CN110776832A - Covering pressure-sensitive adhesive and preparation method and application thereof - Google Patents
Covering pressure-sensitive adhesive and preparation method and application thereof Download PDFInfo
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- CN110776832A CN110776832A CN201911084205.1A CN201911084205A CN110776832A CN 110776832 A CN110776832 A CN 110776832A CN 201911084205 A CN201911084205 A CN 201911084205A CN 110776832 A CN110776832 A CN 110776832A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J4/00—Adhesives based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; adhesives, based on monomers of macromolecular compounds of groups C09J183/00 - C09J183/16
- C09J4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09J159/00 - C09J187/00
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/06—Non-macromolecular additives organic
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/20—Adhesives in the form of films or foils characterised by their carriers
- C09J7/22—Plastics; Metallised plastics
- C09J7/25—Plastics; Metallised plastics based on macromolecular compounds obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/255—Polyesters
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J7/00—Adhesives in the form of films or foils
- C09J7/30—Adhesives in the form of films or foils characterised by the adhesive composition
- C09J7/38—Pressure-sensitive adhesives [PSA]
- C09J7/381—Pressure-sensitive adhesives [PSA] based on macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
- C09J7/385—Acrylic polymers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/10—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet
- C09J2301/12—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers
- C09J2301/122—Additional features of adhesives in the form of films or foils characterized by the structural features of the adhesive tape or sheet by the arrangement of layers the adhesive layer being present only on one side of the carrier, e.g. single-sided adhesive tape
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2301/00—Additional features of adhesives in the form of films or foils
- C09J2301/30—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier
- C09J2301/302—Additional features of adhesives in the form of films or foils characterized by the chemical, physicochemical or physical properties of the adhesive or the carrier the adhesive being pressure-sensitive, i.e. tacky at temperatures inferior to 30°C
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J2467/00—Presence of polyester
- C09J2467/006—Presence of polyester in the substrate
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- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention provides a covering pressure-sensitive adhesive which is prepared from the following raw materials in parts by weight: 20-40 parts of elastomer, 30-50 parts of tackifier, 5-15 parts of softener, 2-5 parts of crosslinking agent, 3-5 parts of auxiliary crosslinking agent, 0-2 parts of coupling agent, 0.01-1 part of antioxidant, 1-5 parts of pigment and 3-10 parts of filler. The invention also discloses a preparation method and application of the covering pressure-sensitive adhesive. The covering pressure-sensitive adhesive provided by the invention has the advantages of small smell, excellent heat resistance and good bonding effect.
Description
Technical Field
The invention relates to a covering pressure-sensitive adhesive and a preparation method and application thereof.
Background
The hot melt pressure sensitive adhesive has simple preparation and construction process, high curing speed and the like, is particularly suitable for occasions with high automation requirements, is very popular in the market, but has the problems of poor solvent resistance, poor heat resistance and the like due to the special system of the hot melt adhesive. Patent CN101824280A discloses an ultraviolet curable pressure sensitive adhesive and a preparation method thereof, the method uses a large amount of low viscosity acrylate diluent, the low reactivity diluent has the problem of incomplete reaction in the short curing process, meanwhile, the system uses a photoinitiator to realize ultraviolet curing, and the decomposition residue of the photoinitiator and the odor of the residual small molecules of the photoinitiator are pungent; patent CN104927697A discloses an adhesive tape made of UV-curable hot-melt pressure-sensitive adhesive for automobile wire harness, which also has the problems of photoinitiator and olefin monomer, and all of the above patents adopt monofunctional dilution monomer with low viscosity, and because the monomer can not form cross-linking with main resin, the heat resistance of the cured system is improved to a limited extent.
Disclosure of Invention
The invention aims to solve the technical problem of providing a covering pressure-sensitive adhesive with small smell, excellent heat resistance and good bonding effect.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a covering pressure-sensitive adhesive is prepared from the following raw materials in parts by weight: 20-40 parts of elastomer, 30-50 parts of tackifier, 5-15 parts of softener, 2-5 parts of crosslinking agent, 3-5 parts of auxiliary crosslinking agent, 0-2 parts of coupling agent, 0.01-1 part of antioxidant, 1-5 parts of pigment and 3-10 parts of filler.
Preferably, the elastomer of the invention is one or a mixture of more than two of EVA, SIS, SBS, SBR, POE and POP. More preferably, the elastomer of the present invention is a styrene-isoprene-styrene elastomer SIS having a styrene content of 15 to 50%, a diblock proportion of 15 to 50%, and a melt index of 6 to 50 g/min.
Preferably, the tackifier of the invention is one or a mixture of more than two of C5 resin, DCPD resin, C9 modified DCPD resin, C9 resin, rosin modified resin, hydrogenated C5 resin, hydrogenated DCPD resin, rosin and terpene resin.
