CN103059785A - Heat resistant type transparent polyolefin hot melt adhesive and preparing method thereof - Google Patents
Heat resistant type transparent polyolefin hot melt adhesive and preparing method thereof Download PDFInfo
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Abstract
The invention discloses heat resistant type transparent polyolefin hot melt adhesive and a preparing method thereof. The Heat resistant type transparent polyolefin hot melt adhesive comprises 1) resin, 2) radical initiator, and 3) grafting monomer by weight. The resin includes by weight 70-99% of ethylene-1-octylenecopolymer, 0-5 % of ethylene homopolymer and 1-30 % of ethylene-propylene-1-butene amorphous copolymer. The dosage of the radical initiator covers 0.01-10% of the total mass of the resin. And the grafting monomer covers 0.1-10% of the total mass of the resin. After the components are premixed evenly, a melt grafting reaction is carried out at the temperature of 160-200 DEG C with a double-screw extruder. Then the granulous, sheet and membranaceous hot melt adhesive is manufactured by cooling through the device, pelleting through a pelletizer, shaping into a granulous shape through a vulcanization mechanism. The hot melt adhesive not only has excellent electrical insulation property, optical property, heat resistance property and adhesive property, but also maintains the physical property, chemical stability and good machinability of the polyolefin materials.
Description
Technical field
The present invention relates to the hot melt adhesive material field, be specifically related to a kind of heat resistant type transparency polyolefin hot melt adhesive and preparation method thereof.
Background technology
Polyolefine material is take polyethylene (PE), polypropylene (PP) as main, it is the maximum kind of commodity polymer material, it has excellent physicals, chemical stability, good processibility, can recycle, and has good electrical insulation capability, be widely used in the fields such as packaging industry, automotive industry, electronic industry, development along with science and technology, the structurizing of product, functionalization are more aobvious important, simple single layer structure can not satisfy service requirements, needs that multilayer material or a plurality of structure unit are bonding could to satisfy performance requriements.For electronics industry, glue often bond conductive component and non-conductive parts or another one conductive component, this just has high requirements to the electrical insulation capability of glue, polarity hot-fusible high-molecular glue has very high adhesive property, but there is hidden danger in its electrical insulation capability, in electron device, use this hot melt adhesive, the phenomenon that short circuit and energy waste run off probably occurs, so this field more needs the polyolefin hot-melt of the higher nonpolar structure of electrical insulating property.Simultaneously, because polyolefinic nonpolar structure, its water vapor barrier property, weather-proof and ageing-resistant performance is all more excellent more is applicable under the physical environment such as outdoor, high humidity.
At present, polyolefin hot-melt is mainly bonding to realize by grafting of polar monomers, it can be multiple polyolefinic mixture, if the application scenario requires polyolefin hot-melt to have certain thermotolerance, then multiselect is main as matrix resin with PE, PP, because PE, PP have high crystalline, light is different from non-crystalline region in the specific refractory power of crystalline region, and resin is creamy white, and is translucent even not transparent, the transmittance of the most transparent PE raw material only is 65%, so this hot melt adhesive does not have preferably optical property; If the application scenario requires polyolefin hot-melt to have certain light transmission, then multiselect is with the higher polyolefin elastomer of transmittance (POE), flexible octene segment has replaced part ethene segment in this resin, whole degree of crystallinity reduces, improved to a certain extent the adhesive property of composition, a kind of novel polyolefin packaging glue film composite and application thereof are disclosed in patent application CN201110449535.3 before such as the applicant, said composition specifically comprises ethylene-octene copolymer, polyethylene, ethylene-methyl methacrylate methyl terpolymer, and linking agent, the composition that oxidation inhibitor and UV stabilizer form.But the fusing point of said composition is low, is lower than generally speaking 60 ℃, and therefore poor heat resistance has limited its range of application.
Summary of the invention
Defective in view of prior art, the object of the present invention is to provide a kind of heat resistant type transparency polyolefin hot melt adhesive, make it not only have excellent electrical insulation capability and optical property, and good thermotolerance and adhesive property, and can also keep physicals, chemical stability and the good processibility of polyolefine material excellence.
