CN102848673A - High-oxygen resistant steaming-resistant polyvinylidene chloride coating film and manufacturing method thereof - Google Patents
High-oxygen resistant steaming-resistant polyvinylidene chloride coating film and manufacturing method thereof Download PDFInfo
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- CN102848673A CN102848673A CN201210294409XA CN201210294409A CN102848673A CN 102848673 A CN102848673 A CN 102848673A CN 201210294409X A CN201210294409X A CN 201210294409XA CN 201210294409 A CN201210294409 A CN 201210294409A CN 102848673 A CN102848673 A CN 102848673A
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- polyvinylidene chloride
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- resistant oxygen
- coating
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- 229920001328 Polyvinylidene chloride Polymers 0.000 title claims abstract description 98
- 239000005033 polyvinylidene chloride Substances 0.000 title claims abstract description 98
- 238000000576 coating method Methods 0.000 title claims abstract description 96
- 239000001301 oxygen Substances 0.000 title claims abstract description 85
- 229910052760 oxygen Inorganic materials 0.000 title claims abstract description 85
- 239000011248 coating agent Substances 0.000 title claims abstract description 79
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 11
- 238000010025 steaming Methods 0.000 title abstract 7
- 239000000839 emulsion Substances 0.000 claims abstract description 49
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000002086 nanomaterial Substances 0.000 claims abstract description 21
- 239000003381 stabilizer Substances 0.000 claims abstract description 10
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 9
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000004816 latex Substances 0.000 claims abstract description 9
- 229920000126 latex Polymers 0.000 claims abstract description 9
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 7
- NLHHRLWOUZZQLW-UHFFFAOYSA-N Acrylonitrile Chemical compound C=CC#N NLHHRLWOUZZQLW-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000008234 soft water Substances 0.000 claims abstract description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 78
- 238000009835 boiling Methods 0.000 claims description 77
- 239000003795 chemical substances by application Substances 0.000 claims description 57
- 238000003756 stirring Methods 0.000 claims description 37
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 36
- 239000010408 film Substances 0.000 claims description 35
- 239000000463 material Substances 0.000 claims description 31
- 239000010409 thin film Substances 0.000 claims description 31
- 239000002904 solvent Substances 0.000 claims description 29
- 238000001035 drying Methods 0.000 claims description 23
- 239000004814 polyurethane Substances 0.000 claims description 22
- 229920002635 polyurethane Polymers 0.000 claims description 22
- 229910000831 Steel Inorganic materials 0.000 claims description 18
- 239000004203 carnauba wax Substances 0.000 claims description 18
- 239000000377 silicon dioxide Substances 0.000 claims description 18
- 239000010959 steel Substances 0.000 claims description 18
- 235000011194 food seasoning agent Nutrition 0.000 claims description 17
- 238000002156 mixing Methods 0.000 claims description 17
- 230000004048 modification Effects 0.000 claims description 17
- 238000012986 modification Methods 0.000 claims description 17
- 229910052799 carbon Inorganic materials 0.000 claims description 16
- 238000000034 method Methods 0.000 claims description 15
- 238000003851 corona treatment Methods 0.000 claims description 11
- 239000002981 blocking agent Substances 0.000 claims description 9
- 238000005096 rolling process Methods 0.000 claims description 9
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Chemical group [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 claims description 8
- 125000002573 ethenylidene group Chemical group [*]=C=C([H])[H] 0.000 claims description 6
- 239000000853 adhesive Substances 0.000 claims description 5
- 230000001070 adhesive effect Effects 0.000 claims description 5
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 4
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 4
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 4
- 150000002148 esters Chemical class 0.000 claims description 4
- 230000008569 process Effects 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 239000000758 substrate Substances 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 2
- 235000010216 calcium carbonate Nutrition 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- 239000010445 mica Substances 0.000 claims description 2
- 229910052618 mica group Inorganic materials 0.000 claims description 2
- 229920006267 polyester film Polymers 0.000 claims description 2
- 239000007787 solid Substances 0.000 claims description 2
- 238000010792 warming Methods 0.000 claims description 2
- 238000004804 winding Methods 0.000 claims description 2
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 abstract description 2
- 239000000178 monomer Substances 0.000 abstract description 2
- 239000011247 coating layer Substances 0.000 abstract 3
- OEPOKWHJYJXUGD-UHFFFAOYSA-N 2-(3-phenylmethoxyphenyl)-1,3-thiazole-4-carbaldehyde Chemical compound O=CC1=CSC(C=2C=C(OCC=3C=CC=CC=3)C=CC=2)=N1 OEPOKWHJYJXUGD-UHFFFAOYSA-N 0.000 abstract 1
- 239000000945 filler Substances 0.000 abstract 1
- 239000003292 glue Substances 0.000 abstract 1
- 239000003999 initiator Substances 0.000 abstract 1
- 239000010410 layer Substances 0.000 abstract 1
- 239000012748 slip agent Substances 0.000 abstract 1
- WSLDOOZREJYCGB-UHFFFAOYSA-N 1,2-Dichloroethane Chemical group ClCCCl WSLDOOZREJYCGB-UHFFFAOYSA-N 0.000 description 21
- 230000001954 sterilising effect Effects 0.000 description 15
- 238000004659 sterilization and disinfection Methods 0.000 description 15
- 238000005303 weighing Methods 0.000 description 14
- 229920006378 biaxially oriented polypropylene Polymers 0.000 description 7
- 239000011127 biaxially oriented polypropylene Substances 0.000 description 7
- 238000010411 cooking Methods 0.000 description 7
- 230000029087 digestion Effects 0.000 description 7
- 239000003595 mist Substances 0.000 description 7
- 230000035515 penetration Effects 0.000 description 7
- 230000035699 permeability Effects 0.000 description 7
- 229920000728 polyester Polymers 0.000 description 7
- 230000004888 barrier function Effects 0.000 description 3
- 235000013305 food Nutrition 0.000 description 3