Preferably, the softener is one or a mixture of more than two of naphthenic oil, paraffin oil, dioctyl terephthalate, white oil, No. 40 engine oil and vacuum pump oil. Pure elastomers are generally hard solids with no adhesive properties and no pressure sensitivity, so that softeners have to be added to reduce hardness.
Preferably, the cross-linking agent of the present invention is one or a mixture of two or more of trimethylolpropane acrylate TMPTA, triallylisocyanurate TAIC, trimethylolpropane trimethacrylate TMPTMA, pentaerythritol triacrylate PETA.
Preferably, the auxiliary crosslinking agent is one or a mixture of more than two of 1, 6-hexanediol diacrylate HDDA, dipropylene glycol diacrylate DPGDA and tripropylene glycol diacrylate TPGDA.
Preferably, the coupling agent is one or a mixture of more than two of vinyl tri (β -methoxyethoxy) silane, gamma-methacryloxypropyl trimethoxysilane, gamma-methacryloxypropyl triisopropoxysilane and gamma-glycidoxypropyltrimethoxysilane
Preferably, the antioxidant of the present invention is one or a mixture of two or more of 2, 2' -methylenebis- (4-methyl-6-tert-butylphenol), diphenylisodecyl phosphite, triphenyl phosphite, diisooctyl phenyl phosphite, β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid n-octadecyl ester, ethylenebis (oxyethylene) bis [3- (5-tert-butyl-4-hydroxy-m-tolyl) propionate ], tris (2, 4-di-tert-butylphenyl) phosphite, and tetrakis (β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionic acid) pentaerythritol ester.
Preferably, the pigment of the present invention is one or a mixture of two or more of α type phthalocyanine blue, β type phthalocyanine blue and epsilon type phthalocyanine blue.
Preferably, the filler of the invention is one or a mixture of more than two of calcium carbonate, barium sulfate, kaolin and titanium dioxide.
The invention also aims to provide a preparation method of the covering pressure-sensitive adhesive.
In order to solve the technical problems, the technical scheme is as follows:
a preparation method of a covering pressure-sensitive adhesive comprises the following steps:
setting the temperature of the reaction kettle at 130 ℃, sequentially adding a softener and an antioxidant into the reaction kettle from a feed inlet according to the formula, heating and stirring, and introducing nitrogen into the reaction kettle; adding the elastomer when the heating temperature reaches 130 ℃, continuously stirring and heating to 160 ℃, maintaining the temperature and stirring for 110-130 minutes; after the elastomer is completely melted, reducing the temperature to 130 ℃, adding the tackifier and other raw materials, stirring and maintaining the temperature until the elastomer is completely melted; stopping heating and stopping introducing nitrogen, closing the charging port, vacuumizing the reaction kettle under the condition of continuously stirring until the vacuum pressure is 0.08MPa and keeping the vacuum pressure for 30-40 minutes, continuously vacuumizing for 5-6 minutes after stopping stirring, evacuating the vacuum, introducing compressed air with the pressure of 0.1MPa into the reaction kettle, discharging, cooling and subpackaging to obtain the finished product.
The invention also aims to provide the application of the covering pressure-sensitive adhesive in the covering pressure-sensitive adhesive tape.
Preferably, the masking pressure sensitive adhesive tape of the present invention is made by the steps of:
setting the temperature of the hot melt coating machine to 140 ℃, melting the covering pressure sensitive adhesive according to the ratio of 30-100g/m
2The coating weight is coated on a PET base film with the width of 1100mm and the thickness of 50um, then electron beam EB curing is carried out, a single-side coated release film is prepared, and then the coating is wound, wherein the curing energy is 10-500kev, and the dosage is 5-200 kGy.
Therefore, compared with the prior art, the invention has the following beneficial effects:
1) the covering pressure-sensitive adhesive consists of an elastomer, a softening agent, a cross-linking assistant, a coupling agent, an antioxidant and pigment and filler, and the optimal proportion and the proper preparation method of the components are finally determined through repeated research experiments. The inspection shows that the covering pressure-sensitive adhesive has the characteristics of good covering property, moderate initial adhesion, high peeling force, good adhesive holding property, good heat resistance and the like, and can completely meet the requirements of the covering adhesive.
2) The invention adopts an EB curing system, does not need to add a photoinitiator, avoids the problems of residue and smell of micromolecules, and has higher monomer curing conversion rate.
3) The crosslinking agent and the auxiliary crosslinking agent used in the invention enable the system to form a complete crosslinking system, the formed cohesion is relatively large, meanwhile, the softening agent contained in the system can still play a role in internal plasticization, the cohesion of the whole system is large, the initial adhesion is moderate, and no adhesive residue is generated after the system is attached.
