CN102051149A - Preparation methods of hot melt pressure-sensitive adhesive and protective film as well as hot melt pressure-sensitive adhesive - Google Patents
Preparation methods of hot melt pressure-sensitive adhesive and protective film as well as hot melt pressure-sensitive adhesive Download PDFInfo
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- CN102051149A CN102051149A CN 201010560902 CN201010560902A CN102051149A CN 102051149 A CN102051149 A CN 102051149A CN 201010560902 CN201010560902 CN 201010560902 CN 201010560902 A CN201010560902 A CN 201010560902A CN 102051149 A CN102051149 A CN 102051149A
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- hot melt
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- 239000012943 hotmelt Substances 0.000 title claims abstract description 43
- 230000001681 protective effect Effects 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 239000004698 Polyethylene Substances 0.000 claims abstract description 22
- 229920000573 polyethylene Polymers 0.000 claims abstract description 21
- 239000000463 material Substances 0.000 claims abstract description 20
- 229920002725 thermoplastic elastomer Polymers 0.000 claims abstract description 16
- -1 polyethylene Polymers 0.000 claims abstract description 12
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 239000011248 coating agent Substances 0.000 claims abstract description 9
- 238000000576 coating method Methods 0.000 claims abstract description 9
- 239000000945 filler Substances 0.000 claims abstract description 9
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 238000005096 rolling process Methods 0.000 claims abstract description 6
- 239000012528 membrane Substances 0.000 claims description 23
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 claims description 19
- 239000011347 resin Substances 0.000 claims description 19
- 229920005989 resin Polymers 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 15
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
- 230000003712 anti-aging effect Effects 0.000 claims description 8
- 239000003795 chemical substances by application Substances 0.000 claims description 8
- 239000007822 coupling agent Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims description 6
- 239000004743 Polypropylene Substances 0.000 claims description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 6
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
- 229920001155 polypropylene Polymers 0.000 claims description 6
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 5
- 238000002844 melting Methods 0.000 claims description 5
- 239000004615 ingredient Substances 0.000 claims description 4
- KPAPHODVWOVUJL-UHFFFAOYSA-N 1-benzofuran;1h-indene Chemical compound C1=CC=C2CC=CC2=C1.C1=CC=C2OC=CC2=C1 KPAPHODVWOVUJL-UHFFFAOYSA-N 0.000 claims description 3
- SKDGWNHUETZZCS-UHFFFAOYSA-N 2,3-ditert-butylphenol Chemical compound CC(C)(C)C1=CC=CC(O)=C1C(C)(C)C SKDGWNHUETZZCS-UHFFFAOYSA-N 0.000 claims description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 3
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 3
- 229960001866 silicon dioxide Drugs 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 239000000377 silicon dioxide Substances 0.000 claims description 3
- 229920001935 styrene-ethylene-butadiene-styrene Polymers 0.000 claims description 3
- 239000004408 titanium dioxide Substances 0.000 claims description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N toluene Substances CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 3
- IOUQJTTZESSBKY-UHFFFAOYSA-L zinc N-butyl-N-sulfidosulfanylbutan-1-amine formate Chemical group C(=O)[O-].C(CCC)N(SS[Zn+])CCCC IOUQJTTZESSBKY-UHFFFAOYSA-L 0.000 claims description 3
- 239000002994 raw material Substances 0.000 claims description 2
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- 244000043261 Hevea brasiliensis Species 0.000 abstract description 4
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- 238000007757 hot melt coating Methods 0.000 abstract description 2
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- 229920000098 polyolefin Polymers 0.000 abstract 1
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- 229910001220 stainless steel Inorganic materials 0.000 description 4
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- 238000005516 engineering process Methods 0.000 description 3
- 229920000178 Acrylic resin Polymers 0.000 description 2
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- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010559 graft polymerization reaction Methods 0.000 description 2
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Abstract
The invention discloses preparation methods of a hot melt pressure-sensitive adhesive and a protective film as well as the hot melt pressure-sensitive adhesive. The preparation method of the hot melt pressure-sensitive adhesive comprises the following steps: adding thermoplastic elastomers, a tackifier, a plasticizer, an antiager, an antioxidant, a crosslinker, a filler and the like into a double-mixed column mixer, stirring, heating until the materials are melted down, and uniformly mixing to obtain the pressure-sensitive adhesive. The preparation method of the protective film comprises the following steps: directly pumping the melted and uniformly mixed pressure-sensitive adhesive into a coating roll of the a hot melt coating machine by a heat transfer pump, coating the pressure-sensitive adhesive onto one face of a polyolefin plastic film or thin plastic-coated paper, cooling, and rolling to obtain the protective film (paper). The hot melt pressure-sensitive adhesive disclosed by the invention can obtain good initial stickiness, cohesion and age stripping property by changing the different ratio of the thermoplastic elastomer as well as the variety and usage amount of the tackifier. The prepared polyethylene (PE) film substrate protective film has low interfacial tension, good initial stickiness, high cohesion and high temperature resistance, light resistance and weather resistance, and the comprehensive performance and product cost of the hot melt pressure-sensitive adhesive disclosed by the invention are better than those of the traditional solvent pressure-sensitive adhesive taking natural rubber as the main material.
