CN115109529A - Anti-aging substrate-free easy-to-pull removable adhesive tape and preparation method thereof - Google Patents

Anti-aging substrate-free easy-to-pull removable adhesive tape and preparation method thereof Download PDF

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Publication number
CN115109529A
CN115109529A CN202111446855.3A CN202111446855A CN115109529A CN 115109529 A CN115109529 A CN 115109529A CN 202111446855 A CN202111446855 A CN 202111446855A CN 115109529 A CN115109529 A CN 115109529A
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China
Prior art keywords
adhesive tape
parts
aging
ethyl alcohol
removable adhesive
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CN202111446855.3A
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Inventor
顾正青
赵欣欣
周奎任
计建荣
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Suzhou Shihua New Material Technology Co ltd
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Suzhou Shihua New Material Technology Co ltd
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Priority to CN202111446855.3A priority Critical patent/CN115109529A/en
Publication of CN115109529A publication Critical patent/CN115109529A/en
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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
    • C09J7/10—Adhesives in the form of films or foils without carriers
    • 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
    • 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
    • C09J153/00—Adhesives based on block copolymers containing at least one sequence of a polymer obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
    • C09J153/02—Vinyl aromatic monomers and conjugated dienes
    • 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
    • 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
    • C09J7/40—Adhesives in the form of films or foils characterised by release liners
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/08—Metals
    • C08K2003/0843—Cobalt
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • 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
    • C09J2301/40—Additional features of adhesives in the form of films or foils characterized by the presence of essential components
    • C09J2301/408—Additional features of adhesives in the form of films or foils characterized by the presence of essential components additives as essential feature of the adhesive layer

Abstract

The invention provides an aging-resistant substrate-free easily-pulled removable adhesive tape and a preparation method thereof, wherein a crosslinking agent is added to crosslink thermoplastic rubber, so that a complex macromolecular chain crosslinked network structure is constructed, and the prepared adhesive tape has the advantages of excellent tensile strength, temperature resistance, aging resistance and the like; when the prepared adhesive tape needs to be removed, one end of the adhesive tape is held, the adhesive tape is kept at an angle of 0-90 degrees with the bonding interface and is stretched along the length direction, the adhesive tape can be smoothly removed without using large force, the use is convenient and simple, and no residual adhesive is left; the amount of biomass silicon carbon and modified nano silicon dioxide is limited to be added as heat-resistant filler, so that the aging rate of the adhesive tape can be inhibited; the modified nano-silica greatly improves the distribution uniformity of the nano-silica-loaded cobalt and chromium in the adhesive tape, enhances the complexity of macromolecular crosslinking in the adhesive tape and simultaneously improves the flame retardant property of the adhesive tape.

Description

Anti-aging substrate-free easy-to-pull removable adhesive tape and preparation method thereof
Technical Field
The invention relates to the field of adhesive tape preparation, in particular to an anti-aging non-substrate easy-to-pull removable adhesive tape and a preparation method thereof.
Background
The adhesive tape product is an indispensable daily necessity in modern society, and plays an important role in the fields of metal, glass, toys, artware, electronic products and the like. With the development of science and technology, adhesive tape products are increasingly popularized in modern electronic products such as smart phones and tablet computers, a plurality of adhesive tape products are only temporarily fixed in the process of product processing and need to be dismounted after sale or recycled by workers, and if electronic devices are difficult to dismount after being fixed by the adhesive tape, the use efficiency of the products and the working efficiency of the workers can be greatly reduced. Therefore, there is a high demand for tape products that have both good adhesive properties and easy removal when stretched. Therefore, the development of the easy-to-pull removable adhesive tape is of great significance.
Most of the currently available easy-to-pull removable adhesive tapes are insufficient in aging resistance, namely, after a sample is subjected to a double 85 aging test, the adhesive surface melts and collapses, or holes are generated on the adhesive surface, so that the adhesion reduction cannot be realized.
Disclosure of Invention
The invention aims to provide an anti-aging substrate-free easily-pulled removable adhesive tape and a preparation method thereof, so as to solve the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
an anti-aging substrate-free easy-to-pull removable adhesive tape comprises the following raw materials in percentage by weight: 70-130 parts of thermoplastic rubber, 50-130 parts of tackifying resin, 300 parts of toluene, 1-20 parts of softener, 1-10 parts of color paste and 0.1-10 parts of cross-linking agent.
Further, the thermoplastic rubber is one or a compound of styrene-isoprene-styrene and styrene-butadiene-styrene block copolymers.
Furthermore, the tackifying resin is prepared from terpene resin, modified resin and liquid rosin in a ratio, and the tackifying resin comprises the following components in parts by weight: 25-50 parts of terpene resin, 10-50 parts of modified resin and 10-15 parts of liquid rosin ester.