Detailed Description
The present invention will be described in detail with reference to specific embodiments, which are illustrative of the invention and are not to be construed as limiting the invention.
Example 1
The covering pressure-sensitive adhesive is prepared from the following raw materials, by weight, 110515 parts of SIS, 112615 parts of SIS, 30 parts of hydrogenated C5 resin, 20 parts of hydrogenated DCPD resin, 401010 parts of naphthenic oil, 3 parts of triallyl isocyanurate TAIC, 5 parts of 1, 6-hexanediol diacrylate HDDA, 1.2 parts of gamma-methacryloxypropyl trimethoxy silane, 0.4 part of antioxidant 168 (tris (2.4-di-tert-butylphenyl) phosphite), 0.4 part of antioxidant 1010 (tetrakis (β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate) pentaerythritol ester), 3 parts of α type phthalocyanine blue (15: 1) and 5 parts of calcium carbonate.
The preparation method of the covering pressure-sensitive adhesive comprises the following steps:
setting the temperature of the reaction kettle at 130 ℃, sequentially adding naphthenic oil 4010, antioxidant 168 and antioxidant 1010 into the reaction kettle from a feed inlet according to the formula, heating and stirring, and introducing nitrogen into the reaction kettle; adding the SIS1105 and the SIS1126 when the heating temperature reaches 130 ℃, continuously stirring and heating to 160 ℃, maintaining the temperature and stirring for 120 minutes; after SIS1105 and SIS1126 are completely melted, reducing the temperature to 130 ℃, adding hydrogenated C5 resin, hydrogenated DCPD resin and other raw materials, stirring and maintaining the temperature until the materials are completely melted; stopping heating, stopping introducing nitrogen, closing the charging port, vacuumizing the reaction kettle under the condition of continuously stirring until the vacuum pressure is 0.08MPa, keeping for 30 minutes, continuously vacuumizing for 5 minutes after stopping stirring, emptying, introducing compressed air with the pressure of 0.1MPa into the reaction kettle, discharging, cooling and subpackaging to obtain the product.
The masking pressure sensitive adhesive is made into a masking pressure sensitive adhesive tape by the following steps:
setting the temperature of the hot melt coating machine to 140 ℃, melting the covering pressure sensitive adhesive according to the ratio of 40g/m
2The coating weight is coated on a PET base film with the width of 1100mm and the thickness of 50um, then electron beam EB curing is carried out, a single-side coated release film is prepared, and then the single-side coated release film is wound, wherein the curing energy is 100kev, the dose is 50kGy, the irradiation height is 50mm, and the coating thickness of the covering pressure sensitive adhesive is 40 mu m.
Reference example 1
The covering pressure-sensitive adhesive is prepared from the following raw materials, by weight, 110515 parts of SIS, 112615 parts of SIS, 30 parts of hydrogenated C5 resin, 20 parts of hydrogenated DCPD resin, 401010 parts of naphthenic oil, 1.2 parts of gamma-methacryloxypropyltrimethoxysilane, 0.4 part of antioxidant 168 (tris (2.4-di-tert-butylphenyl) phosphite), 0.4 part of antioxidant 1010 (pentaerythritol tetrakis (β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate), 3 parts of α type phthalocyanine blue (15: 1) and 5 parts of calcium carbonate.
The masking pressure sensitive adhesive and the masking pressure sensitive adhesive tape were prepared in the same manner as in example 1.
The difference from example 1 is the absence of the crosslinking agent triallyl isocyanurate TAIC and the co-crosslinking agent 1, 6-hexanediol diacrylate HDDA.
Reference example 2
The covering pressure-sensitive adhesive is prepared from, by weight, 110515 parts of SIS, 112615 parts of SIS, 30 parts of hydrogenated C5 resin, 20 parts of hydrogenated DCPD resin, 3 parts of triallyl isocyanurate TAIC, 5 parts of 1, 6-hexanediol diacrylate HDDA, 1.2 parts of gamma-methacryloxypropyl trimethoxy silane, 0.4 part of antioxidant 168 (tris (2.4-di-tert-butylphenyl) phosphite), 0.4 part of antioxidant 1010 (pentaerythrityl tetrakis (β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate)), 3 parts of α type phthalocyanine blue (15: 1) and 5 parts of calcium carbonate.
The masking pressure sensitive adhesive and the masking pressure sensitive adhesive tape were prepared in the same manner as in example 1.
The difference from example 1 is the absence of the softening agent naphthenic oil 4010.