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- OSDWBNJEKMUWAV-UHFFFAOYSA-N Allyl chloride Chemical compound ClCC=C OSDWBNJEKMUWAV-UHFFFAOYSA-N 0.000 description 1
- 206010009866 Cold sweat Diseases 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000005030 aluminium foil Substances 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- NEHMKBQYUWJMIP-UHFFFAOYSA-N chloromethane Chemical group ClC NEHMKBQYUWJMIP-UHFFFAOYSA-N 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 229920001577 copolymer Polymers 0.000 description 1
- 238000002788 crimping Methods 0.000 description 1
- 235000021438 curry Nutrition 0.000 description 1
- 230000032798 delamination Effects 0.000 description 1
- 230000000368 destabilizing effect Effects 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 235000013372 meat Nutrition 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
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- 239000002861 polymer material Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000005028 tinplate Substances 0.000 description 1
- 238000004017 vitrification Methods 0.000 description 1
- 230000002087 whitening effect Effects 0.000 description 1
- 238000004383 yellowing Methods 0.000 description 1
Abstract
The invention relates to a high-oxygen resistant steaming-resistant polyvinylidene chloride coating film and a manufacturing method thereof. The high-oxygen resistant steaming-resistant polyvinylidene chloride coating film comprises a base, a coating layer on the surface of the base, and a base glue layer between the coating layer and the base. The coating layer is a coating obtained by coating modified high-oxygen resistant steaming-resistant polyvinylidene chloride latex. The modified high-oxygen resistant steaming-resistant polyvinylidene chloride latex comprises: by weight, 30 to 38% of a high-oxygen resistant steaming-resistant polyvinylidene chloride blended emulsion, 1.5 to 6% of a nano-material filler, 1 to 8% of a slip agent, 0.1 to 5% of an abherent and 5 to 60% of softened water. The high-oxygen resistant steaming-resistant polyvinylidene chloride blended emulsion comprises: by weight, 40 to 94% of a vinylidene chloride monomer, 1.5 to 10% of an acrylate, 1 to 6% of one or more of acrylic acid and acrylonitrile, 0.5 to 2% of an initiator, 0.1 to 0.8% of an emulsifier, 0.5 to 1% of a stabilizer and 0 to 55% of soft water.
Description
Affiliated technical field
The present invention relates to a kind of high resistant oxygen polyvinylidene chloride of anti-boiling coated thin film and manufacture method thereof, belong to the novel high polymer material field.
Background technology
Vial and metal can are becoming the major way of food storage in very over a long time in the past always, the foods packed in carton containers that American Studies in 1958 goes out is packed and is successfully replaced the tinplate can, and beginning commercialization large-scale production, nineteen sixty-eight is played Japan's beginning with high-temperature retort bag packing curry, rice, meat ball etc., the thermophilic digestion sterilization becomes a kind of method of prolongation effective period of food quality commonly used, but because the thermophilic digestion condition is harsh, the high-temperature retort bag technical capability waits perfect in addition, so far, every year all can be because of the bag that rises that occurs in the digestion process, broken bag, peculiar smell, delamination, surface wrinkling, crimping, gas leakage, the problem such as pin hole occurs and cause quality dispute.At present, when selecting the thermophilic digestion bag material, except overcoming the above problems, safety and environmental protection, low cost, excellent barrier property and can prolong better shelf life and become the technical parameter that manufacturer at first considers.
Summary of the invention
For above problem, the object of the present invention is to provide a kind of high resistant oxygen polyvinylidene chloride of anti-boiling coated thin film, the high resistant oxygen polyvinylidene chloride of anti-boiling latex that this coated thin film makes take modification of the present invention is as organic coating, efficiently solve and adopt aluminium foil etc. to do the shortcoming that pin hole appears in composite bed easily, energy digestion resistant and non-whitening are non-yellowing, and safety and environmental protection, have excellent oxygen barrier property.After dry type is compound, reduced to a great extent vacuumize, high pressure, rise bag, bale broken, gas leak phenomenon during pressure oscillation have prolonged to a great extent shelf life and have reduced cost.
The high resistant oxygen polyvinylidene chloride of anti-boiling coated thin film provided by the invention, the dope layer that comprises base material and substrate surface, primer layer between dope layer and the base material, described dope layer is the high resistant oxygen polyvinylidene chloride of anti-boiling coating that is formed after primer layer surface and oven dry by the high resistant oxygen polyvinylidene chloride of anti-boiling latex-coating that the present invention makes by modification, the described high resistant oxygen polyvinylidene chloride of anti-boiling latex is formulated by the raw material that contains following weight content: the high resistant oxygen polyvinylidene chloride of anti-boiling blending emulsion 30-88%, nanomaterial-filled dose of 1.5-6%, slipping agent 1-8%, antitack agent 0.1-5%, the 5-60% demineralized water; The described high resistant oxygen polyvinylidene chloride of anti-boiling blending emulsion is made by the raw material that contains following weight content: the vinylidene of 40-94%, the esters of acrylic acid of 1.5-10% and the acrylic acid of 1-6% and acrylonitrile mixed liquor or among both any one, the initator of 0.5-2%, the emulsifying agent of 0.1-0.8%, the stabilizing agent of 0.5-1%, 0-55% soft water.
The described high resistant oxygen polyvinylidene chloride of anti-boiling latex, solid content is preferably 45-55%, keeps amorphous state in can be for a long time in this scope, and have good film forming ability when drying.
Described nanomaterial-filled dose is in CaCO3, TiO2, mica, the imvite any one, with the filling-modified core of the inorganic material of particle scale and nanoscale, can improve interface bond strength, prevent from being separated, further improve barrier property and mechanical property.
Described esters of acrylic acid is preferably methyl methacrylate.