Another object of the present invention is to provide a kind of preparation method of heat resistant type transparency polyolefin hot melt adhesive.
The technical solution adopted in the present invention is as follows for achieving the above object:
A kind of heat resistant type transparency polyolefin hot melt adhesive, it comprises following component by weight percentage:
A) resin
Ethene-1-octene copolymer 70-99%
Alathon 0-5%
Ethylene-propylene-1-butylene amorphous copolymer 1-30%;
B) radical initiator, its consumption accounts for the 0.01-0.7% of resin total mass;
C) grafted monomer accounts for the 0.1-10% of total resin weight.
Grafted monomer described in the present invention is the compound that contains alkene functional group or epoxy-functional, can be grafted to the polar monomer that the resin macromole gets on by addition or ring-opening reaction, preferably, described grafted monomer is γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-glycidoxypropyltrietandysilane andysilane, γ-(methacryloxy) propyl trimethoxy silicane, γ-sulfydryl propyl-triethoxysilicane, vinyltrimethoxy silane, vinyltriethoxysilane, vinyl-acetic ester, tertiary ethylene carbonate, propionate, vinyl butyrate, the toxilic acid vinyl acetate, maleic anhydride, itaconic anhydride, citraconic anhydride, the allyl group succinyl oxide, hexamethylene-4-alkene-1, the 2-dicarboxylic anhydride, 4-methylene radical hexamethylene-4-alkene-1, the 2-dicarboxylic anhydride, dicyclo [2.2.1] heptan-5-alkene-2, the 3-dicarboxylic anhydride, x-methyl bicycle [2.2.1] heptan-5-alkene-2, the 3-dicarboxylic anhydride, glycidyl allyl ether, vinyl glycidyl ether, the toxilic acid glycidyl ester, glycidyl itoconate, glycidyl acrylate, glycidyl methacrylate, 2-tetrahydrobenzene-1-base glycidyl ether, tetrahydrobenzene-4,5-diglycidyl carboxylicesters, tetrahydrobenzene-4-glycidyl carboxylicesters, 5-norbornylene-2-methyl-2-glycidyl carboxylicesters, in-cis-dicyclo [2.2.1] heptan-5-alkene-2, one or more mixing in the 3-diglycidyl dicarboxylic ester.The purpose of grafted monomer and effect are by polyfunctional compound being grafted on the matrix resin to improve matrix resin to the cohesive strength of different substrate materials.
In order to guarantee that this hot melt adhesive has excellent transmittance, matrix resin is take ethene/1-octene copolymer (POE) as main, and in the preferred scheme of the present invention, the molar content of octene is 20-50% in described ethene/1-octene copolymer, fusing point is 40-80 ℃, and weight-average molecular weight is 7000-9000.Can not only guarantee under this parameter that the transmittance of POE can also improve the flowability of composition, be beneficial to processing.
In order to improve the thermotolerance of hot melt adhesive on the basis of matrix resin, in the preferred scheme, described Alathon (PE) density is 0.90-0.95g/cm
3, fusing point is 80-150 ℃.Because it belongs to the high crystalline material, addition too much can cause the decline of hot melt adhesive transmittance, thus its consumption must be controlled at 5% and below; If but the consumption of Alathon cross low or do not add Alathon, can cause again the thermotolerance of polymkeric substance not reach the requirement of application.Thermotolerance and light transmission for balance PE-POE binary system, the applicant finds ethylene-propylene-this terpolymer of 1-butylene amorphous copolymer, because the crystallization of propylene tendency will be higher than ethene, so crystallite district of the easier formation some amount of propylene segment in this polymkeric substance, this crystallite district is at the inner physical support point that plays a part of polymkeric substance, make polymkeric substance a high-temperature fusion peak near 110 ℃, occur, thereby can improve the thermotolerance of polymkeric substance, simultaneously because zone, crystalline region and ratio are little, so that this polymkeric substance has high transmittance.Therefore, add ethylene-propylene-1-butylene amorphous copolymer among the present invention with the Substitute For Partial Alathon, thermotolerance and light transmission that can balance PE-POE binary system make its two kinds of performances all reach optimum.But because the molecular weight of this polymkeric substance is not high, do not have enough intensity, therefore unaffected for the mechanical property that guarantees hot melt adhesive, its consumption is controlled between the 1-30%.In the preferred scheme of the present invention, the density of described ethylene-propylene-1-butylene amorphous copolymer is 0.85-0.91g/cm
3, ring and ball softening point is 80-140 ℃.