Furthermore, the softening point of the tackifying resin is 60-150 ℃.
Further, the modified resin is polymerized by pure aromatic petroleum monomers, and the softening point of the modified resin is 100-130 ℃. The modified resin was ytterbium-free Y612.
Further, the cross-linking agent is one or more of dicumyl peroxide, benzoyl peroxide, di-tert-butyl peroxide, dicumyl peroxide, 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane and triallyl cyanurate.
Further, the heat-resistant filler is one or more of silicon dioxide, carbon nano tubes and carbon fibers.
A preparation method of an anti-aging substrate-free easy-to-draw removable adhesive tape comprises the following steps:
(1) ultrasonically stirring tackifying resin, heat-resistant filler and toluene at 20-25 ℃, adding thermoplastic rubber for stirring after the tackifying resin, the heat-resistant filler and the toluene are completely dissolved, sequentially adding a softening agent, color paste and a crosslinking agent after the mixture is uniformly stirred, and uniformly stirring to obtain glue;
(2) the method comprises the steps of coating glue on a release film or release paper by adopting a coating mode, and adjusting the coating thickness to obtain the anti-aging substrate-free easily-pulled removable adhesive tape with the dry glue thickness of 10-200 mu m.
According to the invention, by adding the tackifying resin and the modifying resin with high softening points, the Tg of the whole system is increased, so that the temperature resistance of the adhesive tape is greatly improved; the adhesive tape prepared by the invention is not different from the common double-sided pressure-sensitive adhesive tape in bonding, the connection of different objects can be realized by applying pressure, when the adhesive tape needs to be removed, one end of the adhesive tape is held to keep a certain angle with a bonding interface and stretch along the length direction, the adhesive tape does not need to be pulled out and removed from the interface of the adherend smoothly by using large force, the use is convenient and simple, and no residual adhesive is left; the adhesive tape prepared by the invention is complete, resistant to high temperature and ageing, and can keep a complete adhesive surface after half a month in an ageing-resistant experiment at the temperature of 85 ℃ and the relative humidity of 85%, so that the viscosity reduction is realized, and the defects of the existing commercial products in the ageing resistance aspect are overcome.
Further, the heat-resistant filler is obtained by compounding modified nano silicon dioxide and biomass silicon carbon in a mass ratio of (1.8-3.2): 1; the preparation method of the modified nano silicon dioxide comprises the following steps:
s1, under the protection of nitrogen, ultrasonically stirring 3-aminopropyltriethoxysilane and absolute ethyl alcohol, then dropwise adding salicylaldehyde, continuously stirring for 8min, then heating to 75-80 ℃, carrying out reflux reaction for 3h under the protection of nitrogen, cooling to 15-25 ℃, heating to 60 ℃ by using a rotary evaporator, and carrying out rotary evaporation to obtain a silane-bridged salicylaldimine ligand;
s2, under the protection of nitrogen, ultrasonically stirring silane-bridged salicylaldimine ligand and absolute ethyl alcohol, dividing a ligand solution into 2 parts, marking as a solution A and a solution B, then dropwise adding a mixed solution of cobalt sulfate hexahydrate and ethyl alcohol into the solution A under the stirring condition, dropwise adding a mixed solution of chromium sulfate hexahydrate and ethyl alcohol into the solution B, refluxing for 12 hours at 75-80 ℃, cooling, filtering under negative pressure, washing the solid with absolute ethyl ether for 1-3 times, and drying under vacuum to obtain a Schiff base imine complex cobalt compound and a Schiff base imine complex chromium compound respectively;
s3, under the protection of nitrogen, ultrasonically stirring nano silicon dioxide and absolute ethyl alcohol, dropwise adding an absolute ethyl alcohol solution of a Schiff base imine complex cobalt substance and a Schiff base imine complex chromium substance, and refluxing for 24 hours at 75-80 ℃ in nitrogen; and (3) cooling, filtering under negative pressure, washing with absolute ethyl alcohol for 2-3 times, and drying in vacuum to obtain a mixture of Schiff base imine covalent modification nano-silica-loaded cobalt and Schiff base imine covalent modification nano-silica, so as to obtain the modified nano-silica.
Further, the molar ratio of the 3-aminopropyltriethoxysilane to the salicylaldehyde is 5: 6; the molar ratio of the cobalt sulfate hexahydrate to the silane-bridged salicylaldimine ligand is 2: 1; the molar ratio of the chromium sulfate hexahydrate to the silane-bridged salicylaldehyde is 7: 8; the molar ratio of the chromium sulfate hexahydrate to the cobalt sulfate hexahydrate is 1: 3.
