CN102019738A - POSS (polyhedral oligomeric silsesquioxanes) modified high barrier three-layer co-extrusion packaging film and preparation method thereof - Google Patents
POSS (polyhedral oligomeric silsesquioxanes) modified high barrier three-layer co-extrusion packaging film and preparation method thereof Download PDFInfo
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Abstract
The invention provides a POSS (polyhedral oligomeric silsesquioxanes) modified high barrier three-layer co-extrusion packaging film and a preparation method thereof, relating to a packaging film. The invention provides a polyhedral oligomeric silsesquioxanes modified high barrier three-layer co-extrusion packaging film with better barrier property, mechanical property, heat resistance and transparency and a preparation method thereof. The film comprises an outer layer, an intermediate layer and an inner layer, wherein the outer layer of the film comprises the components of low-density polyethylene, linear low-density polyethylene and a polyhedral oligomeric silsesquioxanes modifier, the intermediate layer of the film comprises the components of ethylene-vinyl alcohol copolymer and compatibilizing resins, and the inner layer of the film comprises the components of LDPE, LLDPE and an opening agent. Firstly, the polyhedral oligomeric silsesquioxanes modifier is prepared, then the outer layer film master batch containing the polyhedral oligomeric silsesquioxanes modifier is prepared, and finally the polyhedral oligomeric silsesquioxanes modified high barrier three-layer co-extrusion packaging film is prepared.
Description
Technical field
The present invention relates to a kind of packing film, relate in particular to three-layer co-extruded packing film of high barrier of a kind of employing polyhedral oligomeric silsesquioxane (POSS) modification and preparation method thereof.
Background technology
Along with science and technology development and growth in the living standard, people have proposed various new requirements to packaging material.In the packaging for foodstuff field, require packaging material higher barrier to be arranged, to prolong the shelf-life of food to oxygen, carbon dioxide and glassware for drinking water.Packing technique method in actual at present the use is a lot, comprises vacuum packaging, gas flush packaging, damp-prrof packing, Deoxygen Packaging, self-regulated atmosphere packaging etc., all be unable to do without the isolation-type film packing material.Up to the present, although the barrier packaging film comprises composite membrane, kind is a lot, still can not satisfy the barrier requirement of people to packaging for foodstuff fully.Therefore, the packing circle is making great efforts to develop high barrier, good combination property, desirable barrier packaging material transparent, safe in utilization always.At present, the barrier packaging material of extensive use mainly contains Vingon (PVDC), ethylene-vinyl alcohol copolymer (EVOH) and nitrile resin.
Wherein EVOH has good barrier properties for gases and resistance is moist, and this is the result who combines behind polyethylene and the polyvinyl alcohol two class superpolymer performances.Polyethylene hinders moist good, and the gas barrier property of polyvinyl alcohol is good.The 1950's, du pont company has obtained EVOH by copolymerization, alcoholysis reaction first.Kuraray company has then realized the suitability for industrialized production of EVOH resin the earliest in 1972.At present domestic existing many people did the research of EVOH packing film aspect.(Jin Tieling such as Jin Tieling, Deng. forest chemical engineering communication, 1995,6:3-6) set forth the urgency of developing novel high-barrier packaging material EVOH resin, the technology and the flow process of synthetic EVOH resin have been studied, and the alcoholysis process of EVOH resin carried out systematic research, and the basic mechanical design feature index of the EVOH resin of succeeding in developing, approaching with Japanese Kuraray company like product.(Chinese invention patent such as Cai Gangfeng, publication number: CN1430627A, improve oxygen barrier performance by ethene improved/ethenol copolymer (EVOH)) EVOH that has oxygen removing functional group is disclosed, the EVOH of this modification can be used for the oxygen barrier applications, as forming the oxygen barrier layer of packing articles.Zhao Xiaodong etc. (Zhao Xiaodong etc., petrochemical technology and application, 2006,6:448-450) studied heat fusing performance, physical and mechanical properties and the processing rheological property of EVOH, and when finding, can significantly improve the hot strength of blend with EVOH modification HDPE; During with HDPE modification EVOH, the melt viscosity of material descends, and the extruder load reduces, and the processing rheological property of blend improves.(Chinese invention patents such as Deng Peng Yang, publication number: CN1948389, ethylene-vinyl alcohol copolymer of a kind of modification and preparation method thereof) disclose a kind of ethylene-vinyl alcohol copolymer and preparation method thereof of modification, under equal conditions, its water absorption rate has only 30%～40% of common EVOH film.(Chinese invention patent such as Wu Yanqiu, publication number: CN101323685A, blend film of LLDPE and ethylene-vinyl alcohol copolymer and preparation method thereof) solves LLDPE and EVOH is incompatible, must between when the two uses have jointly added the problem of adhesive layer.But because polyvinyl alcohol is to belong to hydrophilic film, understand adsorption moisture, will influence the barrier property of film like this.Therefore EVOH preferably uses the intermediate layer at multi-layer compound film, has the moist polyolefine material of high resistant with other again and stops its adsorption moisture at skin.