Reference example 3
The covering pressure-sensitive adhesive is prepared from, by weight, 110515 parts of SIS, 112615 parts of SIS, 30 parts of hydrogenated C5 resin, 20 parts of hydrogenated DCPD resin, 401010 parts of naphthenic oil, 3 parts of triallyl isocyanurate TAIC, 5 parts of 1, 6-hexanediol diacrylate HDDA, 1.2 parts of gamma-methacryloxypropyl trimethoxy silane, 0.4 part of antioxidant 168 (tris (2.4-di-tert-butylphenyl) phosphite), 0.4 part of antioxidant 1010 (tetrakis (β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate) pentaerythritol ester), 3 parts of α type phthalocyanine blue (15: 1), 5 parts of calcium carbonate, 1 part of photoinitiator and 2 parts of 819 photoinitiator.
The masking pressure sensitive adhesive was prepared in the same manner as in example 1.
The masking pressure sensitive adhesive is made into a masking pressure sensitive adhesive tape by the following steps:
setting the temperature of the hot melt coating machine to 140 ℃, melting the covering pressure sensitive adhesive according to the ratio of 40g/m
2Coating the coating weight on a PET base film with the width of 1100mm and the thickness of 50um, carrying out UV curing, preparing a single-side coated release film, and rolling to obtain the UV-curable coating, wherein the power of a UV mercury lamp is 6kW, and the irradiation dose is 3000mj/cm
2The height of the irradiation was 50mm, and the coating thickness of the masking pressure-sensitive adhesive was 40 μm.
The difference from example 1 is that 184 photoinitiator and 819 photoinitiator are added to the raw materials.
Comparative example: example 1 of patent CN104927697A
Test example:
the masking pressure-sensitive tapes prepared in example 1, reference examples 1 to 3 and comparative example 1 were subjected to the following performance test tests: annular initial adhesion test, refer to GB/T31125-; 180-degree peeling force test, and reference GB/T2792-2014 tests 180-degree peeling force; the constant-temperature constant-viscosity force test refers to GB/T4851-1998 to test the constant-viscosity force; and (3) testing the temperature stability: suspending the adhesive tape sample in a 150 ℃ oven for 24H, and observing whether the adhesive overflow phenomenon exists; and (4) testing the smell. The test results are shown in the following table:
| sample (I) | Permanent adhesion | Peeling force | Initial annular adhesion | Temperature stability | Smell(s) |
| Example 1 | 200H | 21N/25mm | 7N/25mm | Glue overflow-free | No pungent smell |
| Reference example 1 | 142H | 15N/25mm | 5N/25mm | A small amount of glue overflow | No pungent smell |
| Reference example 2 | 131H | 14N/25mm | 4N/25mm | A small amount of glue overflow | No pungent smell |
| Reference example 3 | 114H | 22N/25mm | 8N/25mm | A small amount of glue overflow | Has pungent smell |
| Comparative example | 125H | 26N/25mm | 12N/25mm | Slight glue overflow | Has pungent smell |
As can be seen from the above table, inventive example 1 has significantly better tack strength and temperature stability than the comparative example, and no pungent odor. The difference between some of the raw materials of reference examples 1-3 and example 1 indicates that the indexes except for the odor are reduced to different degrees, which indicates that the crosslinking agent, the auxiliary crosslinking agent and the softening agent used in the present invention can effectively improve the bonding effect and the temperature stability of the masking pressure sensitive adhesive tape; in terms of odor, each of example 1, reference example 1 and reference example 2 had no pungent odor, and each of reference example 3 and comparative example had a pungent odor, indicating that the system used in the present invention can largely avoid the odor problem caused by the photoinitiator.
Example 2
The covering pressure-sensitive adhesive is prepared from the following raw materials, by weight, 20 parts of EVA, 40 parts of C5 resin, 15 parts of paraffin oil, 4 parts of TMPTA, 3.5 parts of DPGDA, 0.4 part of vinyl tris (β -methoxyethoxy) silane, 0.6 part of diphenyl isodecyl phosphite, 1 part of β type phthalocyanine blue (15: 3) and 8 parts of barium sulfate.
The preparation method of the covering pressure-sensitive adhesive comprises the following steps:
setting the temperature of the reaction kettle at 130 ℃, sequentially adding paraffin oil and diphenyl isodecyl phosphite into the reaction kettle from a feed inlet according to the formula, heating and stirring, and introducing nitrogen into the reaction kettle; adding EVA when the heating temperature reaches 130 ℃, continuously stirring and heating to 160 ℃, maintaining the temperature and stirring for 110 minutes; after the EVA is completely melted, reducing the temperature to 130 ℃, adding C5 resin and other raw materials, stirring and maintaining the temperature until the EVA is completely melted; stopping heating, stopping introducing nitrogen, closing the charging port, vacuumizing the reaction kettle under the condition of continuously stirring until the vacuum pressure is 0.08MPa, keeping the vacuum pressure for 40 minutes, stopping stirring, continuously vacuumizing for 6 minutes, emptying, introducing compressed air with the pressure of 0.1MPa into the reaction kettle, discharging, cooling and subpackaging to obtain the product.