Description
Technical field
The present invention relates to a kind of prescription of hot-melt pressure sensitive adhesive, preparation method and by the preparation method of its thermoplastic elastomer PE protective membrane of making.
Background technology
Protective membrane or protective tapes are made up of pressure-sensitive adhesive and plastics film, gain the name because of its kind material is had defencive function.The critical material of forming protective membrane is a pressure-sensitive adhesive, and the main raw of formation pressure-sensitive adhesive has rubber and acrylic resin.By solvent-borne type then being arranged, aqueous emulsion type, hot-melting type and radiation-curable four big classes on the production method.With rubber, particularly natural rubber is that main pressure-sensitive adhesive has accounted for very small proportion, and the substitute is acrylic resin.Its major cause is that material over-all properties and cost determine.Dividing from manufacture method, at present still based on the acrylate solvent method, secondly is the acrylate water-latex type, and hot-melting type and radiation-curable are few.
But rubber pressure-sensitive adhesive still occupies certain proportion owing to its some feature at the protective membrane product scope.Big as force of cohesion; low-temperature performance is good; interfacial tension is low; two characteristics of tack and peeling force are easy to balance etc.; by its protective membrane that makes various material surfaces had well posting property; and the adhesive power time dependent increasess slowly, and does not corrode and does not pollute protected material surface, the suitable advantage such as uneven surface that is covered on.Therefore at the mirror face stainless steel material, the material of low surface energy, the protection aspect of the optical thin film material of uneven surface still right and wrong it does not belong to.
The existing rubber-type protective membrane of present domestic minority, its defective be, the one, remain solvent-borne type, and the 2nd, be main material still with natural rubber; therefore, still there is easily aging back cull, peels off difficulty; pollute protected material, discharge toxic harmful exhaust gas, shortcoming such as production efficiency is low.
Summary of the invention
In order to overcome the deficiency of existing background technology and product, the object of the present invention is to provide following two aspect technology and methods:
1, providing a kind of is hot-melt pressure sensitive adhesive prescription and the production method that main raw is formed with the thermoplastic elastomer.Big to make force of cohesion, low-temperature performance is good, and interfacial tension is low, and two characteristic parameters of tack and peeling force are easy to the equilibrated hot-melt pressure sensitive adhesive.And various material surfaces are all had well posting property by the protective membrane that itself and polyethylene film make, and and have the adhesive power time dependent and increases slowly, do not corrode and do not pollute protected material surface, be suitable for advantages such as posting uneven surface.
2, can polyethylene (PE) or polypropylene (PP) plastics film be base material, utilize heat seeling coating machine above-mentioned hot-melt pressure sensitive adhesive on it simultaneously is coated with, through cooling fast, rolling promptly becomes the PE or the PP protective membrane of thermoplastic elastomer.
Concrete technical scheme provided by the invention is:
A kind of hot-melt pressure sensitive adhesive, this hot-melt pressure sensitive adhesive raw material comprises the proportioning that following quality group becomes umber: the hot-melting type elastomerics: 100 parts, tackifying resin: 100～150 parts, tenderizer: 50～60 parts, superoxide: 0.1～0.5 part, acrylate: 5～10 parts, coupling agent: 0.5～2 part.