Polyhedral oligomeric silsesquioxane (POSS) is a kind of polymer reinforcing material that is subjected to extensive concern in recent years in the world, it belongs to the silica/silicon oxygen alkane hybrid of nanoscale, can combine with multiple organic polymer, the inorganic-organic hybridization that forms nanoscale strengthens polymer, significantly improves hear resistance, crocking resistance and the mechanical property of material.
Summary of the invention
Purpose of the present invention aims to provide a kind of barrier property, mechanical property, heat resistance and the transparency three-layer co-extruded packing film of polyhedral oligomeric silsesquioxane (POSS) modification high-barrier and preparation method thereof preferably that has.
That the three-layer co-extruded packing film of described polyhedral oligomeric silsesquioxane modification high-barrier comprises is outer, in, three layers of linings, wherein the outer membrane component is 10%～20% low density polyethylene (LDPE) (LDPE), 74%～87% linear low density polyethylene (LLDPE) (LLDPE) and 3%～6% polyhedral oligomeric silsesquioxane modifier, in the layer film component be 85%～90% ethylene-vinyl alcohol copolymer (EVOH) and 10%～15% compatible resin, nexine film component is 10%～20% LDPE, 79%～89% LLDPE and 1% opening agent.
The thickness of the three-layer co-extruded packing film of described polyhedral oligomeric silsesquioxane modification high-barrier can be 40～60 μ m, and the thickness of the thickness of outer membrane, the thickness of middle layer film and nexine film is preferably identical.
Described compatible resin can be PE-g-MAH etc.
Described opening agent can be oleamide etc.
The structural formula of described polyhedral oligomeric silsesquioxane modifier is as follows:
Wherein: R=-i-C
4H
9, n=1～6.
The preparation method of the three-layer co-extruded packing film of described polyhedral oligomeric silsesquioxane modification high-barrier may further comprise the steps:
1) preparation of polyhedral oligomeric silsesquioxane modifier:
Under the nitrogen protection, in reaction system, add (i-C successively
4H
9)
7Si
8O
9(OH)
319.9%～211%, oxolane (THF) 64.4%～67.0% and Et
3N 7.6%～8.1%, and positive alkyl trichlorosilane CH reinjects
3(CH
2)
nCH
2SiCl
3Behind the stirring reaction, filter (n=1～6) 4.7%～6.6%, and the filtrate rotary evaporation obtains the faint yellow solid powder, and crystallization in the solution of toluene and acetonitrile then obtains polyhedral oligomeric silsesquioxane modifier, and its reaction equation is as follows:
2) contain the preparation of the outer membrane master batch of polyhedral oligomeric silsesquioxane modifier:
By outer membrane component proportioning low density polyethylene (LDPE) 10%～20%, linear low density polyethylene (LLDPE) 74%～87%, polyhedral oligomeric silsesquioxane modifier 3%～6% are put into stirrer for mixing, granulation then, oven dry;
3) preparation of the three-layer co-extruded packing film of polyhedral oligomeric silsesquioxane modification high-barrier:
By middle layer film component and nexine film component proportioning, respectively with the ethylene-vinyl alcohol copolymer (EVOH) of middle level film raw material 85%～90% and 10%～15% compatible resin, the LDPE of nexine film raw material 10%～20%, 79%～89% LLDPE and 1% opening agent are even in stirrer for mixing, then on three-layer co-extruded cast film machine production line, outer master batch, middle level and nexine raw material are carried out the mixed melting plasticizing respectively, by dosage coextrusion curtain coating, obtain the three-layer co-extruded packing film of polyhedral oligomeric silsesquioxane modification high-barrier.