Described initator is preferably sodium peroxydisulfate.
Described emulsifying agent is preferably neopelex.
The preferred J-1 stabilizing agent of described stabilizing agent, its characteristics be to the good stability of light and heat, and transparency is high, can keep not roll banding in high temperature process, not stop up, and especially has good later stage heat endurance.
Described acrylate monomer is: methyl acrylate, acrylonitrile monemer with a small amount of polar group, can change the different vitrification point of copolymer.
Described stabilizing agent can improve in PVC is synthetic generation allyl chloride, tertiary carbon chlorine and two keys etc. and is in its molecular chain structure destabilizing factor and make the polyvinylidene chloride coated film possess high-fire resistance and long-actingization in thermophilic digestion.
Described base material film is biaxially oriented polyester film, and thickness is 8-120 μ m.
Described primer layer is that aqueous polyurethane or solvent borne polyurethane add the coating that solvent forms, and polyurethane adhesive shows activity and the polarity of height, can make the base material and the coating that contain active hydrogen that good chemical adhesive power is arranged.
Described polyurethane adhesive comprises host, curing agent.
Described slipping agent is the palm wax slipping agent, has good dispersive property in coating, and suitable consumption can prevent from being clamminess mildew-resistant.
Described antitack agent is the silica anti-blocking agent.
The coating weight of described dope layer is 0.8-5.0g/m
2
The coating weight of described primer layer is 0.3-1.5g/m
2
Correspondingly, the present invention also provides a kind of manufacture method of the high resistant oxygen polyvinylidene chloride of anti-boiling coated thin film, and the method comprises the steps:
1, the soft water that in reactor, adds successively first 0-55%, the initator sodium peroxydisulfate of 0.5-2%, the J-1 stabilizing agent of 0.5-1% and the vinylidene of 40-94%, then vacuumize--adding nitrogen--row pressure-vacuumize-Jia nitrogen-row pressure, finish half operation twice, pressure is controlled to be-0.08Mpa., mixing speed is 60-180 rev/min, heats up temperature is controlled in the 50-85 ℃ of scope, fully stirs 30-60 minute, and vinylidene is dissolved fully, obtains seed emulsion.Drip the 1.5-10% methyl methacrylate, 1-6% acrylic acid, the emulsifying agent neopelex of 1-6% acrylonitrile and 0.1-0.8%, rate of addition 5-15 gram/minute.Be warming up to 90 ℃ after dripping and continue to keep 30-90 minute, whole system is fully reacted.At last, be cooled to normal temperature and pressure, make the high resistant oxygen polyvinylidene chloride of anti-boiling blending emulsion.
2, add the above-mentioned high resistant oxygen polyvinylidene chloride of anti-boiling blending emulsion that makes in rustless steel container, stirred 20-40 minute, speed 60-200 rev/min, temperature is controlled in the 40-50 ℃ of scope.Then add nanomaterial-filled dose of 1.5-6%, and then improve temperature of reaction kettle to 55-60 ℃, the interior material of reactor is fully mixed.While stirring the palm wax slipping agent that adds successively 1-8%, the silica anti-block of 0.1-5% and the demineralized water of 5-60%, after stirring the high resistant oxygen polyvinylidene chloride of anti-boiling latex, operation to be coated is used.
3, polyurethane adhesive host and the curing agent ratio in 5: 1 is added in another rustless steel container successively, add solvent dilution while stir, solvent proportion is 4 times of host, can form primer after stirring, and next process to be entered uses.
4, unwinding tension being set is 2-6bar, and base film is carried out sided corona treatment, with coating apparatus primer evenly is coated with and oven dry on the substrate surface after the sided corona treatment, and coating speed is 80-250 m/min, and the primary coat coating weight is controlled at 0.2-1.5g/m
2Bake out temperature is 80-160 ℃, and be 6 seconds drying time.After cooling, through coating apparatus the high resistant oxygen polyvinylidene chloride of anti-boiling emulsion uniform that above-mentioned steps 2 makes is coated on the primer, coating weight is controlled to be 0.8-4.5g/m again
2, the film of then coating being finished is dried, and coating speed is 80-250 m/min, and bake out temperature is 80-160 ℃, drying time 8 seconds.The complete rear rolling of the high resistant oxygen polyvinylidene chloride of anti-boiling coated and dried, the winding tension rate of decay is 40-55%.Coated film volume is placed under 45 ℃ of conditions and solidified 2 days, makes the high resistant oxygen polyvinylidene chloride of anti-boiling coated thin film of the present invention.
Coating speed in the above-mentioned steps is preferably 150-250m/min, can guarantee coating quality and make production efficiency higher; The preferred hot-air seasoning of drying course or Far-infrared Heating oven dry, or adopt simultaneously far infrared and hot-air seasoning dual mode; Coating method preferably reverses the roller kiss-type coating method, and can effectively solve traditional coating method coating and pollute other roller problem, and the difficult problem of coating coating lack of homogeneity.
The anti-boiling coated film of the high resistant oxygen that the present invention makes, be thirty minutes long 135 ℃ thermophilic digestion of Gao Kenai, transparent coated film presentation the exterior quality of interior bag thing uniqueness.Table one is compared with the existing polyvinylidene chloride of anti-boiling the (hereinafter to be referred as PVDC) coated film for the anti-boiling coated film of high resistant oxygen has following advantage:
Table one
Annotate: 1) the oxygen flow testing conditions is: 23 ℃, and 0%RH; Permeable testing conditions is: 38 ℃, and 90%RH
The specific embodiment
Following specific embodiment is described further the high resistant oxygen polyvinylidene chloride of anti-boiling coated thin film of the present invention and manufacture method thereof.
Embodiment one
Base material: biaxial stretching polyester (BOPET), thickness are 12 μ m.
