CN102051149B - Preparation methods of hot melt pressure-sensitive adhesive and protective film - Google Patents
Preparation methods of hot melt pressure-sensitive adhesive and protective film Download PDFInfo
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- CN102051149B CN102051149B CN 201010560902 CN201010560902A CN102051149B CN 102051149 B CN102051149 B CN 102051149B CN 201010560902 CN201010560902 CN 201010560902 CN 201010560902 A CN201010560902 A CN 201010560902A CN 102051149 B CN102051149 B CN 102051149B
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- 239000012943 hotmelt Substances 0.000 title claims abstract description 41
- 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
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- -1 polyethylene Polymers 0.000 claims abstract description 12
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- 238000001816 cooling Methods 0.000 claims abstract description 6
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- SOGAXMICEFXMKE-UHFFFAOYSA-N Butylmethacrylate Chemical compound CCCCOC(=O)C(C)=C SOGAXMICEFXMKE-UHFFFAOYSA-N 0.000 claims description 14
- 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
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 7
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 7
- 239000004743 Polypropylene Substances 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 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
- 238000009413 insulation Methods 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
- 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
- JEIPFZHSYJVQDO-UHFFFAOYSA-N ferric oxide Chemical compound O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 claims description 3
- 239000003208 petroleum Substances 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
- 239000000463 material Substances 0.000 abstract description 19
- 244000043261 Hevea brasiliensis Species 0.000 abstract description 4
- 229920003052 natural elastomer Polymers 0.000 abstract description 4
- 229920001194 natural rubber Polymers 0.000 abstract description 4
- 238000007757 hot melt coating Methods 0.000 abstract description 2
- 239000002904 solvent Substances 0.000 abstract description 2
- 239000004971 Cross linker Substances 0.000 abstract 1
- 239000003963 antioxidant agent Substances 0.000 abstract 1
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- 239000002985 plastic film Substances 0.000 abstract 1
- 229920006255 plastic film Polymers 0.000 abstract 1
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- 239000004014 plasticizer Substances 0.000 abstract 1
- 229920000098 polyolefin Polymers 0.000 abstract 1
- 238000005086 pumping Methods 0.000 abstract 1
- 239000000758 substrate Substances 0.000 abstract 1
- 239000010408 film Substances 0.000 description 9
- 238000004519 manufacturing process Methods 0.000 description 9
- 238000000034 method Methods 0.000 description 8
- 230000000176 photostabilization Effects 0.000 description 5
- 229920001971 elastomer Polymers 0.000 description 4
- 229910001220 stainless steel Inorganic materials 0.000 description 4
- 239000010935 stainless steel Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 3
- 238000002844 melting Methods 0.000 description 3
- NIXOWILDQLNWCW-UHFFFAOYSA-M Acrylate Chemical compound [O-]C(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-M 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 2
- 239000004925 Acrylic resin Substances 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000032683 aging Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 238000010559 graft polymerization reaction Methods 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 2
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- 239000003292 glue Substances 0.000 description 1
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- Adhesives Or Adhesive Processes (AREA)
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 comprised of pressure-sensitive adhesive and plastics film, gain the name because its kind material is had defencive function.The critical material that forms protective membrane is 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 large 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 take the acrylate solvent method as main, 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.Large such 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, still take natural rubber as main material; therefore, still there is easily aging rear cull, peels off difficulty; pollute protected material, discharge toxic harmful exhaust gas, the 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, provides a kind of hot-melt pressure sensitive adhesive prescription and production method that forms take thermoplastic elastomer as main raw.Large 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 hot-melt pressure sensitive adhesive of balance.And by the protective membrane that itself and polyethylene film make various material surfaces are all had well posting property, 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 its coated on one side, through fast cooling, rolling namely becomes 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: thermoplastic elastomer: 100 parts, tackifying resin: 100~150 parts, tenderizer: 50~60 parts, superoxide: 0.1~0.5 part, acrylic acid derivative: 5~10 parts, coupling agent: 0.5~2 part, wherein acrylic acid derivative is one or more the mixture in methyl methacrylate, butyl methacrylate or the methacrylic acid.
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 one or two or more kinds the mixture in the petroleum resin of terpine resin, coumarone indene resin, staybelite resin and C5~9.
Described filler is the mixture of a kind of in aeroponics silicon-dioxide and the titanium dioxide or two kinds.
Described coupling agent is silane coupling agent.
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:
Said components except superoxide and acrylic acid derivative according to proportion ingredient, and is joined in two pillar molten-baths that stir, and logical nitrogen slowly is heated with stirring to liquid state; The acrylic acid derivative that is dissolved with superoxide slowly is added dropwise in the still, 110~120 ℃ of lower insulations 4~5 hours; Wherein acrylic acid derivative is one or more the mixture in methyl methacrylate, butyl methacrylate or the methacrylic acid.
