CN112677611B - High-transparency recyclable low-temperature-resistant sheet and preparation method thereof - Google Patents
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- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 238000001816 cooling Methods 0.000 claims abstract description 22
- 238000004132 cross linking Methods 0.000 claims abstract description 22
- 238000001125 extrusion Methods 0.000 claims abstract description 15
- 238000007493 shaping process Methods 0.000 claims abstract description 15
- 238000005096 rolling process Methods 0.000 claims abstract description 8
- 239000010410 layer Substances 0.000 claims description 55
- 239000000463 material Substances 0.000 claims description 35
- 239000000155 melt Substances 0.000 claims description 28
- 229920001526 metallocene linear low density polyethylene Polymers 0.000 claims description 17
- 229920001862 ultra low molecular weight polyethylene Polymers 0.000 claims description 17
- 229920000219 Ethylene vinyl alcohol Polymers 0.000 claims description 16
- UFRKOOWSQGXVKV-UHFFFAOYSA-N ethene;ethenol Chemical compound C=C.OC=C UFRKOOWSQGXVKV-UHFFFAOYSA-N 0.000 claims description 16
- 239000004715 ethylene vinyl alcohol Substances 0.000 claims description 16
- 239000002346 layers by function Substances 0.000 claims description 15
- 239000012790 adhesive layer Substances 0.000 claims description 13
- 239000012793 heat-sealing layer Substances 0.000 claims description 12
- 230000004888 barrier function Effects 0.000 claims description 10
- 238000012545 processing Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 2
- 239000002253 acid Substances 0.000 abstract description 2
- 239000003513 alkali Substances 0.000 abstract description 2
- 239000005416 organic matter Substances 0.000 abstract description 2
- 238000007789 sealing Methods 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 14
- 229920003023 plastic Polymers 0.000 description 5
- 239000004033 plastic Substances 0.000 description 5
- 230000032683 aging Effects 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 238000009448 modified atmosphere packaging Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000010408 film Substances 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 229910052760 oxygen Inorganic materials 0.000 description 2
- 239000001301 oxygen Substances 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 238000002834 transmittance Methods 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000013039 cover film Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention provides a high-transparency recyclable low-temperature-resistant sheet and a preparation method thereof. The thickness of the sheet is 300-600 um. The preparation method comprises the steps of batching, extrusion plasticizing, cooling shaping, crosslinking treatment, rolling and the like. The high-transparency recyclable low-temperature-resistant sheet provided by the invention. Good transparency, recoverability, good low temperature resistance, good heat sealing property and toughness at low temperature, and good acid, alkali and polar organic matter resistance.
Description
Technical field:
The invention relates to the technical field of low-temperature sheets, in particular to a high-transparency recyclable low-temperature-resistant sheet and a preparation method thereof.
The background technology is as follows:
the development of plastic packages brings convenience to human society life and production, and simultaneously, a large amount of waste plastic garbage is continuously generated. The waste plastics are difficult to degrade, the influence on the environment is more obvious, correct treatment is needed, and especially, the environmental protection treatment, the plastic limiting and the plastic reduction are actively carried out all over the world in recent years. Environmentally friendly, recyclable, degradable materials are increasingly favored by consumers.
In addition, the modified atmosphere packaging can prevent the quality of food from being reduced or slow down the quality reduction in physical, chemical, biological and other aspects, so that the shelf life of the food is prolonged, and the modified atmosphere packaging is a packaging form which is more and more popular in recent years. The modified atmosphere packaging is divided into a cover film and a bottom film, the bottom film of the current modified atmosphere packaging is low in general transparency, poor in low temperature resistance, good in display effect on contents, and incapable of meeting the preservation requirement of foods under the low temperature condition.
The invention comprises the following steps:
The invention aims at overcoming the defects of the prior art and provides a high-transparency recyclable low-temperature-resistant sheet and a preparation method thereof.
The technical scheme for realizing the aim of the invention is as follows: the utility model provides a high transparent recoverable low temperature resistant sheet is from outside to interior including structure heat seal layer, functional layer, filling layer, adhesive layer, barrier layer, adhesive layer, functional layer, structure heat seal layer and structure heat seal layer in proper order, the material of structure heat seal layer is MLLDPE, the material of functional layer is COC, the material of filling layer is ULDPE, the material of adhesive layer is the TIE, the material of barrier layer is EVOH. The thickness of the sheet is 300-600 um.