Nanomaterial-filled dose of 7.5kg
Host: commercially available host 17.5kg
Curing agent: commercially available curing agent 3.5kg
Solvent: commercially available solvent 70kg
Polyvinylidene chloride emulsion: homemade polyvinylidene chloride emulsion 175kg
Demineralized water: 300kg
Slipping agent: commercially available palm wax slipping agent 3kg
Anti-blocking agent: commercially available silica anti-block 2.5kg
Taking by weighing the above-mentioned polyvinylidene chloride blending emulsion that makes of 175kg adds in the rustless steel container, add successively 3kg palm wax slipping agent, nanomaterial-filled dose of 7.5kg, 2.5kg silica anti-block and 300kg demineralized water while stirring, after stirring the modification polyvinylidene chloride of anti-boiling emulsion, operation to be coated is used.
Take by weighing 17.5kg host, 3.5kg curing agent adds in another rustless steel container, add the 70kg solvent while stirring, it is the generating polyurethane primer after stirring, carry out sided corona treatment after will unreeling as the Biaxially oriented polypropylene base material of base material, by reversing roll-type kiss formula coating method the aqueous polyurethane primer is evenly transferred on the base film, coating weight is 0.3g/m
2, behind far infrared and hot-air seasoning, forming primer layer, and then by reversing the roller kiss-type coating method the above-mentioned modification polyvinylidene chloride of anti-boiling emulsion that makes is evenly transferred on the film primer layer, coating weight is 4.0g/m
2, behind far infrared and hot-air seasoning, forming modified polyvinilidene dichloroethylene coating, coating speed is 200m/min.The primer layer baking temperature is 125 ℃, and be 6 seconds drying time, and modified polyvinilidene dichloroethylene coating baking temperature is 120 ℃, and be 8 seconds drying time.The complete rear rolling of modified polyvinilidene dichloroethylene coated and dried was solidified 2 days under 45 ℃ of conditions, made the polyvinylidene chloride of anti-boiling coated thin film of the present invention.
The anti-boiling coated film of the high resistant oxygen performance that present embodiment makes is as follows
| The anti-conditions of cooking of high resistant oxygen | 121 ℃ of sterilizations half an hour | 135 ℃ of sterilizations half an hour |
| Outward appearance | Transparent | Transparent |
| The coating shedding situation | Do not come off | Do not come off |
| Oxygen permeability (cc/m 2.24hr) | 6.5 | 8.0 |
| Water penetration (g/m 2.24hr) | 9.3 | 10.1 |
| Mist degree (%) | 3.5 | 3.6 |
Annotate: 1) the oxygen flow testing conditions is: 23 ℃, and 0%RH; Permeable testing conditions is: 38 ℃, and 90%RH
Embodiment two
Base material: biaxial stretching polyester (BOPET), thickness are 12 μ m.
Nanomaterial-filled dose of 24kg
Host: commercially available host 20kg
Curing agent: commercially available curing agent 4kg
Solvent: commercially available solvent 80kg
Polyvinylidene chloride emulsion: homemade polyvinylidene chloride emulsion 200kg
Demineralized water: 152kg
Slipping agent: commercially available palm wax slipping agent 4kg
Anti-blocking agent: commercially available silica anti-block 20kg
Taking by weighing the above-mentioned polyvinylidene chloride blending emulsion that makes of 200kg adds in the rustless steel container, add successively 4kg palm wax slipping agent, nanomaterial-filled dose of 24kg, 20kg silica anti-block and 152kg demineralized water while stirring, after stirring the modification polyvinylidene chloride of anti-boiling emulsion, operation to be coated is used.
Take by weighing 20kg host, the 4kg curing agent adds in another rustless steel container, add the 80kg solvent while stirring, it is the generating polyurethane primer after stirring, carry out sided corona treatment after will unreeling as the Biaxially oriented polypropylene base material of base material, by reversing roll-type kiss formula coating method the aqueous polyurethane primer is evenly transferred on the base film, coating weight is 0.3g/m
2, behind far infrared and hot-air seasoning, forming primer layer, and then by reversing the roller kiss-type coating method the above-mentioned modification polyvinylidene chloride of anti-boiling emulsion that makes is evenly transferred on the film primer layer, coating weight is 5.0g/m
2, behind far infrared and hot-air seasoning, forming modified polyvinilidene dichloroethylene coating, coating speed is 250m/min.The primer layer baking temperature is 160 ℃, and be 6 seconds drying time, and modified polyvinilidene dichloroethylene coating baking temperature is 160 ℃, and be 8 seconds drying time.The complete rear rolling of modified polyvinilidene dichloroethylene coated and dried was solidified 2 days under 45 ℃ of conditions, made the polyvinylidene chloride of anti-boiling coated thin film of the present invention.
The anti-boiling coated film of the high resistant oxygen performance that present embodiment makes is as follows
| The anti-conditions of cooking of high resistant oxygen | 121 ℃ of sterilizations half an hour | 135 ℃ of sterilizations half an hour |
| Outward appearance | Transparent | Transparent |
| The coating shedding situation | Do not come off | Do not come off |
| Oxygen permeability (cc/m 2.24hr) | 5.6 | 7.8 |
| Water penetration (g/m 2.24hr) | 9.1 | 10.1 |
| Mist degree (%) | 3.5 | 3.6 |
Annotate: 1) the oxygen flow testing conditions is: 23 ℃, and 0%RH; Permeable testing conditions is: 38 ℃, and 90%RH
Embodiment three
Base material: biaxial stretching polyester (BOPET), thickness are 12 μ m.