Thermotolerance and light transmission for further this polyolefin hot-melt of balance, the present invention can add fusing point other polyolefin plastomers (POP) part high than POE and replace POE, POE is different owing to monomer content when synthetic with POP, has similar structures, but the thermotolerance of POP is better, therefore the adding of POP can under the prerequisite of the transmittance that does not reduce mixture, further improve its thermotolerance.Because the POP resin is not easy grafting, so it can not replace the POE use fully.The weight percentage of the polyolefin plastomers of adding among preferred the present invention is 5-20%.
In order to make polyolefin resin have cohesiveness, cause resin macromolecular radical grafting of polar monomers group, initiator of the present invention is selected radical initiator.Preferably, the radical initiator that adopts among the present invention is 3, two (tert-pentyl peroxide) ethyl butyrates, 4 of 3-, two (t-butyl peroxy) n-butyl pentanoates, 1 of 4-, two (t-butyl peroxy)-3 of 1-, 5,5-trimethyl-cyclohexane, 2,5,-dimethyl-2,5-is two-(t-butyl peroxy)-3-hexin, di-t-butyl peroxide, peroxidation two tert-pentyls, tert-butyl peroxide isopropyl benzene, two-(t-butyl peroxy sec.-propyl) benzene, 2, and 5-dimethyl-2,5-is two-one or more mixing in (t-butyl peroxy) hexane, dicumyl peroxide.
In the preferred scheme, heat resistant type transparency polyolefin hot melt adhesive of the present invention also comprises one or more in free radical activator, chainextender, fire retardant, uv-absorbing agent, photostabilizer, oxidation inhibitor, softening agent, tinting material or the white dyes.Wherein, the free radical activator can play the effect of Nitroxyl stable radical, prolong radical life, reduce between the macromolecular radical because the DeR degree that coupling stops the crosslinking reaction degree that occurs and ruptures and occur owing to β the raising grafting efficiency.This free radical activator is to contain that alkene can be rolled into a ball or the compound of active H, be preferably one of following or two or more mixture wherein: triallyl isocyanate, triallyl cyanate, Ethylene glycol dimethacrylate, a phenyl bismaleimides, Viscoat 295, trimethylolpropane trimethacrylate, phthalic acid diisopropyl alkene ester, 1,2-polyhutadiene, ethidine polybutene.In order further to prolong its work-ing life, can add uv-absorbing agent and photostabilizer.Described uv-absorbing agent is selected from benzophenone and benzotriazole category, is preferably one of following or two or more mixture wherein: 2-(2'-hydroxyl-uncle's 5'-octyl phenyl) benzotriazole, 2-hydroxyl-4 (2'-hydroxyl-3'-acryloxy propoxy-) benzophenone, Octabenzone, 2-(2'-hydroxyl-5'-aminomethyl phenyl) benzotriazole, N-(2-ethylphenyl)-the N'-(2-ethoxyl phenenyl) oxalic acid diamide, 2-(2'-hydroxyl-uncle's 5'-octyl phenyl) benzotriazole.Described photostabilizer is selected from hindered amines, is preferably one of following or two or more mixture wherein: 2,2,6,6-tetramethyl--4-pyridine alcohol fatty acid ester, two (2,2,6,6-tetramethyl--4-piperidyl) sebate, Succinic Acid and 4-hydroxyl-2,2,6,6-tetramethyl--the polymkeric substance of 1-piperidines ethanol, 4-benzoyloxy-2,2,6,6-tetramethyl piperidine.In order to prevent the transition thermooxidative degradation jaundice of composition in the blending extrusion process, the present invention can add oxidation inhibitor, and described oxidation inhibitor is selected from Hinered phenols antioxidant, suffocated amine antioxidant, phosphite ester kind antioxidant and thioether kind antioxidant; Preferred Hinered phenols antioxidant and phosphite ester kind antioxidant are also used.The present invention can also add softening agent to improve the processing rheological, enhances productivity, and preferred described softening agent is selected from paraffin mineral oil and aromatic mineral oil, preferred paraffin mineral oil; They can also improve composition to the wetting property of bonded thing, further improve adhesive property.Heat resistant type transparency polyolefin hot melt adhesive of the present invention also can add physics or the mechanical property that chainextender, fire retardant, tinting material or white dyes change hot melt adhesive.