Preferably, the layer thickness ratio of each layer of the sheet from outside to inside is as follows: 10 to 15 percent, 8 to 15 percent, 10 to 15 percent, 7 to 10 percent, 2 to 5 percent, 7 to 10 percent, 10 to 15 percent, 7 to 13 percent and 7 to 13 percent.
Preferably, the density of the MLLDPE is 0.880-0.920 g/cm 3, and the melt index is 0.5-4 g/10min. The material is used as a structural heat seal layer, and good heat sealing property and toughness are kept at low temperature.
Preferably, the COC has a number average molecular weight of 14000-450000, a density of 0.950-1.450 g/cm 3, and a melt index of 3-6 g/10min. The material is used as a functional layer, has good water vapor and oxygen barrier property and excellent acid, alkali and polar organic matter resistance.
Preferably, the ULDPE has a density of 0.870-0.910 g/cm 3 and a melt index of 0.5-5 g/10min. The material is used as the filling layer, so that the toughness, the strength and the impact resistance of the film are greatly improved.
Preferably, the TIE has a density of 0.905 to 0.925g/cm 3 and a melt index of 3 to 4g/10min.
Preferably, the density of the EVOH is 1.17 to 1.21g/cm 3. The material has good oxygen and fragrance resistance.
In addition, the application also provides a preparation method of the high-transparency recyclable low-temperature-resistant sheet, which comprises the following steps: the preparation method comprises the steps of batching, extrusion plasticizing, cooling shaping, crosslinking treatment and rolling, wherein the cooling temperature in the cooling shaping step is 2-10 ℃, and the crosslinking treatment dosage in the crosslinking treatment step is 200-250 KGy.
Preferably, in the extrusion plasticizing step, the processing temperatures of each material in the first temperature zone, the second temperature zone, the third temperature zone, the fourth temperature zone and the die head in the extruder are respectively as follows:
MLLDPE:160-180℃、180-200℃、190-210℃、195-210℃、225-240℃
ULDPE:150-165℃、160-175℃、165-170℃、170-185℃、225-240℃
COC:170-190℃、190-210℃、195-215℃、200-220℃、225-240℃
TIE:190-210℃、210-230℃、215-235℃、215-235℃、225-240℃
EVOH:180-220℃、200-220℃、210-225℃、220-230℃、225-240℃。
the high-transparency recyclable low-temperature-resistant sheet and the preparation method thereof have the beneficial effects that:
The invention provides a high-transparency recyclable low-temperature-resistant sheet, which sequentially comprises a structural heat sealing layer, a functional layer, a filling layer, an adhesive layer, a barrier layer, an adhesive layer, a functional layer, a structural heat sealing layer and a structural heat sealing layer from outside to inside.
Description of the drawings:
Fig. 1 is a schematic structural view of the present invention.
In the figure: 1a structural heat sealing layer, 2a functional layer, 3a filling layer, 4 an adhesive layer and 5 a barrier layer.
The specific embodiment is as follows:
The preferred embodiments of the present invention will be described in detail below with reference to the attached drawings so that the advantages and features of the present invention can be more easily understood by those skilled in the art, thereby making clear and defining the scope of the present invention.
Example 1
Referring to fig. 1, the high-transparency recyclable low-temperature-resistant sheet sequentially comprises a structural heat seal layer 1, a functional layer 2, a filling layer 3, an adhesive layer 4, a barrier layer 5, an adhesive layer 4, a functional layer 2, the structural heat seal layer 1 and the structural heat seal layer 1 from outside to inside. The heat sealing layer 1 is made of MLLDPE, the functional layer 2 is made of COC, the filling layer 3 is made of ULDPE, the bonding layer 4 is made of TIE, and the barrier layer 5 is made of EVOH.
The thickness of the sheet was 300um. And the layer thickness ratio of each layer of the sheet from outside to inside is as follows: 10%, 15%, 7%, 5%, 7%, 15%, 13%.
The MLLDPE has a density of 0.880g/cm 3 and a melt index of 0.5g/10min.
The number average molecular weight of the COC is 14000, the density is 0.950g/cm 3, and the melt index is 6g/10min.
The ULDPE had a density of 0.910g/cm 3 and a melt index of 5g/10min.
The TIE had a density of 0.925g/cm 3 and a melt index of 3g/10min.
The density of the EVOH was 1.21g/cm 3.