Nanomaterial-filled dose of 5kg
Host: commercially available host 8.8kg
Curing agent: commercially available curing agent 1.76kg
Solvent: commercially available solvent 35.2kg
Polyvinylidene chloride emulsion: homemade polyvinylidene chloride emulsion 88kg
Demineralized water: 5.9kg
Slipping agent: commercially available palm wax slipping agent 1kg
Anti-blocking agent: commercially available silica anti-block 0.1kg
Taking by weighing the above-mentioned polyvinylidene chloride blending emulsion that makes of 88kg adds in the rustless steel container, add successively 1kg palm wax slipping agent, nanomaterial-filled dose of 5kg, 0.1kg silica anti-block and 5.9kg demineralized water while stirring, after stirring the modification polyvinylidene chloride of anti-boiling emulsion, operation to be coated is used.
Take by weighing 8.8kg host, 1.76kg curing agent adds in another rustless steel container, add the 35.2kg solvent while stirring, it is the generating polyurethane primer after stirring, carry out sided corona treatment after will unreeling as the Biaxially oriented polypropylene base material of base material, by reversing roll-type kiss formula coating method the aqueous polyurethane primer is evenly transferred on the base film, coating weight is 0.3g/m
2, behind far infrared and hot-air seasoning, forming primer layer, and then by reversing the roller kiss-type coating method the above-mentioned modification polyvinylidene chloride of anti-boiling emulsion that makes is evenly transferred on the film primer layer, coating weight is 2.0g/m
2, behind far infrared and hot-air seasoning, forming modified polyvinilidene dichloroethylene coating, coating speed is 150m/min.The primer layer baking temperature is 100 ℃, and be 6 seconds drying time, and modified polyvinilidene dichloroethylene coating baking temperature is 100 ℃, and be 8 seconds drying time.The complete rear rolling of modified polyvinilidene dichloroethylene coated and dried was solidified 2 days under 45 ℃ of conditions, made the polyvinylidene chloride of anti-boiling coated thin film of the present invention.
The anti-boiling coated film of the high resistant oxygen performance that present embodiment makes is as follows
| The anti-conditions of cooking of high resistant oxygen | 121 ℃ of sterilizations half an hour | 135 ℃ of sterilizations half an hour |
| Outward appearance | Transparent | Transparent |
| The coating shedding situation | Do not come off | Do not come off |
| Oxygen permeability (cc/m 2.24hr) | 6.0 | 8.2 |
| Water penetration (g/m 2.24hr) | 9.6 | 10.2 |
| Mist degree (%) | 3.7 | 3.8 |
Annotate: 1) the oxygen flow testing conditions is: 23 ℃, and 0%RH; Permeable testing conditions is: 38 ℃, and 90%RH
Embodiment four
Base material: biaxial stretching polyester (BOPET), thickness are 12 μ m.
Nanomaterial-filled dose of 25kg
Host: commercially available host 15kg
Curing agent: commercially available curing agent 3kg
Solvent: commercially available solvent 60kg
Polyvinylidene chloride emulsion: homemade polyvinylidene chloride emulsion 150kg
Demineralized water: 275kg
Slipping agent: commercially available palm wax slipping agent 40kg
Anti-blocking agent: commercially available silica anti-block 10kg
Taking by weighing the above-mentioned polyvinylidene chloride blending emulsion that makes of 150kg adds in the rustless steel container, add successively 40kg palm wax slipping agent, nanomaterial-filled dose of 25kg, 10kg silica anti-block and 275kg demineralized water while stirring, after stirring the modification polyvinylidene chloride of anti-boiling emulsion, operation to be coated is used.
Take by weighing 15kg host, the 3kg curing agent adds in another rustless steel container, add the 60kg solvent while stirring, it is the generating polyurethane primer after stirring, carry out sided corona treatment after will unreeling as the Biaxially oriented polypropylene base material of base material, by reversing roll-type kiss formula coating method the aqueous polyurethane primer is evenly transferred on the base film, coating weight is 0.9g/m
2, behind far infrared and hot-air seasoning, forming primer layer, and then by reversing the roller kiss-type coating method the above-mentioned modification polyvinylidene chloride of anti-boiling emulsion that makes is evenly transferred on the film primer layer, coating weight is 3.5g/m
2, behind far infrared and hot-air seasoning, forming modified polyvinilidene dichloroethylene coating, coating speed is 250m/min.The primer layer baking temperature is 160 ℃, and be 6 seconds drying time, and modified polyvinilidene dichloroethylene coating baking temperature is 160 ℃, and be 8 seconds drying time.The complete rear rolling of modified polyvinilidene dichloroethylene coated and dried was solidified 2 days under 45 ℃ of conditions, made the polyvinylidene chloride of anti-boiling coated thin film of the present invention.
The anti-boiling coated film of the high resistant oxygen performance that present embodiment makes is as follows
| The anti-conditions of cooking of high resistant oxygen | 121 ℃ of sterilizations half an hour | 135 ℃ of sterilizations half an hour |
| Outward appearance | Transparent | Transparent |
| The coating shedding situation | Do not come off | Do not come off |
| Oxygen permeability (cc/m 2.24hr) | 5.8 | 8.0 |
| Water penetration (g/m 2.24hr) | 9.4 | 10.0 |
| Mist degree (%) | 3.6 | 3.7 |
Annotate: 1) the oxygen flow testing conditions is: 23 ℃, and 0%RH; Permeable testing conditions is: 38 ℃, and 90%RH
Embodiment five
Base material: biaxial stretching polyester (BOPET), thickness are 12 μ m.
Nanomaterial-filled dose of 4.5kg
Host: commercially available host 25.5kg
Curing agent: commercially available curing agent 5.1kg
Solvent: commercially available solvent 102kg
Polyvinylidene chloride emulsion: homemade polyvinylidene chloride emulsion 255kg
Demineralized water: 1.5kg
Slipping agent: commercially available palm wax slipping agent 24kg
Anti-blocking agent: commercially available silica anti-block 15kg
Taking by weighing the above-mentioned polyvinylidene chloride blending emulsion that makes of 255kg adds in the rustless steel container, add successively 24kg palm wax slipping agent, nanomaterial-filled dose of 4.5kg, 15kg silica anti-block and 1.5kg demineralized water while stirring, after stirring the modification polyvinylidene chloride of anti-boiling emulsion, operation to be coated is used.