Its material component can comprise in addition, anti-aging agent: 1～3 part, and filler: 2～5 parts.
Wherein,
Described thermoplastic elastomer is to elect a kind of among SBS, SIS, SEBS and the SEIS or mixture that they are two or more as.
Described tackifying resin is terpine resin, coumarone indene resin, staybelite resin and C5～9
StoneThe mixture of one or two or more kinds in the oleo-resinous.
Described filler is the mixture of a kind of in aeroponics silicon-dioxide and the titanium dioxide or two kinds.
Described coupling agent is a silane coupling agent.
Described acrylate is one or two or more kinds the mixture in methyl methacrylate, butyl methacrylate, the methacrylic acid.
Described anti-aging agent is N, N-dibutylamino dithio zinc formate, 2, the mixture of one or two or more kinds in the 6-toluene di-tert-butyl phenol.
The present invention also provides a kind of preparation method of hot-melt pressure sensitive adhesive, comprises step:
Will except that the said components superoxide and the acrylate according to proportion ingredient, and join in two pillar molten-baths that stir, logical nitrogen slowly is heated with stirring to liquid state; The acrylate that is dissolved with superoxide slowly is added dropwise in the still, is incubated 4～5 hours down at 110～120 ℃.
And a kind of preparation method who uses the protective membrane of described hot-melt pressure sensitive adhesive, it is characterized in that, comprise step:
Will be except that superoxide and acrylate component according to proportion ingredient, and join in two pillar molten-baths that stir, logical nitrogen slowly is heated with stirring to liquid state; The acrylate that is dissolved with superoxide slowly is added dropwise in the still, is incubated 4～5 hours down, obtain this translucent hot-melt pressure sensitive adhesive at 110～120 ℃;
This hot-melt pressure sensitive adhesive is pumped into the coating roll of heat seeling coating machine with hot transferpump, and it is coated on the one side of polyethylene (PE) film or polypropylene (PP) film, through cooling fast, rolling and become the PE protective membrane of thermoplastic elastomer.
The invention has the advantages that:
Do not use any organic solvent in the present invention prescription, so environmental friendliness, the production cycle by the usual vehicle method 20 surplus hour foreshorten to 5～6 hours, so production efficiency improves, cost reduces.The present invention adopts acrylate monomer, graft polymerization or crosslinking polymerization and improved the thermotolerance and the weathering resistance of hot-melt pressure sensitive adhesive, thereby overcome the easy aged shortcoming of unsaturated double-bond.Added compound silane coupling agent in the present invention prescription, therefore improved weathering resistance and with the fastness that combines of PE base material, guaranteed that the protective membrane accident of coming unstuck does not take place.
Use the hot-melt pressure sensitive adhesive among the present invention to cooperate the PE protective membrane thermotolerance that makes with polyethylene film, weathering resistance, photostabilization are better than natural rubber type pressure-sensitive adhesive.The interfacial tension of pressure-sensitive adhesive is low, and tack is good, and surfaces of various materials is had good posting property, particularly has posting property preferably for uneven surface.
Embodiment
Of the present invention a kind of be the hot-melt pressure sensitive adhesive that main raw is formed with the thermoplastic elastomer, mainly become the material of umber to form by following quality group.A. hot-melting type elastomerics: 100 parts, the b. tackifying resin: 100～150 parts, the c. tenderizer: 50～60 parts, the d. anti-aging agent: 1～3 part, the e. superoxide: 0.1～0.5 part, the f. acrylate: 5～10 parts, the g. filler: 2～6 parts, h. coupling agent: 0.5～2 part.
Described thermoplastic elastomer is to be chosen as SBS, SIS, SEBS, the mixture of one or two or more kinds among the SEIS.
Described tackifying resin is to be chosen as terpine resin, coumarone indene resin, staybelite resin, C5～9
StoneThe mixture of one or two or more kinds in the oleo-resinous.