The masking pressure sensitive adhesive is made into a masking pressure sensitive adhesive tape by the following steps:
setting the temperature of the hot melt coating machine to 140 ℃, melting the covering pressure sensitive adhesive according to 100g/m
2The coating weight is coated on a PET base film with the width of 1100mm and the thickness of 50um, then electron beam EB curing is carried out, a single-side coated release film is prepared and then the single-side coated release film is wound, the curing energy is 200kev, the dose is 100kGy, the irradiation height is 50mm, and the coating thickness of the covering pressure-sensitive adhesive is 40 mu m.
Example 3
The covering pressure-sensitive adhesive is prepared from the following raw materials in parts by weight: 40 parts of SBS, 30 parts of DCPD resin, 5 parts of dioctyl terephthalate, 2.5 parts of TMPTMA, 4 parts of TPGDA, 1.5 parts of gamma-methacryloxypropyltrimethoxysilane, 0.2 part of triphenyl phosphite, 4 parts of gamma-type phthalocyanine blue (15: 6) and 10 parts of kaolin.
The preparation method of the covering pressure-sensitive adhesive comprises the following steps:
setting the temperature of the reaction kettle at 130 ℃, sequentially adding dioctyl terephthalate and triphenyl phosphite into the reaction kettle from a feed inlet according to the formula, heating and stirring, and introducing nitrogen into the reaction kettle; adding SBS when the heating temperature reaches 130 deg.c, stirring and heating to 160 deg.c, maintaining the temperature and stirring for 130 min; after SBS is completely melted, reducing the temperature to 130 ℃, adding DCPD resin and other raw materials, stirring and maintaining the temperature until the mixture is completely melted; stopping heating, stopping introducing nitrogen, closing the charging port, vacuumizing the reaction kettle under the condition of continuously stirring until the vacuum pressure is 0.08MPa, keeping for 35 minutes, continuously vacuumizing for 6 minutes after stopping stirring, emptying, introducing compressed air with the pressure of 0.1MPa into the reaction kettle, discharging, cooling and subpackaging to obtain the product.
The masking pressure sensitive adhesive is made into a masking pressure sensitive adhesive tape by the following steps:
setting the temperature of the hot melt coating machine to 140 ℃, melting the covering pressure sensitive adhesive according to the ratio of 50g/m
2The coating weight is coated on a PET base film with the width of 1100mm and the thickness of 50um, then electron beam EB curing is carried out, a single-side coated release film is prepared and then the single-side coated release film is wound, the curing energy is 10kev, the dose is 150kGy, the irradiation height is 50mm, and the coating thickness of the covering pressure-sensitive adhesive is 40 mu m.
Example 4
The covering pressure-sensitive adhesive is prepared from the following raw materials, by weight, 25 parts of SBR, 35 parts of C9 modified DCPD resin, 9 parts of white oil, 2 parts of PETA, 5 parts of HDDA, 1.8 parts of gamma-methacryloxypropyl triisopropoxysilane, 0.5 part of phenyl diisooctyl phosphite, 2 parts of α type phthalocyanine blue (15: 1) and 6 parts of titanium dioxide.
The preparation method of the covering pressure-sensitive adhesive comprises the following steps:
setting the temperature of the reaction kettle at 130 ℃, sequentially adding white oil and diisooctyl phenyl phosphite into the reaction kettle from a feed inlet according to the formula, heating and stirring, and introducing nitrogen into the reaction kettle; adding SBR when the heating temperature reaches 130 ℃, continuously stirring and heating to 160 ℃, maintaining the temperature and stirring for 125 minutes; after the SBR is completely melted, reducing the temperature to 130 ℃, adding C9 modified DCPD resin and other raw materials, stirring and maintaining the temperature until the materials are completely melted; stopping heating, stopping introducing nitrogen, closing the charging port, vacuumizing the reaction kettle under the condition of continuously stirring until the vacuum pressure is 0.08MPa, keeping for 30 minutes, continuously vacuumizing for 6 minutes after stopping stirring, emptying, introducing compressed air with the pressure of 0.1MPa into the reaction kettle, discharging, cooling and subpackaging to obtain the product.
The masking pressure sensitive adhesive is made into a masking pressure sensitive adhesive tape by the following steps:
setting the temperature of the hot melt coating machine to 140 ℃, melting the covering pressure sensitive adhesive according to the ratio of 30g/m
2The coating weight is coated on a PET base film with the width of 1100mm and the thickness of 50um, then electron beam EB curing is carried out, a single-side coated release film is prepared, and then the single-side coated release film is wound, wherein the curing energy is 300kev, the dose is 5kGy, the irradiation height is 50mm, and the coating thickness of the covering pressure sensitive adhesive is 40 mu m.