Take by weighing 25.5kg host, 5.1kg curing agent adds in another rustless steel container, add the 102kg solvent while stirring, it is the generating polyurethane primer after stirring, carry out sided corona treatment after will unreeling as the Biaxially oriented polypropylene base material of base material, by reversing roll-type kiss formula coating method the aqueous polyurethane primer is evenly transferred on the base film, coating weight is 1.0g/m
2, behind far infrared and hot-air seasoning, forming primer layer, and then by reversing the roller kiss-type coating method the above-mentioned modification polyvinylidene chloride of anti-boiling emulsion that makes is evenly transferred on the film primer layer, coating weight is 4.0g/m
2, behind far infrared and hot-air seasoning, forming modified polyvinilidene dichloroethylene coating, coating speed is 250m/min.The primer layer baking temperature is 160 ℃, and be 6 seconds drying time, and modified polyvinilidene dichloroethylene coating baking temperature is 160 ℃, and be 8 seconds drying time.The complete rear rolling of modified polyvinilidene dichloroethylene coated and dried was solidified 2 days under 45 ℃ of conditions, made the polyvinylidene chloride of anti-boiling coated thin film of the present invention.
The anti-boiling coated film of the high resistant oxygen performance that present embodiment makes is as follows
| The anti-conditions of cooking of high resistant oxygen | 121 ℃ of sterilizations half an hour | 135 ℃ of sterilizations half an hour |
| Outward appearance | Transparent | Transparent |
| The coating shedding situation | Do not come off | Do not come off |
| Oxygen permeability (cc/m 2.24hr) | 5.8 | 7.9 |
| Water penetration (g/m 2.24hr) | 9.3 | 10.1 |
| Mist degree (%) | 3.5 | 3.6 |
Annotate: 1) the oxygen flow testing conditions is: 23 ℃, and 0%RH; Permeable testing conditions is: 38 ℃, and 90%RH
Embodiment six
Base material: biaxial stretching polyester (BOPET), thickness are 12 μ m.
Nanomaterial-filled dose of 9kg
Host: commercially available host 13.5kg
Curing agent: commercially available curing agent 2.7kg
Solvent: commercially available solvent 54kg
Polyvinylidene chloride emulsion: homemade polyvinylidene chloride emulsion 135kg
Demineralized water: 135kg
Slipping agent: commercially available palm wax slipping agent 12kg
Anti-blocking agent: commercially available silica anti-block 9kg
Taking by weighing the above-mentioned polyvinylidene chloride blending emulsion that makes of 135kg adds in the rustless steel container, add successively 12kg palm wax slipping agent, nanomaterial-filled dose of 9kg, 9kg silica anti-block and 135kg demineralized water while stirring, after stirring the modification polyvinylidene chloride of anti-boiling emulsion, operation to be coated is used.
Take by weighing 13.5kg host, 2.7kg curing agent adds in another rustless steel container, add the 54kg solvent while stirring, it is the generating polyurethane primer after stirring, carry out sided corona treatment after will unreeling as the Biaxially oriented polypropylene base material of base material, by reversing roll-type kiss formula coating method the aqueous polyurethane primer is evenly transferred on the base film, coating weight is 1.5g/m
2, behind far infrared and hot-air seasoning, forming primer layer, and then by reversing the roller kiss-type coating method the above-mentioned modification polyvinylidene chloride of anti-boiling emulsion that makes is evenly transferred on the film primer layer, coating weight is 3.0g/m
2, behind far infrared and hot-air seasoning, forming modified polyvinilidene dichloroethylene coating, coating speed is 250m/min.The primer layer baking temperature is 150 ℃, and be 6 seconds drying time, and modified polyvinilidene dichloroethylene coating baking temperature is 150 ℃, and be 8 seconds drying time.The complete rear rolling of modified polyvinilidene dichloroethylene coated and dried was solidified 2 days under 45 ℃ of conditions, made the polyvinylidene chloride of anti-boiling coated thin film of the present invention.
The anti-boiling coated film of the high resistant oxygen performance that present embodiment makes is as follows
| The anti-conditions of cooking of high resistant oxygen | 121 ℃ of sterilizations half an hour | 135 ℃ of sterilizations half an hour |
| Outward appearance | Transparent | Transparent |
| The coating shedding situation | Do not come off | Do not come off |
| Oxygen permeability (cc/m 2.24hr) | 5.9 | 8.3 |
| Water penetration (g/m 2.24hr) | 9.6 | 10.2 |
| Mist degree (%) | 3.6 | 3.8 |
Annotate: 1) the oxygen flow testing conditions is: 23 ℃, and 0%RH; Permeable testing conditions is: 38 ℃, and 90%RH
Embodiment seven
Base material: biaxial stretching polyester (BOPET), thickness are 12 μ m.
Nanomaterial-filled dose of 12kg
Host: commercially available host 10kg
Curing agent: commercially available curing agent 2kg
Solvent: commercially available solvent 40kg
Polyvinylidene chloride emulsion: homemade polyvinylidene chloride emulsion 100kg
Demineralized water: 70kg
Slipping agent: commercially available palm wax slipping agent 16kg
Anti-blocking agent: commercially available silica anti-block 2kg
Taking by weighing the above-mentioned polyvinylidene chloride blending emulsion that makes of 100kg adds in the rustless steel container, add successively 16kg palm wax slipping agent, nanomaterial-filled dose of 12kg, 2kg silica anti-block and 70kg demineralized water while stirring, after stirring the modification polyvinylidene chloride of anti-boiling emulsion, operation to be coated is used.