In step 1), the time of described stirring reaction can be 12～20h; Obtain being preferably in behind the polyhedral oligomeric silsesquioxane modifier behind 50～70 ℃ of following vacuum drying 12h standby.
In step 2) in, described granulation, available double screw extruder melt extrudes granulation, and 9 district's heating-up temperatures of described double screw extruder can be respectively 170～180 ℃, 180～200 ℃, 200～220 ℃, 210～220 ℃, 210～220 ℃, 200～210 ℃, 190～210 ℃, 190～200 ℃, 180～190 ℃.
In step 3), the thickness of the three-layer co-extruded packing film of described polyhedral oligomeric silsesquioxane modification high-barrier is preferably 40～60 μ m, and the thickness of the outer membrane of the three-layer co-extruded packing film of described polyhedral oligomeric silsesquioxane modification high-barrier, the thickness of middle layer film are identical with the thickness of nexine film.
The present invention adopts POSS to carry out modification, utilize POSS to have certain hydrophobicity and the characteristics that have to surface enrichment trend, by adding the skin of an amount of POSS to three-layer co-extruded film, make it form the comparatively fine and close thin layer of one deck at film surface, evoh layer adsorption moisture in the middle of can effectively stoping improves the barrier property of film and the wearability on surface; And the rigid structure of POSS and steric effect, hindered the disconnected motion of Polyethylene Chain, thereby increased the difficulty that little molecule permeates in polymer, also improved mechanical properties in films and hear resistance simultaneously; In addition, POSS endorses the microfacies district that forms nano inorganic by the inorganic cage shape that silica constituted, and avoids a large amount of reunions of inorganic particulate, makes it be scattered in the matrix resin equably, and have stronger surperficial adhesion between POSS and the matrix, guaranteed the transparency that film is good.
The specific embodiment
The invention will be further described below by embodiment.
Embodiment 1:
Step 1: in being full of the flask of high pure nitrogen, add (i-C successively
4H
9)
7Si
8O
9(OH)
37.119g, THF 25ml and Et
3N 2.732g slowly injects positive alkyl trichlorosilane CH then
3(CH
2)
nCH
2SiCl
3(n=1) 1.598g.After stirring is spent the night, filter, the filtrate rotary evaporation obtains the faint yellow solid powder.Crystallization in the solution of toluene and acetonitrile obtains POSS modifier, and is standby behind 50 ℃ of following vacuum drying 12h.
Step 2: with LDPE, LLDPE, that POSS modifier is put into stirrer for mixing in 10: 87: 3 ratio is even, melt extrudes granulation with double screw extruder then, the temperature of 9 districts heating is respectively 170,180,200,210,210,200,190,190,180 ℃.The master batch of making is dried under vacuum condition, and POSS content is 3% in the master batch.。
15) and nexine (LDPE: LLDPE: oleamide=20: 79: 1) even in stirrer for mixing respectively step 3: with middle level (EVOH: PE-g-MAH=85:, then with outer master batch (LDPE: LLDPE: POSS modifier=10: 87: 3) by three-layer co-extruded cast film machine coextrusion curtain coating, obtain the three-layer co-extruded packing film of POSS modification high barrier, thickness is 60 μ m.
Step 4: sample is placed the performance of each side such as its hot strength of test, elongation at break, maximum heat sealing strength, water vapour permeability after 3 days at normal temperatures, the results are shown in Table 1.
Embodiment 2:
Step 1: in being full of the flask of high pure nitrogen, add (i-C successively
4H
9)
7Si
8O
9(OH)
37.910g, THF 30ml and Et
3N 3.036g slowly injects positive alkyl trichlorosilane CH then
3(CH
2)
nCH
2SiCl
3(n=4) 2.195g.After stirring is spent the night, filter, the filtrate rotary evaporation obtains the faint yellow solid powder.Crystallization in the solution of toluene and acetonitrile obtains POSS modifier, and is standby behind 70 ℃ of following vacuum drying 12h.
Step 2: with embodiment 1.
10) and nexine (LDPE: LLDPE: oleamide=10: 89: 1) even in stirrer for mixing respectively step 3: with middle level (EVOH: PE-g-MAH=90:, then with outer master batch (LDPE: LLDPE: POSS modifier=10: 87: 3) by three-layer co-extruded cast film machine coextrusion curtain coating, obtain the three-layer co-extruded packing film of POSS modification high barrier, thickness is 60 μ m.
