %, the poly- valerolactone of 1 weight %, the tributyl citrate of 2 weight %, 2 weight % phosphorous acid three
Ester puts into double screw extruder.By internal layer a3 masterbatch component be the polycaprolactone containing 90 weight %, 1 weight % poly- penta in
Ester, the tributyl citrate of 1 weight %, the polytrimethylene carbonate of 2 weight %, the tris phosphite investment of 6 weight % are double
Screw extruder.It is the polycaprolactone containing 88 weight %, the poly- valerolactone of 1 weight %, 3 weight % by internal layer b4 masterbatch component
Tributyl citrate, the polytrimethylene carbonate of 2 weight %, 6 weight % tris phosphite put into double screw extruder.
It is the citric acid three of the polycaprolactone containing 86 weight %, the poly- valerolactone of 1 weight %, 5 weight % by internal layer c5 masterbatch component
Butyl ester, the polytrimethylene carbonate of 2 weight %, 6 weight % tris phosphite put into double screw extruder.Internal layer d6 is female
Expect that component is the polycaprolactone containing 86 weight %, the poly- valerolactone of 1 weight %, the tributyl citrate of 5 weight %, 2 weights
The tris phosphite of the polytrimethylene carbonate, 6 weight % of measuring % puts into double screw extruder.Each master batch is passing through extrusion die
Converge masterbatch in the cylinder of the concetrated pipe of head, together by die head under conditions of streamline flow, wherein die head size can
It is adjusted with being needed according to film thickness.The film with a thickness of 250 microns is obtained by up- coiler.It obtains product properties and is shown in Table 1,
Show that the polycaprolactone MULTILAYER COMPOSITE degradable package film properties meet general packaging material requirement.
The expression formula of the composite package film are as follows: the first outer layer/internal layer a/ internal layer b/ internal layer c/ internal layer the second outer layer of d/.
The performance of one polycaprolactone MULTILAYER COMPOSITE degradable packaging film of table
Claims (3)
1. a kind of polycaprolactone MULTILAYER COMPOSITE degradable packaging film, which is characterized in that the packaging film is by four layers or four layers or more
Resin layer composition, structure includes the outer layer containing biodegradable component, and being covered on one of outer layer includes that can give birth to
The internal layer of object degradable component；The internal layer is that two main surface is all directly adhered to the multilayered structure in a kind of multilayered structure
Any layer on other layers, the outer layer be a kind of multilayered structure in have and only one surface adhesion into the multilayered structure its
Any layer on his layer；Any one resin layer of the packaging film is single polycaprolactone material or polycaprolactone and other resins
The blend of the different proportion of material；And each resin layer of the packaging film, from the center to outer layer, polycaprolactone content is with ladder
Degree form incremental variations, melting temperature are also successively decreased variation with gradient profile；The outer layer contains in 80~90 weight % ranges
Interior polycaprolactone, the internal layer contain the polycaprolactone within the scope of 25~75 weight %；The packaging film with a thickness of
50~250 microns；Any two layers of thickness ratio of the packaging film is 4:1~7:1.
2. degradable packaging film according to claim 1, which is characterized in that the group subpackage of each resin layer of the packaging film
Include polycaprolactone, caprolactone-ethanol copolymer, Caprolactone oligomers, poly- valerolactone, tris phosphite, poly- tetramethyl oneself two
It is de- that acyl is total to terephthalate, polytetramethylene glycol-adipic acid-terephthalic acid (TPA), polytrimethylene carbonate, tributyl citrate, illiteracy
Soil, antioxidant and lubricant.
3. degradable packaging film according to claim 2, which is characterized in that the antioxidant be triphenyl phosphite,
One of phosphorous acetoacetic ester, cetyl pentaerythritol diphosphites are a variety of；The lubricant is hard amide, tristearin
Any one in sour zinc, ethylenebisstearamide.
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| CN201510484442.2A CN105173383B (en) | 2015-08-07 | 2015-08-07 | Polycaprolactone MULTILAYER COMPOSITE degradable packaging film |
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| CN201510484442.2A CN105173383B (en) | 2015-08-07 | 2015-08-07 | Polycaprolactone MULTILAYER COMPOSITE degradable packaging film |
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| CN105173383B true CN105173383B (en) | 2019-02-12 |
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| CN108017888A (en) * | 2017-12-02 | 2018-05-11 | 无锡福尔顺科技有限公司 | One kind sealing polycaprolactone pack case and its application |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201026690Y (en) * | 2007-01-17 | 2008-02-27 | 广东德冠包装材料有限公司 | Paper or plastic complex photodegradation biaxial tension polypropylene film without glue |
| EP2144221A1 (en) * | 2008-07-08 | 2010-01-13 | LG Chem, Ltd. | Biodegradable film for advertisement |
| CN102407644A (en) * | 2011-07-22 | 2012-04-11 | 蚌埠蓝天塑料包装有限公司 | Biodegradable multilayer composite polyethylene film and preparation method thereof |
| CN102858649A (en) * | 2010-03-12 | 2013-01-02 | 斯塔诺阿埃索澳吉有限公司 | Heat-sealable biodegradable packaging material, a method for its manufacture, and a product package made from the material |
-
2015
- 2015-08-07 CN CN201510484442.2A patent/CN105173383B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201026690Y (en) * | 2007-01-17 | 2008-02-27 | 广东德冠包装材料有限公司 | Paper or plastic complex photodegradation biaxial tension polypropylene film without glue |
| EP2144221A1 (en) * | 2008-07-08 | 2010-01-13 | LG Chem, Ltd. | Biodegradable film for advertisement |
| CN102858649A (en) * | 2010-03-12 | 2013-01-02 | 斯塔诺阿埃索澳吉有限公司 | Heat-sealable biodegradable packaging material, a method for its manufacture, and a product package made from the material |
| CN102407644A (en) * | 2011-07-22 | 2012-04-11 | 蚌埠蓝天塑料包装有限公司 | Biodegradable multilayer composite polyethylene film and preparation method thereof |
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Effective date of registration: 20210926 Address after: No.36 Shuanggao Road, economic development zone, Gaochun District, Nanjing, Jiangsu Province Patentee after: Nanjing Guoxing Biotechnology Research Institute Co.,Ltd. Address before: No. 18, Fangshui East Road, chemical industry park, Liuhe District, Nanjing, Jiangsu 210047 Patentee before: JIANGSU HONGTAIYANG NEW MATERIAL Co.,Ltd. |