Take by weighing 10kg host, the 2kg curing agent adds in another rustless steel container, add the 40kg solvent while stirring, it is the generating polyurethane primer after stirring, carry out sided corona treatment after will unreeling as the Biaxially oriented polypropylene base material of base material, by reversing roll-type kiss formula coating method the aqueous polyurethane primer is evenly transferred on the base film, coating weight is 0.5g/m
2, behind far infrared and hot-air seasoning, forming primer layer, and then by reversing the roller kiss-type coating method the above-mentioned modification polyvinylidene chloride of anti-boiling emulsion that makes is evenly transferred on the film primer layer, coating weight is 0.8g/m
2, behind far infrared and hot-air seasoning, forming modified polyvinilidene dichloroethylene coating, coating speed is 80m/min.The primer layer baking temperature is 80 ℃, and be 6 seconds drying time, and modified polyvinilidene dichloroethylene coating baking temperature is 80 ℃, and be 8 seconds drying time.The complete rear rolling of modified polyvinilidene dichloroethylene coated and dried was solidified 2 days under 45 ℃ of conditions, made the polyvinylidene chloride of anti-boiling coated thin film of the present invention.
The anti-boiling coated film of the high resistant oxygen performance that present embodiment makes is as follows
| The anti-conditions of cooking of high resistant oxygen | 121 ℃ of sterilizations half an hour | 135 ℃ of sterilizations half an hour |
| Outward appearance | Transparent | Transparent |
| The coating shedding situation | Do not come off | Do not come off |
| Oxygen permeability (cc/m 2.24hr) | 6.2 | 8.5 |
| Water penetration (g/m 2.24hr) | 10.0 | 10.5 |
| Mist degree (%) | 3.8 | 4.0 |
Annotate: 1) the oxygen flow testing conditions is: 23 ℃, and 0%RH; Permeable testing conditions is: 38 ℃, and 90%RH.
Claims (15)
1. the high resistant oxygen polyvinylidene chloride of anti-boiling coated thin film, comprise the primer layer between dope layer, dope layer and the base material of base material and substrate surface, described base material film is biaxially oriented polyester film, thickness is 8-120 μ m, described primer layer is that aqueous polyurethane or solvent borne polyurethane add the coating that solvent forms, and the coating weight of primer layer is 0.3-1.5g/m
2It is characterized in that: described dope layer is the high resistant oxygen polyvinylidene chloride of anti-boiling coating that is formed after primer layer surface and oven dry by the high resistant oxygen polyvinylidene chloride of anti-boiling latex-coating that the present invention makes by modification, the described high resistant oxygen polyvinylidene chloride of anti-boiling latex is formulated by the raw material that contains following weight content: the high resistant oxygen polyvinylidene chloride of anti-boiling blending emulsion 30-88%, nanomaterial-filled dose of 1.5-6%, slipping agent 1-8%, antitack agent 0.1-5%, 5-60% demineralized water; The described high resistant oxygen polyvinylidene chloride of anti-boiling blending emulsion is made by the raw material that contains following weight content: the vinylidene of 40-94%, the esters of acrylic acid of 1.5-10% and the acrylic acid of 1-6% and acrylonitrile mixed liquor or among both any one, the initator of 0.5-2%, the emulsifying agent of 0.1-0.8%, the stabilizing agent of 0.5-1%, 0-55% soft water.
2. the high resistant oxygen polyvinylidene chloride of anti-boiling coated thin film as claimed in claim 1, it is characterized in that: the described high resistant oxygen polyvinylidene chloride of anti-boiling latex, solid content is preferably 45-55%.
3. any one high resistant oxygen polyvinylidene chloride of anti-boiling coated thin film as claimed in claim 1 or 2, it is characterized in that: the coating weight of described dope layer is 0.8-5.0g/m
2
4. such as described any one high resistant oxygen polyvinylidene chloride of anti-boiling coated thin film of claim 1-3, it is characterized in that: described nanomaterial-filled dose is in CaCO3, TiO2, mica, the imvite any one.
5. such as described any one high resistant oxygen polyvinylidene chloride of anti-boiling coated thin film of claim 1-3, it is characterized in that: described esters of acrylic acid is methyl methacrylate.
6. such as described any one high resistant oxygen polyvinylidene chloride of anti-boiling coated thin film of claim 1-3, it is characterized in that: described initator is sodium peroxydisulfate.
7. such as described any one high resistant oxygen polyvinylidene chloride of anti-boiling coated thin film of claim 1-3, it is characterized in that: described emulsifying agent is neopelex.
8. such as described any one high resistant oxygen polyvinylidene chloride of anti-boiling coated thin film of claim 1-3, it is characterized in that: described emulsifying agent is neopelex.
9. such as described any one high resistant oxygen polyvinylidene chloride of anti-boiling coated thin film of claim 1-3, it is characterized in that: described stabilizing agent is the J-1 stabilizing agent.
10. such as described any one high resistant oxygen polyvinylidene chloride of anti-boiling coated thin film of claim 1-9, it is characterized in that: described slipping agent is the palm wax slipping agent.
11. such as described any one high resistant oxygen polyvinylidene chloride of anti-boiling coated thin film of claim 1-9, it is characterized in that: described antitack agent is the silica anti-blocking agent.