And a kind of preparation method who uses the protective membrane of described hot-melt pressure sensitive adhesive, comprise step:
Will be except superoxide and acrylic acid derivative 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 acrylic acid derivative that is dissolved with superoxide slowly is added dropwise in the still, 110~120 ℃ of lower insulations 4~5 hours, obtains this translucent hot-melt pressure sensitive adhesive; Wherein acrylic acid derivative is one or more the mixture in methyl methacrylate, butyl methacrylate or the methacrylic acid;
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 fast cooling, 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 foreshortens to 5~6 hours by more than 20 hours of usual vehicle method, so production efficiency improves cost.The present invention adopts the acrylic acid derivative monomer, graft polymerization or crosslinking polymerization and improved thermotolerance and the weathering resistance of hot-melt pressure sensitive adhesive, thereby overcome easily aging shortcoming of unsaturated double-bond.Added compound silane coupling agent in the present invention prescription, therefore improved weathering resistance and with the binding strength of PE base material, guaranteed that the protective membrane accident of coming unstuck does not occur.
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 preferably posting property for uneven surface.
Embodiment
A kind of hot-melt pressure sensitive adhesive that forms take thermoplastic elastomer as main raw of the present invention mainly becomes the material of umber to form by following quality group.A. hot-melting type elastomerics: 100 parts, the b. tackifying resin: 100~150 parts, c. tenderizer: 50~60 parts, d. anti-aging agent: 1~3 part, the e. superoxide: 0.1~0.5 part, f. acrylic acid derivative: 5~10 parts, g. filler: 2~6 parts, h. coupling agent: 0.5~2 part.Its acrylic acid derivative refers to methyl methacrylate, butyl methacrylate, the mixture of one or two or more kinds in the methacrylic acid.
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, the mixture of one or two or more kinds in the petroleum resin of C5~9.
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 anti-aging agent (oxidation inhibitor) is N, N-dibutylamino dithio zinc formate, the mixture of one or two or more kinds in 2, the 6-toluene di-tert-butyl phenol.
The hot-melt pressure sensitive adhesive production method that forms take this thermoplastic elastomer as main raw comprises lower step:
1.. with the in order weighing and joining in two pillar molten-baths that stir of described thermoplastic elastomer, tackifying resin, tenderizer, anti-aging agent, filler, coupling agent, logical nitrogen slowly is heated with stirring to liquid state.The aforesaid propylene acid derivative that is dissolved with superoxide is slowly splashed in the still, 110 ℃~120 ℃ lower insulations 4~5 hours, namely obtain translucent hot-melt pressure sensitive adhesive.
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 fast cooling, 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 kettle, and logical nitrogen slowly is heated with stirring to liquid state.With the molten aforesaid propylene acid derivative monomer that superoxide is arranged, slowly splash in the hot melt kettle, 110 ℃~120 ℃ lower insulations 4~5 hours, namely 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, namely 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 processed through silane coupling agent.
For proving certain effect of the present invention; to be carried out by the black PE protective membrane that the method in the above-mentioned specific embodiment and step obtain the detection of the projects such as 180 ° of peeling forces, slope rolling ball method initial bonding strength, interfacial tension, photostabilization, temperature tolerance, posting property, contaminative, 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 UV-light of all 200W and the infrared lamp of 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 respectively photostabilization, temperature tolerance, temperature tolerance test after, tear protective membrane off, observe under the natural light and have or not to fall glue, cull and estimate, the results are shown in Table 2.
Table 2. detects evaluation result
Can find out by table 1 and table 2; 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; and select the high tackifying resin of softening temperature and graft polymerization; 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 (8)
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:
Thermoplastic elastomer: 100 parts, tackifying resin: 100~150 parts, tenderizer: 50~60 parts, superoxide: 0.1~0.5 part; Acrylic acid derivative: 5~10 parts, coupling agent: 0.5~2 part; Wherein, acrylic acid derivative is one or more the mixture in methyl methacrylate, butyl methacrylate or the methacrylic acid;
Described thermoplastic elastomer is to be selected from a kind of among SBS, SIS, SEBS and the SEIS or mixture that they are two or more.
2. 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~C9.
3. hot-melt pressure sensitive adhesive according to claim 1 is characterized in that, described coupling agent is silane coupling agent.
4. according to the described hot-melt pressure sensitive adhesive of above arbitrary claim, it is characterized in that this hot-melt pressure sensitive adhesive feed composition comprises anti-aging agent in addition: 1~3 part and/or filler: 2~5 parts.
5. hot-melt pressure sensitive adhesive according to claim 4 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.
6. hot-melt pressure sensitive adhesive according to claim 4 is characterized in that, described filler is the mixture of a kind of in aeroponics silicon-dioxide and the titanium dioxide or two kinds.
7. 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 superoxide and acrylic acid derivative 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 acrylic acid derivative that is dissolved with superoxide slowly is added dropwise in the still, 110~120 ℃ of lower insulations 4~5 hours; Wherein, acrylic acid derivative is one or more the mixture in methyl methacrylate, butyl methacrylate or the methacrylic acid.
8. an application rights requires the preparation method of the protective membrane of the described hot-melt pressure sensitive adhesive of any one among the 1-6, it is characterized in that, comprises step:
Will be except superoxide and acrylic acid derivative 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 acrylic acid derivative that is dissolved with superoxide slowly is added dropwise in the still, 110~120 ℃ of lower insulations 4~5 hours, obtains this translucent hot-melt pressure sensitive adhesive; Wherein, acrylic acid derivative is one or more the mixture in methyl methacrylate, butyl methacrylate or the methacrylic acid;
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 fast cooling, rolling and become PE or the PP protective membrane of thermoplastic elastomer.
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