Monomer-grafted method of the present invention can use method known to those skilled in the art to carry out.Such as solution grafting or melt grafting etc.
A kind of preparation method of heat resistant type transparency polyolefin hot melt adhesive, it may further comprise the steps:
According to the above-mentioned component of the present invention and consumption with each component premix evenly after; use twin screw extruder under 160-200 ℃, to carry out melting graft reaction; then by device cooling, through the dicing machine granulation, re-use vulcanizer and make granular, sheet and membranaceous hot melt adhesive.
With respect to prior art, beneficial effect of the present invention is: polyolefin hot-melt of the present invention can be realized effectively bonding, excellent electrical insulation capability and optical property, have good thermotolerance and light transmission, and kept physicals, chemical stability and the good processibility of polyolefine material excellence.Can satisfy the service requirements of electronic equipment display screen and the fields such as view port, solar module, mobile phone and tablet personal computer display screen (may under hot and humid environment, use) under the electronic display of outdoor application and decoration, the high-temperature operation environment.
Below in conjunction with concrete embodiment the present invention is described in further detail.
Embodiment
It below is the preferred embodiment of the invention.
Raw material of the present invention comprises:
The ethene that polyolefin elastomer (A) is produced for DOW/1-octene copolymer elastomerics POE, commodity are called Engage 8137;
The LLDPE that Alathon (B) is produced for limited-liability company of China Petrochemical Industry, commodity are called DFDA-2001;
Ethylene/propene/1-butylene amorphous copolymer (C) is produced for Evonik, and commodity are called VESTOPLAST 750;
The polyolefin plastomers POP that polyolefin plastomers (D) is produced for DOW, commodity are called AFFINITY 1140G;
Above-mentioned raw materials is according to following steps machine-shaping: with each component premix evenly after, use twin screw extruder under 160-200 ℃, to carry out melting graft reaction, then by the device cooling, through the dicing machine granulation, re-use vulcanizer and suppress 0.5 membranaceous hot melt adhesive.The concrete prescription of embodiment 1-9 sees Table 1.