Example 5
The covering pressure-sensitive adhesive is prepared from the following raw materials, by weight, 35 parts of POE, 45 parts of C9 resin, 8 parts of No. 40 engine oil, 5 parts of TAIC, 3 parts of DPGDA, 0.5 part of gamma-glycidyl ether oxypropyl trimethoxysilane, 0.9 part of β - (3, 5-di-tert-butyl-4-hydroxyphenyl) n-octadecyl propionate, 2.5 parts of β type phthalocyanine blue (15: 3), and 3 parts of calcium carbonate.
The preparation method of the covering pressure-sensitive adhesive comprises the following steps:
setting the temperature of a reaction kettle to 130 ℃, sequentially adding 40# engine oil and β - (3, 5-di-tert-butyl-4-hydroxyphenyl) n-octadecyl propionate into the reaction kettle from a feed inlet according to the formula, heating and stirring, simultaneously introducing nitrogen into the reaction kettle, adding POE when the heating temperature reaches 130 ℃, continuously stirring and heating to 160 ℃, maintaining the temperature and stirring for 120 minutes, reducing the temperature to 130 ℃ after the POE is completely dissolved, adding C9 resin and other raw materials, stirring and maintaining the temperature until the POE is completely dissolved, stopping heating and introducing nitrogen, closing the feed inlet, vacuumizing the reaction kettle under the condition of continuously stirring until the vacuum pressure is 0.08MPa and the vacuum pressure is maintained for 40 minutes, stopping stirring, continuously vacuumizing for 5 minutes, emptying, introducing compressed air with the pressure of 0.1MPa into the reaction kettle, discharging, cooling and subpackaging.
The masking pressure sensitive adhesive is made into a masking pressure sensitive adhesive tape by the following steps:
setting the temperature of the hot melt coating machine to 140 ℃, melting the covering pressure sensitive adhesive according to the ratio of 60g/m
2The coating weight is coated on a PET base film with the width of 1100mm and the thickness of 50um, then electron beam EB curing is carried out, the PET base film is prepared into a single-side coated release film and then is rolled, the single-side coated release film is obtained, the curing energy is 50kev, the dose is 50kGy, the irradiation height is 50mm, and the coating thickness of the pressure-sensitive adhesive is coveredAnd 40 μm.
Example 6
The covering pressure-sensitive adhesive is prepared from the following raw materials in parts by weight: POP 27 parts, rosin modified resin 36 parts, vacuum pump oil 6 parts, PETA 3.5 parts, TPGDA 4.5 parts, ethylene bis (oxyethylene) bis [3- (5-tert-butyl-4-hydroxy-m-tolyl) propionate ]1 part, gamma-type phthalocyanine blue (15: 6) 4.5 parts and barium sulfate 7 parts.
The preparation method of the covering pressure-sensitive adhesive comprises the following steps:
setting the temperature of the reaction kettle at 130 ℃, sequentially adding vacuum pump oil and ethylene bis (oxyethylene) bis [3- (5-tert-butyl-4-hydroxy-m-tolyl) propionate ] into the reaction kettle from a feed inlet according to the formula, heating and stirring, and introducing nitrogen into the reaction kettle; adding POP when the heating temperature reaches 130 ℃, continuously stirring and heating to 160 ℃, maintaining the temperature and stirring for 120 minutes; after the POP is completely melted, reducing the temperature to 130 ℃, adding rosin modified resin and other raw materials, stirring and maintaining the temperature until the POP is completely melted; stopping heating, stopping introducing nitrogen, closing the charging port, vacuumizing the reaction kettle under the condition of continuously stirring until the vacuum pressure is 0.08MPa, keeping the vacuum pressure for 40 minutes, stopping stirring, continuously vacuumizing for 5 minutes, emptying, introducing compressed air with the pressure of 0.1MPa into the reaction kettle, discharging, cooling and subpackaging to obtain the product.
The masking pressure sensitive adhesive is made into a masking pressure sensitive adhesive tape by the following steps:
setting the temperature of the hot melt coating machine to 140 ℃, melting the covering pressure sensitive adhesive according to the ratio of 70g/m
2The coating weight is coated on a PET base film with the width of 1100mm and the thickness of 50um, then electron beam EB curing is carried out, a single-side coated release film is prepared, and then the single-side coated release film is wound, wherein the curing energy is 400kev, the dose is 200kGy, the irradiation height is 50mm, and the coating thickness for covering the pressure-sensitive adhesive is 40 mu m.