The application also provides a preparation method of the high-transparency recyclable low-temperature-resistant sheet, which comprises the following steps: the preparation method comprises the steps of batching, extrusion plasticizing, cooling shaping, crosslinking treatment and rolling, wherein the cooling temperature in the cooling shaping step is 2 ℃, and the crosslinking treatment dosage in the crosslinking treatment step is 250KGy.
In the extrusion plasticizing step, the processing temperatures of each material in a first temperature zone, a second temperature zone, a third temperature zone, a fourth temperature zone and a die head in an extruder are respectively as follows:
MLLDPE:180℃、200℃、210℃、210℃、240℃
ULDPE:150℃、160℃、165℃、170℃、240℃
COC:170℃、190℃、195℃、200℃、240℃
TIE:210℃、230℃、235℃、235℃、240℃
EVOH:180℃、200℃、210℃、220℃、240℃。
Example 2
In this embodiment, the thickness of the sheet is 400um.
The layer thickness ratio of each layer of the sheet from outside to inside is as follows: 15%, 10%, 5%, 10%, 15%, 10%.
The MLLDPE has a density of 0.890g/cm 3 and a melt index of 3g/10min.
The COC has a number average molecular weight of 25000, a density of 1.30g/cm 3 and a melt index of 4g/10min.
The ULDPE had a density of 0.880g/cm 3 and a melt index of 3g/10min.
The TIE had a density of 0.910g/cm 3 and a melt index of 3g/10min.
The density of the EVOH was 1.150g/cm 3.
The application also provides a preparation method of the high-transparency recyclable low-temperature-resistant sheet, which comprises the following steps: the preparation method comprises the steps of batching, extrusion plasticizing, cooling shaping, crosslinking treatment and rolling, wherein the cooling temperature in the cooling shaping step is 6 ℃, and the crosslinking treatment dosage in the crosslinking treatment step is 220KGy.
In the extrusion plasticizing step, the processing temperatures of each material in a first temperature zone, a second temperature zone, a third temperature zone, a fourth temperature zone and a die head in an extruder are respectively as follows:
MLLDPE：170℃、190℃、200℃、205℃、235℃
ULDPE：160℃、170℃、170℃、180℃、235℃
COC：180℃、200℃、205℃、210℃、235℃
TIE：200℃、220℃、225℃、225℃、235℃
EVOH：190℃、210℃、220℃、225℃、235℃
Other conditions were the same as in example 1.
Example 3
In this embodiment, the thickness of the sheet is 450um.
The layer thickness ratio of each layer of the sheet from outside to inside is as follows: 13%, 15%, 10%, 4%, 10%, 15%, 10%.
The MLLDPE has a density of 0.90g/cm 3 and a melt index of 3g/10min.
The COC has a number average molecular weight of 30000, a density of 1.250g/cm 3 and a melt index of 5g/10min.
The ULDPE had a density of 0.890g/cm 3 and a melt index of 3g/10min.
The TIE had a density of 0.920g/cm 3 and a melt index of 3g/10min.
The density of the EVOH was 1.20g/cm 3.
The application also provides a preparation method of the high-transparency recyclable low-temperature-resistant sheet, which comprises the following steps: the preparation method comprises the steps of batching, extrusion plasticizing, cooling shaping, crosslinking treatment and rolling, wherein the cooling temperature in the cooling shaping step is 4 ℃, and the crosslinking treatment dosage in the crosslinking treatment step is 240KGy.
In the extrusion plasticizing step, the processing temperatures of each material in a first temperature zone, a second temperature zone, a third temperature zone, a fourth temperature zone and a die head in an extruder are respectively as follows:
MLLDPE：170℃、190℃、200℃、200℃、230℃
ULDPE：155℃、165℃、168℃、175℃、230℃
COC：180℃、200℃、205℃、210℃、230℃
TIE：195℃、215℃、220℃、225℃、230℃
EVOH：200℃、210℃、215℃、225℃、230℃
Other conditions were the same as in example 1.
Comparative example 1
A sheet material, wherein the distribution and the materials of each layer in the structure are the same as those in the embodiments 1-3, sequentially comprises a structural heat sealing layer, a functional layer, a filling layer, an adhesive layer, a barrier layer, an adhesive layer, a functional layer, a structural heat sealing layer and a structural heat sealing layer from outside to inside.
The thickness of the sheet was 750um.
The layer thickness ratio of each layer of the sheet from outside to inside is as follows: 15%, 10%, 5%, 10%, 15%, 10%.
The MLLDPE has a density of 0.93g/cm 3 and a melt index of 0.3g/10min.