Due to the introduction of the biomass silicon carbon, the tensile strength of the adhesive tape is greatly improved; under the condition of high-temperature thin oxygen, the molecular main chain in the adhesive tape can generate weak bond fracture to generate free radicals, so that crosslinking reaction is initiated, the number of intermolecular chemical crosslinking points is increased, the tensile strength is improved, but the crosslinking reaction is accumulated along with the prolonging of aging time, the strength is in a descending trend, and the mechanical property is more quickly attenuated when the temperature is higher, namely the aging rate is higher; the biomass silicon carbon is added into the adhesive tape as a heat-resistant filler, the introduction amount of the modified nano silicon dioxide and the biomass silicon carbon is limited, the tensile strength of the adhesive tape is synergistically improved, the arrangement structure of carbon atoms loaded on the surface has the density of a single electron cloud of a delocalized free radical, the capability of inhibiting the aging crosslinking reaction of the free radical is realized, and the dual effects of enhancing the crosslinking degree of the adhesive tape and resisting aging are achieved.
3-aminopropyltriethoxysilane is used as a bridging group, salicylaldehyde and a transition metal compound are used as raw materials, Schiff base imine complex transition metal substances with different structures are synthesized, the Schiff base imine complex transition metal substances are grafted on a nano material through covalent bond modification, and Schiff base imine covalent modification nano silicon dioxide loaded cobalt and chromium are synthesized to serve as modified nano silicon dioxide, so that the distribution uniformity of the nano silicon dioxide loaded cobalt and chromium in the adhesive tape is greatly improved, and the introduction of cobalt and chromium not only synergistically improves the mechanical strength of the adhesive tape, but also greatly improves the flame retardance of the adhesive tape; by limiting the introduction amount of cobalt and chromium, a complex macromolecular cross-linked network system is constructed in the adhesive tape, so that the adhesive tape has tensile strength and excellent aging resistance and flame retardance.
The invention has the beneficial effects that:
the invention provides an anti-aging substrate-free easily-pulled removable adhesive tape and a preparation method thereof, wherein a complex macromolecular chain cross-linked network structure is constructed by adding tackifying resin with a high softening point, so that the prepared adhesive tape has excellent tensile strength and has the advantages of good temperature resistance, no precipitation residue, anti-aging property and the like;
the adhesive tape prepared by the invention can realize the connection of different objects by applying pressure, and when the adhesive tape needs to be removed, as long as one end of the adhesive tape is held to keep an angle of 0-90 degrees with a bonding interface and is stretched along the length direction, molecules are subjected to orientation rearrangement, so that the adhesive tape can be smoothly pulled out from the interface of an adherend to be removed, the use is convenient and simple, and no residual adhesive is left; the adhesive tape prepared by the invention has high temperature resistance and ageing resistance, and after a double 85 ageing test, the adhesive surface is kept complete while the viscosity is reduced;
the amount of the biomass silicon carbon and the modified nano silicon dioxide is limited to be added as heat-resistant filler, so that the aging rate of the adhesive tape can be inhibited; the adhesive tape is filled with the reticular structure, so that the adhesive tape has high tensile strength and excellent aging resistance; the modified nano-silica is Schiff base imine covalent modification nano-silica supported cobalt and chromium, so that the distribution uniformity of the nano-silica supported cobalt and chromium in the adhesive tape is greatly improved, the macromolecular crosslinking complexity in the adhesive tape is enhanced, and the flame retardant property of the adhesive tape is improved.
Detailed Description
The technical solutions in the present invention will be described clearly and completely with reference to the following embodiments of the present invention, and it should be understood that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that if directional indications such as up, down, left, right, front and back … … are involved in the embodiment of the present invention, the directional indications are only used for explaining a specific posture such as relative position relationship between components, motion situation, etc., and if the specific posture is changed, the directional indication is changed accordingly. In addition, technical solutions between the embodiments may be combined with each other, but must be based on the realization of the technical solutions by a person skilled in the art, and when the technical solutions are contradictory to each other or cannot be realized, such a combination should not be considered to exist, and is not within the protection scope of the present invention.
The technical solutions of the present invention are further described in detail with reference to specific examples, which should be understood that the following examples are only illustrative of the present invention and are not intended to limit the present invention.