Step 4: sample is placed the performance of its each side of test after 3 days at normal temperatures, the results are shown in Table 1.
Embodiment 3:
Step 1: in being full of the flask of high pure nitrogen, add (i-C successively
4H
9)
7Si
8O
9(OH)
38.701g, THF 30ml and Et
3N 3.340g slowly injects positive alkyl trichlorosilane CH then
3(CH
2)
nCH
2SiCl
3(n=6) 2.732g.After stirring is spent the night, filter, the filtrate rotary evaporation obtains the faint yellow solid powder.Crystallization in the solution of toluene and acetonitrile obtains POSS modifier, and is standby behind 70 ℃ of following vacuum drying 12h.
Step 2: with LDPE, LLDPE, that POSS modifier is put into stirrer for mixing in 20: 74: 6 ratio is even, POSS content is 6% in the master batch.Melt extrude granulation with double screw extruder then, the temperature of 9 districts heating is respectively 180,200,220,220,220,210,210,200,190 ℃.The master batch of making is dried under vacuum condition.
15) and nexine (LDPE: LLDPE: oleamide=10: 89: 1) even in stirrer for mixing respectively step 3: with middle level (EVOH: PE-g-MAH=85:, then with outer master batch (LDPE: LLDPE: POSS modifier=20: 74: 6) by three-layer co-extruded cast film machine coextrusion curtain coating, obtain the three-layer co-extruded packing film of POSS modification high barrier, thickness is 60 μ m.
Step 4: sample is placed the performance of its each side of test after 3 days at normal temperatures, the results are shown in Table 1.
Embodiment 4:
Step 1: with embodiment 3.
Step 2: with LDPE, LLDPE, that POSS modifier is put into stirrer for mixing in 10: 87: 3 ratio is even, POSS content is 3% in the master batch.Melt extrude granulation with double screw extruder then, the temperature of 9 districts heating is respectively 180,200,220,220,220,210,210,200,190 ℃.The master batch of making is dried under vacuum condition.
Step 3: with embodiment 2.
Step 4: sample is placed the performance of test its each side in back after 3 days at normal temperatures, the results are shown in Table 1.
Embodiment 5:
Step 1: with embodiment 2.
Step 2: with LDPE, LLDPE, that POSS modifier is put into stirrer for mixing in 20: 74: 6 ratio is even, POSS content is 6% in the master batch.Melt extrude granulation with double screw extruder then, the temperature of 9 districts heating is respectively 170,180,200,210,210,200,190,190,180 ℃.The master batch of making is dried under vacuum condition.
Step 3: with embodiment 3.
Step 4: sample is placed the performance of test its each side in back after 3 days at normal temperatures, the results are shown in Table 1.
Embodiment 6:
Step 1: with embodiment 2.
Step 2: with embodiment 3.
10) and nexine (LDPE: LLDPE: oleamide=20: 79: 1) even in stirrer for mixing respectively step 3: with middle level (EVOH: PE-g-MAH=90:, then with outer master batch (LDPE: LLDPE: POSS modifier=20: 74: 6) by three-layer co-extruded cast film machine coextrusion curtain coating, obtain the three-layer co-extruded packing film of POSS modification high barrier, thickness is 60 μ m.
Step 4: sample is placed the performance of test its each side in back after 3 days at normal temperatures, the results are shown in Table 1.
Table 1 The performance test results
Claims (10)
1. three-layer co-extruded packing film of polyhedral oligomeric silsesquioxane modification high-barrier, it is characterized in that comprising outer, in, three layers of linings, wherein the outer membrane component is 10%～20% low density polyethylene (LDPE), 74%～87% linear low density polyethylene (LLDPE) and 3%～6% polyhedral oligomeric silsesquioxane modifier, in the layer film component be 85%～90% ethylene-vinyl alcohol copolymer and 10%～15% compatible resin, nexine film component is 10%～20% low density polyethylene (LDPE), 79%～89% linear low density polyethylene (LLDPE) and 1% opening agent.
2. the three-layer co-extruded packing film of a kind of polyhedral oligomeric silsesquioxane modification high-barrier as claimed in claim 1, the thickness that it is characterized in that the three-layer co-extruded packing film of described polyhedral oligomeric silsesquioxane modification high-barrier is 40～60 μ m.