The number average molecular weight of the COC is 30000, the density is 1.36g/cm 3, and the melt index is 0.1g/10min.
The ULDPE had a density of 0.910g/cm 3 and a melt index of 0.2g/10min.
The TIE had a density of 0.926g/cm 3 and a melt index of 0.5g/10min.
The density of the EVOH was 1.23g/cm 3.
The application also provides a preparation method of the high-transparency recyclable low-temperature-resistant sheet, which comprises the following steps: the preparation method comprises the steps of batching, extrusion plasticizing, cooling shaping, crosslinking treatment and rolling, wherein the cooling temperature in the cooling shaping step is 20 ℃, and the crosslinking treatment dosage in the crosslinking treatment step is 300KGy.
In the extrusion plasticizing step, the processing temperatures of each material in a first temperature zone, a second temperature zone, a third temperature zone, a fourth temperature zone and a die head in an extruder are respectively as follows:
MLLDPE：120℃、150℃、180℃、210℃、240℃
ULDPE：135℃、160℃、180℃、200℃、240℃
COC：150℃、170℃、190℃、220℃、240℃
TIE：160℃、180℃、200℃、220℃、240℃
EVOH：160℃、180℃、200℃、220℃、240℃
Comparative example 2
The thickness of the sheet was 100um.
The layer thickness ratio of each layer of the sheet from outside to inside is as follows: 15%, 10%, 5%, 10%, 15%, 10%.
The density of the MLLDPE is 0.870g/cm 3, and the melt index is 8g/10min.
The number average molecular weight of the COC is 30000, the density is 0.930g/cm 3, and the melt index is 10g/10min.
The ULDPE had a density of 0.860g/cm 3 and a melt index of 7.5g/10min.
The TIE had a density of 0.903g/cm 3 and a melt index of 6g/10min.
The density of the EVOH was 1.23g/cm 3.
The application also provides a preparation method of the high-transparency recyclable low-temperature-resistant sheet, which comprises the following steps: the preparation method comprises the steps of batching, extrusion plasticizing, cooling shaping, crosslinking treatment and rolling, wherein the cooling temperature in the cooling shaping step is 25 ℃, and the crosslinking treatment dosage in the crosslinking treatment step is 100KGy.
In the extrusion plasticizing step, the processing temperatures of each material in a first temperature zone, a second temperature zone, a third temperature zone, a fourth temperature zone and a die head in an extruder are respectively as follows:
MLLDPE：120℃、150℃、180℃、210℃、240℃
ULDPE：135℃、160℃、180℃、200℃、240℃
COC：150℃、170℃、190℃、220℃、240℃
TIE：160℃、180℃、200℃、220℃、240℃
EVOH：160℃、180℃、200℃、220℃、240℃
Other conditions were the same as in comparative example 1.
The above examples 1,2 and 3 were subjected to wet heat aging at 85 ℃ and 85% RH for 500 hours, and then the reclaimed materials were mixed and collected for standby, and 10% reclaimed materials were mixed into each layer of the sheet, and other materials, layer thicknesses and process conditions were kept unchanged according to the schemes of examples 1,2 and 3.
The method comprises the steps of mixing and collecting reclaimed materials after the wet heat aging of comparative examples 1 and 2 for 500 hours at the temperature of 85 ℃ and RH of 85%, mixing 10% reclaimed materials into each layer of the sheet, and keeping other materials, layer thicknesses and process conditions unchanged according to the schemes of comparative examples 1 and 2. The sheets prepared in examples 1-3 and comparative examples 1-2 were subjected to performance testing, and the results are shown in Table 1. As can be seen from Table 1, the sheets prepared under the conditions of examples 1, 2 and 3 of the present application had high transmittance, low haze and excellent transparency, in the case of mechanical properties equivalent to those of comparative examples 1 and 2.
The sheets obtained by blending 10% reclaimed materials into each layer of the sheets prepared in examples 1,2 and 3 and comparative examples 1 and 2 were subjected to performance test, and the results are shown in Table 2. It can be seen that the sheets of examples 1,2 and 3, after 10% of reclaimed materials were mixed into each layer, had good transparency and mechanical strength, indicating good recyclability.