Example 7
The covering pressure-sensitive adhesive is prepared from the following raw materials in parts by weight: 32 parts of SIS, 48 parts of rosin, 12 parts of naphthenic oil, 4.5 parts of TMPTA, 4 parts of HDDA, 2 parts of gamma-methacryloxypropyltrimethoxysilane, 0.01 part of 2, 2' -methylene bis- (4-methyl-6-tert-butylphenol), 5 parts of gamma-type phthalocyanine blue (15: 6) and 4 parts of kaolin.
The preparation method of the covering pressure-sensitive adhesive comprises the following steps:
setting the temperature of a reaction kettle at 130 ℃, sequentially adding naphthenic oil and 2, 2' -methylene bis- (4-methyl-6-tert-butylphenol) into the reaction kettle from a feed inlet according to the formula, heating and stirring, and introducing nitrogen into the reaction kettle; adding SIS when the heating temperature reaches 130 ℃, continuously stirring and heating to 160 ℃, maintaining the temperature and stirring for 120 minutes; after the SIS is completely melted, reducing the temperature to 130 ℃, adding rosin and other raw materials, stirring and maintaining the temperature until the SIS is completely melted; stopping heating, stopping introducing nitrogen, closing the charging port, vacuumizing the reaction kettle under the condition of continuously stirring until the vacuum pressure is 0.08MPa, keeping for 35 minutes, stopping stirring, continuously vacuumizing for 5 minutes, emptying, introducing compressed air with the pressure of 0.1MPa into the reaction kettle, discharging, cooling and subpackaging to obtain the product.
The masking pressure sensitive adhesive is made into a masking pressure sensitive adhesive tape by the following steps:
setting the temperature of the hot melt coating machine to 140 ℃, melting the covering pressure sensitive adhesive according to the ratio of 80g/m
2The coating weight is coated on a PET base film with the width of 1100mm and the thickness of 50um, then electron beam EB curing is carried out, a single-side coated release film is prepared, and then the single-side coated release film is wound, wherein the curing energy is 50kev, the dose is 80kGy, the irradiation height is 50mm, and the coating thickness of the covering pressure sensitive adhesive is 40 mu m.
Example 8
The covering pressure-sensitive adhesive is prepared from the following raw materials, by weight, 36 parts of SIS, 42 parts of terpene resin, 14 parts of white oil, 3 parts of TAIC, 4.5 parts of HDDA, 0.9 part of gamma-methacryloxypropyltrimethoxysilane, 0.3 part of 2, 2' -methylenebis- (4-methyl-6-tert-butylphenol), 3.5 parts of α type phthalocyanine blue (15: 1) and 9 parts of titanium dioxide.
The preparation method of the covering pressure-sensitive adhesive comprises the following steps:
setting the temperature of a reaction kettle at 130 ℃, sequentially adding white oil and 2, 2' -methylene bis- (4-methyl-6-tert-butylphenol) into the reaction kettle from a feed inlet according to the formula, heating and stirring, and introducing nitrogen into the reaction kettle; adding SIS when the heating temperature reaches 130 ℃, continuously stirring and heating to 160 ℃, maintaining the temperature and stirring for 115 minutes; after the SIS is completely melted, reducing the temperature to 130 ℃, adding terpene resin and other raw materials, stirring and maintaining the temperature until the SIS is completely melted; stopping heating, stopping introducing nitrogen, closing the charging port, vacuumizing the reaction kettle under the condition of continuously stirring until the vacuum pressure is 0.08MPa, keeping for 30 minutes, continuously vacuumizing for 5 minutes after stopping stirring, emptying, introducing compressed air with the pressure of 0.1MPa into the reaction kettle, discharging, cooling and subpackaging to obtain the product.
The masking pressure sensitive adhesive is made into a masking pressure sensitive adhesive tape by the following steps:
setting the temperature of the hot melt coating machine to 140 ℃, melting the covering pressure sensitive adhesive according to the ratio of 90g/m
2The coating weight is coated on a PET base film with the width of 1100mm and the thickness of 50um, then electron beam EB curing is carried out, a single-side coated release film is prepared, and then the single-side coated release film is wound, wherein the curing energy is 450kev, the dose is 90kGy, the irradiation height is 50mm, and the coating thickness of the covering pressure sensitive adhesive is 40 mu m.
The foregoing embodiments are merely illustrative of the principles and utilities of the present invention and are not intended to limit the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which can be made by those skilled in the art without departing from the spirit and technical spirit of the present invention be covered by the claims of the present invention.