3. the three-layer co-extruded packing film of a kind of polyhedral oligomeric silsesquioxane modification high-barrier as claimed in claim 1 or 2 is characterized in that the thickness of the thickness of the outer membrane of the three-layer co-extruded packing film of described polyhedral oligomeric silsesquioxane modification high-barrier, middle layer film is identical with the thickness of nexine film.
4. the three-layer co-extruded packing film of a kind of polyhedral oligomeric silsesquioxane modification high-barrier as claimed in claim 1 is characterized in that described compatible resin is PE-g-MAH.
5. the three-layer co-extruded packing film of a kind of polyhedral oligomeric silsesquioxane modification high-barrier as claimed in claim 1 is characterized in that described opening agent is an oleamide.
6. the three-layer co-extruded packing film of a kind of polyhedral oligomeric silsesquioxane modification high-barrier as claimed in claim 1 is characterized in that the structural formula of described polyhedral oligomeric silsesquioxane modifier is as follows:
Wherein: R=-i-C
4H
9, n=1～6.
7. the preparation method of the three-layer co-extruded packing film of a kind of polyhedral oligomeric silsesquioxane modification high-barrier as claimed in claim 1 is characterized in that may further comprise the steps:
1) preparation of polyhedral oligomeric silsesquioxane modifier:
Under the nitrogen protection, in reaction system, add (i-C successively
4H
9)
7Si
8O
9(OH)
319.9%～21.1%, oxolane 64.4%～67.0% and Et
3N 7.6%～8.1%, and positive alkyl trichlorosilane CH reinjects
3(CH
2)
nCH
2SiCl
34.7%～6.6%, behind the stirring reaction, filter n=1～6, and the filtrate rotary evaporation obtains the faint yellow solid powder, and crystallization in the solution of toluene and acetonitrile then obtains polyhedral oligomeric silsesquioxane modifier;
2) contain the preparation of the outer membrane master batch of polyhedral oligomeric silsesquioxane modifier:
By outer membrane component proportioning low density polyethylene (LDPE) 10%～20%, linear low density polyethylene (LLDPE) 74%～87%, polyhedral oligomeric silsesquioxane modifier 3%～6% are put into stirrer for mixing, granulation then, oven dry;
3) preparation of the three-layer co-extruded packing film of polyhedral oligomeric silsesquioxane modification high-barrier:
By middle layer film component and nexine film component proportioning, respectively with the ethylene-vinyl alcohol copolymer of middle level film raw material 85%～90% and 10%～15% compatible resin, the low density polyethylene (LDPE) of nexine film raw material 10%～20%, 79%～89% linear low density polyethylene (LLDPE) and 1% opening agent are in stirrer for mixing, then on three-layer co-extruded cast film machine production line, with outer master batch, middle level and nexine raw material carry out the mixed melting plasticizing respectively, by dosage coextrusion curtain coating, obtain the three-layer co-extruded packing film of polyhedral oligomeric silsesquioxane modification high-barrier.
8. the preparation method of the three-layer co-extruded packing film of a kind of polyhedral oligomeric silsesquioxane modification high-barrier as claimed in claim 7 is characterized in that in step 1) the time of described stirring reaction is 12～20h; Obtain behind the polyhedral oligomeric silsesquioxane modifier standby behind 50～70 ℃ of following vacuum drying 12h.
9. the preparation method of the three-layer co-extruded packing film of a kind of polyhedral oligomeric silsesquioxane modification high-barrier as claimed in claim 7 is characterized in that in step 2) in, described granulation, melt extrude granulation with double screw extruder, 9 district's heating-up temperatures of described double screw extruder are respectively 170～180 ℃, and 180～200 ℃, 200～220 ℃, 210～220 ℃, 210～220 ℃, 200～210 ℃, 190～210 ℃, 190～200 ℃, 180～190 ℃.
10. the preparation method of the three-layer co-extruded packing film of a kind of polyhedral oligomeric silsesquioxane modification high-barrier as claimed in claim 7, it is characterized in that in step 3) the thickness of the three-layer co-extruded packing film of described polyhedral oligomeric silsesquioxane modification high-barrier is 40～60 μ m; The thickness of the outer membrane of the three-layer co-extruded packing film of described polyhedral oligomeric silsesquioxane modification high-barrier, the thickness of middle layer film are identical with the thickness of nexine film.
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