Table 1: resin proportioning (weight percent) in each example
| Composition/% | 1 | 2 | 3 | 4 | 5 | 6 | 7 | 8 | 9 |
| A | 70 | 85 | 98 | 70 | 80 | 75 | 70 | 65 | 70 |
| B | 5 | 3 | 0 | -- | - | - | - | - | - |
| C | 25 | 12 | 2 | 10 | 10 | 15 | 20 | 30 | 25 |
| D | - | - | - | 20 | 10 | 10 | 10 | 10 | 5 |
| Two (t-butyl peroxy) n-butyl pentanoates of 4,4- | 0.2 | 0.3 | 0.1 | 0.1 | 0.3 | 0.05 | 0.3 | 0.2 | 0.2 |
| Maleic anhydride | 3 | 2.5 | 2 | 1 | 1.5 | 2 | - | - | - |
| Vinyltriethoxysilane | - | - | - | - | - | - | 4 | - | - |
| Vinyl-acetic ester | - | - | - | - | - | - | - | 2.5 | - |
| Glycidyl methacrylate | - | - | - | - | - | - | - | - | 8 |
| Triallyl isocyanate | - | - | - | - | - | 1 | 1.5 | 0.8 | 1 |
| Four (3,5-di-t-butyl-4-hydroxyl) phenylpropionic acid pentaerythritol ester (Hinered phenols antioxidant) | 0.3 | 0.3 | 0.2 | 0.2 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 |
| Three (2,4-di-t-butyl) phenyl-phosphites (phosphite ester kind antioxidant) | 0.1 | 0.1 | 0.1 | 0.1 | - | - | - | - | - |
| 2-(2'-hydroxyl-uncle's 5'-octyl phenyl) benzotriazole | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
| Succinic Acid and 4-hydroxyl-2,2,6, the polymkeric substance of 6-tetramethyl--1-piperidine alcohols | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 | 0.1 |
Performance test
1. adhesive property
Press the GB/T8808-88 test method, polyolefine packaging adhesive film among test the present invention and the cohesive force of different substrate materials, wherein the hot melt adhesive film of embodiment 1-6 is tested adhesive property at aluminium flake, the hot melt adhesive film of embodiment 7 is at glass on-chip testing adhesive property, the hot melt adhesive film of embodiment 8 is tested adhesive property at the PE film, and the hot melt adhesive film of embodiment 9 is tested adhesive property at the PET film.
2. testing vapor transmission
Packaging adhesive film after the process heated lamination, is tested by standard GB/T 21529-2008 in laminating machine, adopted the electrolytic sensors method to measure water vapor transmittance (WVTR), test condition is 38 ℃, 90% relative humidity.
3. volume specific resistance
Packaging adhesive film after the process heated lamination, is pressed standard GB/T1410-2006 test volume resistivity in laminating machine.Test voltage is 100V, and the test duration is 120s.
With the packaging adhesive film that above-described embodiment obtains, test as stated above its adhesive property, transmittance, water vapor transmittance and volume specific resistance, test result sees Table 2.
Table 2: the traditional performance of each example
The result of table 2 shows: adopt the present invention program's heat resistant type transparency polyolefin hot melt adhesive, have excellent optical property, electrical insulation capability and water vapor rejection performance, by grafting opposed polarity monomer, can realize effectively bonding to different substrate materials.
4. creep test
With the packaging adhesive film multiple-layer stacked in laminating machine through after the heated lamination, being made into the test department bit width is 4mm, and thickness is the dumbbell shape sample of 2mm, by standard GB/T 11546.1-2008 test tensile creep strain (%), test load is 10N, and test result sees Table 3.
Table 3: the tensile creep strain result of each example
The result of table 3 shows: adopt the present invention program's heat resistant type transparency polyolefin hot melt adhesive, still have very excellent creep strength under 110 ℃ high temperature, have certain thermotolerance, satisfy service requirements.
These tests show that polyolefin hot-melt of the present invention can realize excellent electrical insulation capability and optical property, have certain thermotolerance and adhesive property, and have kept physicals, chemical stability and the good processibility of polyolefine material excellence.Can satisfy the service requirements of electronic equipment display screen and the fields such as view port, solar module, mobile phone and tablet personal computer display screen (may under hot and humid environment, use) under the electronic display of outdoor application and decoration, the high-temperature operation environment.Therefore, the solution of the present invention has obvious superiority.
Above-mentioned embodiment only is preferred implementation of the present invention; can not limit the scope of protection of the invention with this, the variation of any unsubstantiality that those skilled in the art does on basis of the present invention and replacement all belong to the present invention's scope required for protection.
Claims (9)
1. heat resistant type transparency polyolefin hot melt adhesive, it is characterized in that: it comprises following component by weight percentage
A) resin comprises:
Ethene-1-octene copolymer 70-99%
Alathon 0-5%
Ethylene-propylene-1-butylene amorphous copolymer 1-30%;
B) radical initiator, its consumption accounts for the 0.01-0.7% of resin total mass;
C) grafted monomer, its consumption accounts for the 0.1-10% of total resin weight.