Described filler can be aeroponics silicon-dioxide, the mixture of a kind of in the titanium dioxide or two kinds.
Described coupling agent can be silane coupling agent.
Described acrylate is meant methyl methacrylate, butyl methacrylate, the mixture of one or two or more kinds in the methacrylic acid.
Described anti-aging agent (oxidation inhibitor) is N, N-dibutylamino dithio zinc formate, 2, the mixture of one or two or more kinds in the 6-toluene di-tert-butyl phenol.
With this thermoplastic elastomer is the hot-melt pressure sensitive adhesive production method that main raw is formed, and comprises step down:
1.. with the weighing and joining in two pillar molten-baths that stir in order of described thermoplastic elastomer, tackifying resin, tenderizer, anti-aging agent, filler, coupling agent, logical nitrogen slowly is heated with stirring to liquid state.The acrylate that is dissolved with superoxide is slowly splashed in the still, be incubated 4～5 hours down, promptly obtain translucent hot-melt pressure sensitive adhesive at 110 ℃～120 ℃.
2.. this hot-melt pressure sensitive adhesive is pumped into the coating roll of heat seeling coating machine with hot transferpump, and it is coated on the one side of polyethylene (PE) film, through cooling fast, rolling and become the PE protective membrane of thermoplastic elastomer.
Below describe the present invention in detail by specific embodiment and comparative example.See Table 1:
Table 1. embodiment and comparative example
The manufacture method of the specific embodiment among the present invention is carried out according to the following steps:
1.. thermoplastic elastomer, tackifying resin, tenderizer, anti-aging agent, filler, coupling agent are sequentially added in the hot melt still, and logical again nitrogen slowly is heated with stirring to liquid state.With the molten acrylate monomer that superoxide is arranged, slowly splash in the hot melt still, be incubated 4～5 hours down at 110 ℃～120 ℃, promptly obtain translucent hot-melt pressure sensitive adhesive.
2.. the hot-melt pressure sensitive adhesive that obtains is coated on black or other colors uniformly with small-sized hot melt coating machine; thickness is the one side of the polyethylene film of 50～80 μ m; after cooling off fast, promptly obtaining the pressure-sensitive adhesive layer thickness is the thermoplastic elastomer pressure sensitive adhesive protective membrane of 10～20 μ m.Employed polyethylene film coated face is handled through silane coupling agent.
For proving certain effect of the present invention; to carry out the detection of projects such as 180 ° of peeling forces, slope rolling ball method initial bonding strength, interfacial tension, photostabilization, temperature tolerance, posting property, contaminative by the black PE protective membrane that method in the above-mentioned specific embodiment and step obtain, to estimate the over-all properties of this kind protective membrane of the present invention.
Wherein, 180 ° of peeling forces detect and are undertaken by GB/2192-81; Initial bonding strength detects and is undertaken by GB/4852-84; Interfacial tension detects carries out with tension force liquid; Photostabilization is that the infrared lamp with the UV-light of 200W and 200W shone respectively 72 hours apart from sample 200mm; Temperature tolerance is that sample is placed in 100 ℃, the climatic chamber of relative humidity 90% 72 hours; Posting property testing is that protective membrane is affixed on mirror face stainless steel plate and coarse stainless steel plate; Contaminative is that protective membrane is affixed on the standard stainless steel plate, carry out photostabilization, temperature tolerance, temperature tolerance test respectively after, tear protective membrane off, natural light is observed down and is had or not to fall glue, cull and estimate, and the results are shown in Table 2.
Table 2. detects evaluation result
By table 1 and table 2 as can be seen; the hot-melt pressure sensitive adhesive of manufacturing of the present invention can be by selecting a kind of of thermoplastic elastic body rubber or two kinds of collocation for use; and select high tackifying resin of softening temperature and graft polymerization for use; make the hot melt process PE protective membrane that makes have high temperature resistant, photostabilization, characteristics that resistance to crocking is good, thereby finish the present invention.
Claims (10)
1. a hot-melt pressure sensitive adhesive is characterized in that, this hot-melt pressure sensitive adhesive raw material comprises the proportioning that following quality group becomes umber:
The hot-melting type elastomerics: 100 parts, tackifying resin: 100～150 parts, tenderizer: 50～60 parts, superoxide: 0.1～0.5 part, acrylate: 5～10 parts, coupling agent: 0.5～2 part.