12. the manufacture method of the high resistant oxygen polyvinylidene chloride of anti-boiling coated thin film as claimed in claim 1 is characterized in that the method comprises the steps:
(1) elder generation adds the soft water of 0-55% successively in reactor, the initator sodium peroxydisulfate of 0.5-2%, the J-1 stabilizing agent of 0.5-1% and the vinylidene of 40-94%, then vacuumize--adding nitrogen--row pressure-vacuumize-Jia nitrogen-row pressure, finish half operation twice, pressure is controlled to be-0.08Mpa, mixing speed is 60-180 rev/min, intensification is controlled in the 50-85 ℃ of scope temperature, fully stirred 30-60 minute, vinylidene is dissolved fully, obtain seed emulsion, drip the 1.5-10% methyl methacrylate, 1-6% acrylic acid, the neopelex of 1-6% acrylonitrile and 0.1-0.8%, rate of addition 5-15 gram/minute is warming up to 90 ℃ and continues to keep 30-90 minute after dripping, whole system is fully reacted, be cooled at last normal temperature and pressure, make the high resistant oxygen polyvinylidene chloride of anti-boiling blending emulsion;
(2) in rustless steel container, add the above-mentioned high resistant oxygen polyvinylidene chloride of anti-boiling blending emulsion that makes, stirred 20-40 minute, speed 60-200 rev/min, temperature is controlled in the 40-50 ℃ of scope, then add nanomaterial-filled dose of 1.5-6%, and then improve temperature of reaction kettle to 55-60 ℃, the interior material of reactor is fully mixed, while stirring the palm wax slipping agent that adds successively 1-8%, the silica anti-block of 0.1-5% and the demineralized water of 5-60%, after stirring the high resistant oxygen polyvinylidene chloride of anti-boiling latex, operation to be coated is used;
(3) polyurethane adhesive host and the curing agent ratio in 5: 1 is added in another rustless steel container successively, add solvent dilution while stir, solvent proportion is 4 times of host, can form primer after stirring, and next process to be entered uses;
(4) unwinding tension being set is 2-6bar, and base film is carried out sided corona treatment, with coating apparatus primer evenly is coated with and oven dry on the substrate surface after the sided corona treatment, and coating speed is 80-250 m/min, and the primary coat coating weight is controlled at 0.2-1.5g/m
2,Bake out temperature is 80-160 ℃, and be 6 seconds drying time, after cooling, through coating apparatus the high resistant oxygen polyvinylidene chloride of anti-boiling emulsion uniform that above-mentioned steps 2 makes is coated on the primer again, and coating weight is controlled to be 0.8-4.5g/m
2Then the film of coating being finished is dried, coating speed is 80-250 m/min, bake out temperature is 80-160 ℃, drying time 8 seconds, the complete rear rolling of the high resistant oxygen polyvinylidene chloride of anti-boiling coated and dried, the winding tension rate of decay is 40-55%, coated film volume is placed under 45 ℃ of conditions and solidified 2 days, makes the high resistant oxygen polyvinylidene chloride of anti-boiling coated thin film of the present invention.
13. the manufacture method of the high resistant oxygen polyvinylidene chloride of anti-boiling coated thin film as claimed in claim 12 is characterized in that: described drying mode adopts hot-air seasoning.
14. the manufacture method of the high resistant oxygen polyvinylidene chloride of anti-boiling coated thin film as claimed in claim 12 is characterized in that: described drying mode adopts the Far-infrared Heating oven dry.
15. the manufacture method of the high resistant oxygen polyvinylidene chloride of anti-boiling coated thin film as claimed in claim 12 is characterized in that: described drying mode employing hot blast adds the Far-infrared Heating mode dries.
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| CN103275260A (en) * | 2013-05-13 | 2013-09-04 | 浙江科冠聚合物有限公司 | Preparation method of acrylic plastic-plastic composite latex |
| CN103626909A (en) * | 2013-12-02 | 2014-03-12 | 苏州福斯特光伏材料有限公司 | Polyvinylidene chloride (PVDC) emulsion and preparation method thereof as well as weather-proof barrier coating and application thereof |
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| CN105482572A (en) * | 2014-10-09 | 2016-04-13 | 南通瑞普埃尔生物工程有限公司 | Preparation method of PVDC latex for egg freshness retaining coating |
| CN105820304A (en) * | 2016-05-18 | 2016-08-03 | 常德市金润新材料科技有限公司无锡新材料研究院 | High-barrier PVDC emulsion for paper and preparation method of emulsion |
| CN105820304B (en) * | 2016-05-18 | 2018-11-30 | 常德市金润新材料科技有限公司 | A kind of high barrier paper PVDC lotion and preparation method thereof |
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| CN106366322A (en) * | 2016-08-27 | 2017-02-01 | 合肥普庆新材料科技有限公司 | Preparation method of waterborne epoxy cationic emulsion for preparing waterborne epoxy steaming and boiling resistant coating |
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| CN108164729B (en) * | 2017-12-21 | 2019-11-01 | 海南赛诺实业有限公司 | It is a kind of to be suitble to light-weight packed low-temperature heat-sealing coated film and its manufacturing method |
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Denomination of invention: High-oxygen resistant steaming-resistant polyvinylidene chloride coating film and manufacturing method thereof Effective date of registration: 20181225 Granted publication date: 20150429 Pledgee: China Construction Bank Co., Ltd. Haikou Daying Shan Branch Pledgor: Hai'nan Sainuo Industry Co., Ltd. Registration number: 2018460000012 |
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Date of cancellation: 20190213 Granted publication date: 20150429 Pledgee: China Construction Bank Co., Ltd. Haikou Daying Shan Branch Pledgor: Hai'nan Sainuo Industry Co., Ltd. Registration number: 2018460000012 |
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Denomination of invention: High-oxygen resistant steaming-resistant polyvinylidene chloride coating film and manufacturing method thereof Effective date of registration: 20190702 Granted publication date: 20150429 Pledgee: China Construction Bank Co., Ltd. Haikou Daying Shan Branch Pledgor: Hai'nan Sainuo Industry Co., Ltd. Registration number: 2019460000008 |
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Date of cancellation: 20201201 Granted publication date: 20150429 Pledgee: China Construction Bank Co.,Ltd. Haikou Daying Shan Branch Pledgor: HAINAN SHINER INDUSTRIAL Co.,Ltd. Registration number: 2019460000008 |