2. heat resistant type transparency polyolefin hot melt adhesive according to claim 1, it is characterized in that: described resin also comprises the polyolefin plastomers of 5-20%.
3. heat resistant type transparency polyolefin hot melt adhesive according to claim 1, it is characterized in that: described grafted monomer is γ-glycidyl ether oxygen propyl trimethoxy silicane, γ-glycidoxypropyltrietandysilane andysilane, γ-(methacryloxy) propyl trimethoxy silicane, γ-sulfydryl propyl-triethoxysilicane, vinyltrimethoxy silane, vinyltriethoxysilane, vinyl-acetic ester, tertiary ethylene carbonate, propionate, vinyl butyrate, the toxilic acid vinyl acetate, maleic anhydride, itaconic anhydride, citraconic anhydride, the allyl group succinyl oxide, hexamethylene-4-alkene-1, the 2-dicarboxylic anhydride, 4-methylene radical hexamethylene-4-alkene-1, the 2-dicarboxylic anhydride, dicyclo [2.2.1] heptan-5-alkene-2, the 3-dicarboxylic anhydride, x-methyl bicycle [2.2.1] heptan-5-alkene-2, the 3-dicarboxylic anhydride, glycidyl allyl ether, vinyl glycidyl ether, the toxilic acid glycidyl ester, glycidyl itoconate, glycidyl acrylate, glycidyl methacrylate, 2-tetrahydrobenzene-1-base glycidyl ether, tetrahydrobenzene-4,5-diglycidyl carboxylicesters, tetrahydrobenzene-4-glycidyl carboxylicesters, 5-norbornylene-2-methyl-2-glycidyl carboxylicesters, in-cis-dicyclo [2.2.1] heptan-5-alkene-2, one or more mixing in the 3-diglycidyl dicarboxylic ester.
4. heat resistant type transparency polyolefin hot melt adhesive according to claim 1, it is characterized in that: the molar content of octene is 20-50% in described ethene/1-octene copolymer, and fusing point is 40-80 ℃, and weight-average molecular weight is 7000-9000.
5. heat resistant type transparency polyolefin hot melt adhesive according to claim 1, it is characterized in that: described Alathon density is 0.90-0.95g/cm
3, fusing point is 80-150 ℃.
6. heat resistant type transparency polyolefin hot melt adhesive according to claim 1, it is characterized in that: the density of described ethylene-propylene-1-butylene amorphous copolymer is 0.85-0.91g/cm
3, ring and ball softening point is 80-140 ℃.
7. heat resistant type transparency polyolefin hot melt adhesive according to claim 1, it is characterized in that: described radical initiator is 3, two (tert-pentyl peroxide) ethyl butyrates of 3-, 4, two (t-butyl peroxy) n-butyl pentanoates of 4-, 1, two (t-butyl peroxy)-3 of 1-, 5, the 5-trimethyl-cyclohexane, 2,5,-dimethyl-2,5-pair-(t-butyl peroxy)-3-hexin, di-t-butyl peroxide, peroxidation two tert-pentyls, the tert-butyl peroxide isopropyl benzene, two-(t-butyl peroxy sec.-propyl) benzene, 2,5-dimethyl-2,5-pair-(t-butyl peroxy) hexane, one or more mixing in the dicumyl peroxide.
8. heat resistant type transparency polyolefin hot melt adhesive according to claim 1, it is characterized in that: it also comprises in free radical activator, chainextender, fire retardant, uv-absorbing agent, photostabilizer, oxidation inhibitor, softening agent, tinting material or the white dyes one or more.
9. the preparation method of a heat resistant type transparency polyolefin hot melt adhesive is characterized in that it may further comprise the steps:
According to claim 1 with each component premix evenly after, use twin screw extruder under 160-200 ℃, to carry out melting graft reaction, then by the device cooling, through the dicing machine granulation, re-use vulcanizer and be pressed into granular, sheet and membranaceous hot melt adhesive.
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