Claims (10)
1. A masking pressure sensitive adhesive, characterized by: the feed is prepared from the following raw materials in parts by weight: 20-40 parts of elastomer, 30-50 parts of tackifier, 5-15 parts of softener, 2-5 parts of crosslinking agent, 3-5 parts of auxiliary crosslinking agent, 0-2 parts of coupling agent, 0.01-1 part of antioxidant, 1-5 parts of pigment and 3-10 parts of filler.
2. A masking pressure sensitive adhesive as defined in claim 1, wherein: the elastomer is one or a mixture of more than two of EVA, SIS, SBS, SBR, POE and POP.
3. A masking pressure sensitive adhesive as defined in claim 1, wherein: the tackifier is one or a mixture of more than two of C5 resin, DCPD resin, C9 modified DCPD resin, C9 resin, rosin modified resin, hydrogenated C5 resin, hydrogenated DCPD resin, rosin and terpene resin.
4. A masking pressure sensitive adhesive as defined in claim 1, wherein: the softener is one or a mixture of more than two of naphthenic oil, paraffin oil, dioctyl terephthalate, white oil, 40# engine oil and vacuum pump oil.
5. A masking pressure sensitive adhesive as defined in claim 1, wherein: the cross-linking agent is one or a mixture of more than two of trimethylolpropane acrylate TMPTA, triallyl isocyanurate TAIC, trimethylolpropane trimethacrylate TMPTMA and pentaerythritol triacrylate PETA.
6. A masking pressure sensitive adhesive as defined in claim 1, wherein: the auxiliary crosslinking agent is one or a mixture of more than two of 1, 6-hexanediol diacrylate HDDA, dipropylene glycol diacrylate DPGDA and tripropylene glycol diacrylate TPGDA.
7. The covering pressure-sensitive adhesive according to claim 1, wherein the coupling agent is one or a mixture of two or more of vinyltris (β -methoxyethoxy) silane, γ -methacryloxypropyltrimethoxysilane, γ -methacryloxypropyltriisopropoxysilane, and γ -glycidyloxypropyltrimethoxysilane, the antioxidant is one or a mixture of two or more of 2, 2' -methylenebis- (4-methyl-6-tert-butylphenol), diphenylisodecylphosphite, triphenylphosphite, diisooctylphenyl phosphite, n-octadecyl β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate, ethylenebis (oxyethylene) bis [3- (5-tert-butyl-4-hydroxy-m-tolyl) propionate ], tris (2, 4-di-tert-butylphenyl) phosphite, tetrakis (β - (3, 5-di-tert-butyl-4-hydroxyphenyl) propionate) pentaerythritol ester, the pigment is one or a mixture of two or more of vinyltris (α) -phthalocyanine blue, epsilon-type phthalocyanine blue, one or a mixture of two or a filler of phthalocyanine blue, and one or a mixture of calcium carbonate and a titanium pigment.
8. The method of preparing a masking pressure sensitive adhesive according to any one of claims 1-7, wherein: the method comprises the following steps:
setting the temperature of the reaction kettle at 130 ℃, sequentially adding a softener and an antioxidant into the reaction kettle from a feed inlet according to the formula, heating and stirring, and introducing nitrogen into the reaction kettle; adding the elastomer when the heating temperature reaches 130 ℃, continuously stirring and heating to 160 ℃, maintaining the temperature and stirring for 110-130 minutes; after the elastomer is completely melted, reducing the temperature to 130 ℃, adding the tackifier and other raw materials, stirring and maintaining the temperature until the elastomer is completely melted; stopping heating and stopping introducing nitrogen, closing the charging port, vacuumizing the reaction kettle under the condition of continuously stirring until the vacuum pressure is 0.08MPa and keeping the vacuum pressure for 30-40 minutes, continuously vacuumizing for 5-6 minutes after stopping stirring, evacuating the vacuum, introducing compressed air with the pressure of 0.1MPa into the reaction kettle, discharging, cooling and subpackaging to obtain the finished product.
9. Use of the masking pressure sensitive adhesive of any one of claims 1-7 in a masking pressure sensitive adhesive tape.
10. Use according to claim 9, characterized in that: the masking pressure sensitive tape is made by the steps of:
setting the temperature of the hot melt coating machine to 140 ℃, melting the covering pressure sensitive adhesive according to the ratio of 30-100g/m
2The coating weight is coated on a PET base film with the width of 1100mm and the thickness of 50um, then electron beam EB curing is carried out, a single-side coated release film is prepared, and then the coating is wound, wherein the curing energy is 10-500kev, and the dosage is 5-200 kGy.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112210329A (en) * | 2020-09-22 | 2021-01-12 | 广东新时代新材料科技有限公司 | Heat-sealing adhesive and preparation method and application thereof |
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| CN107743513A (en) * | 2015-06-17 | 2018-02-27 | 罗曼有限合资公司 | Bonding material |
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