2. hot-melt pressure sensitive adhesive according to claim 1 is characterized in that, described thermoplastic elastomer is to elect a kind of among SBS, SIS, SEBS and the SEIS or mixture that they are two or more as.
3. hot-melt pressure sensitive adhesive according to claim 1 is characterized in that, described tackifying resin is one or two or more kinds the mixture in the petroleum resin of terpine resin, coumarone indene resin, staybelite resin and C5～9.
4. hot-melt pressure sensitive adhesive according to claim 1 is characterized in that, described coupling agent is a silane coupling agent.
5. hot-melt pressure sensitive adhesive according to claim 1 is characterized in that, described acrylate is one or two or more kinds the mixture in methyl methacrylate, butyl methacrylate, the methacrylic acid.
6. hot-melt pressure sensitive adhesive according to claim 1 is characterized in that described anti-aging agent is N, N-dibutylamino dithio zinc formate, 2, the mixture of one or two or more kinds in the 6-toluene di-tert-butyl phenol.
7. according to the described hot-melt pressure sensitive adhesive of above arbitrary claim, it is characterized in that its material component comprises in addition, anti-aging agent: 1～3 part and/or filler: 2～5 parts.
8. hot-melt pressure sensitive adhesive according to claim 7 is characterized in that, described filler is the mixture of a kind of in aeroponics silicon-dioxide and the titanium dioxide or two kinds.
9. the preparation method of the hot-melt pressure sensitive adhesive of the above arbitrary claim of a basis is characterized in that it comprises step:
Will be except that superoxide and acrylate component according to proportion ingredient, and join in two pillar molten-baths that stir, logical nitrogen slowly is heated with stirring to liquid state; The acrylate that is dissolved with superoxide slowly is added dropwise in the still, is incubated 4～5 hours down at 110～120 ℃.
10. an application rights requires the preparation method of the protective membrane of any described hot-melt pressure sensitive adhesive among the 1-8, it is characterized in that, comprises step:
Will be except that superoxide and acrylate component according to proportion ingredient, and join in two pillar molten-baths that stir, logical nitrogen slowly is heated with stirring to liquid state; The acrylate that is dissolved with superoxide slowly is added dropwise in the still, is incubated 4～5 hours down, obtain this translucent hot-melt pressure sensitive adhesive at 110～120 ℃;
This hot-melt pressure sensitive adhesive is pumped into the coating roll of heat seeling coating machine with hot transferpump, and it is coated on the one side of polyethylene film or polypropylene film, through cooling fast, rolling and become the PE protective membrane of thermoplastic elastomer.
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| CN 201010560902 CN102051149B (en) | 2010-11-26 | 2010-11-26 | Preparation methods of hot melt pressure-sensitive adhesive and protective film |
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| CN 201010560902 CN102051149B (en) | 2010-11-26 | 2010-11-26 | Preparation methods of hot melt pressure-sensitive adhesive and protective film |
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| CN102051149B CN102051149B (en) | 2013-04-24 |
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| CN113004842A (en) * | 2021-04-16 | 2021-06-22 | 江苏欧西建材科技发展有限公司 | Special hot-melt pressure-sensitive adhesive for HDPE (high-density polyethylene) waterproof coiled material and preparation method thereof |
| CN115651553A (en) * | 2022-10-28 | 2023-01-31 | 烟台德邦科技股份有限公司 | High-adhesion-holding hot-melt pressure-sensitive foam adhesive tape for lithium battery packaging and preparation method thereof |
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Address after: 215347 No. 3123 Huanqing Road, Yushan Town, Kunshan City, Suzhou City, Jiangsu Province Patentee after: Boyi Xincheng Polymer Materials Co.,Ltd. Address before: 215347 No. 1798 Zhonghua Garden West Road, Development Zone, Yushan Town, Kunshan City, Suzhou City, Jiangsu Province Patentee before: KUNSHAN BYE POLYMER MATERIAL Co.,Ltd. |