TABLE 1
| Detecting items | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 |
| Transmittance (%) | 90 | 88 | 89 | 61 | 76 |
| Haze (%) | 1.2 | 1.8 | 1.6 | 39 | 22 |
| Tensile Strength (MPa) | 43 | 51 | 46 | 53 | 27 |
| Tensile modulus (GPa) | 2.7 | 3.2 | 3.1 | 3.4 | 1.8 |
| Elongation at break (%) | 590 | 610 | 530 | 120 | 380 |
TABLE 2
After the above examples 1,2 and 3 were subjected to wet heat aging at 85 ℃ and 85% RH for 500 hours, the reclaimed materials were mixed and collected for standby, and 30% reclaimed materials were mixed into each layer of the claims, and other materials, layer thicknesses and process conditions were kept unchanged according to the schemes of examples 1,2 and 3.
The recovered materials are mixed and collected for standby after the humidity and heat aging of comparative examples 1 and 2 is carried out for 500 hours at the temperature of 85 ℃ and RH of 85%, 30% of recovered materials are mixed into each layer of the claims, and other materials, layer thicknesses and process conditions are kept unchanged according to the schemes of comparative examples 1 and 2.
The sheets obtained by blending 30% reclaimed materials into each layer of the sheets prepared in examples 1,2 and 3 and comparative examples 1 and 2 were subjected to performance test, and the results are shown in Table 3. It can be seen that the sheets still have good transparency and mechanical strength after 30% recycled material is mixed in each layer of examples 1,2 and 3, indicating good recyclability.
TABLE 3 Table 3
The samples of examples 1, 2,3 and comparative examples 1, 2 were placed in an environmental chamber at-40℃for 1000 hours, and allowed to stand at room temperature for 2 hours, respectively, to conduct the test. The test results are shown in Table 4. As can be seen from Table 4, the sheets prepared in examples 1, 2 and 3 have good low temperature resistance.
TABLE 4 Table 4
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention.
Claims (4)
1. The high-transparency recyclable low-temperature-resistant sheet is characterized by sequentially comprising a structural heat sealing layer, a functional layer, a filling layer, an adhesive layer, a barrier layer, an adhesive layer, a functional layer, a structural heat sealing layer and a structural heat sealing layer from outside to inside, wherein the structural heat sealing layer is made of MLLDPE, the functional layer is made of COC, the filling layer is made of ULDPE, the adhesive layer is made of TIE, the barrier layer is made of EVOH, and the thickness of the sheet is 300-600 mu m;
The density of the MLLDPE is 0.880-0.920 g/cm 3, and the melt index is 0.5-4 g/10min;
The number average molecular weight of the COC is 14000-450000, the density is 0.950-1.450 g/cm 3, and the melt index is 3-6 g/10min;
The density of the ULDPE is 0.870-0.910 g/cm 3, and the melt index is 0.5-5 g/10min;
The density of the TIE is 0.905-0.925 g/cm 3, and the melt index is 3-4 g/10min;
The density of the EVOH is 1.17-1.21 g/cm 3.
2. The high transparency recyclable low temperature resistant sheet as claimed in claim 1, wherein: the layer thickness ratio of each layer of the sheet from outside to inside is as follows: 10 to 15 percent, 8 to 15 percent, 10 to 15 percent, 7 to 10 percent, 2 to 5 percent, 7 to 10 percent, 10 to 15 percent, 7 to 13 percent and 7 to 13 percent.
3. The method for producing a high-transparency recyclable low-temperature resistant sheet as claimed in claim 1 or 2, comprising the steps of: the preparation method comprises the steps of batching, extrusion plasticizing, cooling shaping, crosslinking treatment and rolling, wherein the cooling temperature in the cooling shaping step is 2-10 ℃, and the crosslinking treatment dosage in the crosslinking treatment step is 200-250 KGy.
4. A method of producing a highly transparent recyclable low temperature resistant sheet as described in claim 3 wherein in the extrusion plasticizing step, the processing temperatures of each material in the first temperature zone, the second temperature zone, the third temperature zone, the fourth temperature zone and the die in the extruder are as follows:
MLLDPE:160-180℃、180-200℃、190-210℃、195-210℃、225-240℃
ULDPE:150-165℃、160-175℃、165-170℃、170-185℃、225-240℃
COC:170-190℃、190-210℃、195-215℃、200-220℃、225-240℃
TIE:190-210℃、210-230℃、215-235℃、215-235℃、225-240℃EVOH:180-220℃、200-220℃、210-225℃、220-230℃、225-240℃。
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| CN102501511A (en) * | 2011-11-18 | 2012-06-20 | 佛山佛塑科技集团股份有限公司 | Barrier heat sealing type biaxial tensile composite thin film and preparation method thereof |
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