Example 1
100 parts of styrene-isoprene-styrene block copolymer and 70 parts of blended tackifying resin, wherein the blend comprises 25 parts of Keteng B115 terpene resin, 25 parts of tin-free remote modified resin Y61235 parts of stannum-free remote modified resin, 10 parts of crude Sichuan chemical liquid rosin ester, 170 parts of toluene, 1 part of Shanghai Jun Sheng crosslinking agent and heat-resistant filler of Kabot SiO 2 1 part of10 parts of softener and 2.5 parts of color paste;
dispersing SiO with toluene 2 Then dissolving the blended tackifying resin, sequentially adding the styrene-isoprene-styrene segmented copolymer, the color paste and the cross-linking agent, and uniformly stirring to obtain glue;
after complete dissolution, the coating thickness is adjusted by adopting a scraper coating mode, the glue is coated on a release film, the release film is dried for 3min at 120 ℃, and the dried release film is cured in a drying oven at 48 ℃ for 12h to obtain the anti-aging non-substrate easy-to-pull removable adhesive tape with the dry glue thickness of 100 mu m.
Example 2
100 parts of styrene-isoprene-styrene block copolymer and 100 parts of blended tackifying resin, wherein the blend comprises 40 parts of Keteng B115 terpene resin, 40 parts of tin-free remote modified resin Y61250 parts of stannum-free remote modified resin, 10 parts of crude Sichuan chemical liquid rosin ester, 200 parts of toluene, 2 parts of Shanghai junsheng cross-linking agent and heat-resistant filler which is Kabot SiO 2 2 parts of softener, 10 parts of color paste and 2.5 parts of color paste;
dispersing SiO with toluene 2 Then dissolving the blended tackifying resin, sequentially adding the styrene-isoprene-styrene segmented copolymer, the color paste and the cross-linking agent, and uniformly stirring to obtain glue;
after complete dissolution, the coating thickness is adjusted by adopting a scraper coating mode, the glue is coated on a release film, the release film is dried for 3min at 120 ℃, and the dried release film is cured in a drying oven at 48 ℃ for 12h to obtain the anti-aging non-substrate easy-to-pull removable adhesive tape with the dry glue thickness of 100 mu m.
Example 3
100 parts of styrene-isoprene-styrene block copolymer and 130 parts of blended tackifying resin, wherein the blend comprises 50 parts of Keteng B115 terpene resin, 50 parts of tin-free remote modified resin Y61265 parts, 15 parts of crude chemical liquid rosin ester, 230 parts of toluene, 2 parts of cross-linking agent of Shanghai Jun Sheng and SiO of Kabot as heat-resistant filler 2 3 parts of color paste 2.5 parts of softening agent 10 parts;
dispersing SiO with toluene 2 Then dissolving the blended tackifying resin, sequentially adding the styrene-isoprene-styrene segmented copolymer, the color paste and the cross-linking agent, and stirringObtaining glue after the glue is uniform;
after complete dissolution, the coating thickness is adjusted by adopting a scraper coating mode, glue is coated on a release film, the release film is dried for 3min at 120 ℃, the dried release film is attached to two sides of a base material, and the base material-free easy-to-pull removable adhesive tape with the dry adhesive thickness of 100 mu m is obtained after curing in a 48 ℃ oven for 12 h.
Example 4
(1) Ultrasonically stirring tackifying resin, heat-resistant filler and toluene at 20 ℃, adding thermoplastic rubber for stirring after the tackifying resin, the heat-resistant filler and the toluene are completely dissolved, sequentially adding a softening agent, color paste and a crosslinking agent after the materials are uniformly stirred, and uniformly stirring to obtain glue;
the raw materials comprise the following components in parts by weight: 70 parts of thermoplastic rubber, 50 parts of tackifying resin, 100 parts of toluene, 1 part of softener, 1 part of color paste, 0.1 part of cross-linking agent and 1 part of heat-resistant filler;
the thermoplastic rubber is a styrene-isoprene-styrene block copolymer; the cross-linking agent is benzoyl peroxide; the tackifying resin comprises the following components in parts by weight: 25 parts of Keteng B115 terpene resin, Y61215 parts of tin-free remote modified resin and 10 parts of Sichuan chemical liquid rosin ester;
the heat-resistant filler is obtained by compounding modified nano silicon dioxide and biomass silicon carbon in a mass ratio of 1.8: 1; the preparation method of the modified nano silicon dioxide comprises the following steps:
s1, under the protection of nitrogen, ultrasonically stirring 3-aminopropyltriethoxysilane and absolute ethyl alcohol, then dropwise adding salicylaldehyde, continuously stirring for 8min, then heating to 75 ℃, carrying out reflux reaction for 3h under the protection of nitrogen, cooling to 15 ℃, heating to 60 ℃ by using a rotary evaporator, and carrying out rotary evaporation to obtain a silane bridging salicylaldehyde imine ligand;
s2, under the protection of nitrogen, ultrasonically stirring silane-bridged salicylaldimine ligand and absolute ethyl alcohol, dividing a ligand solution into 2 parts, recording as a solution A and a solution B, then dropwise adding a mixed solution of cobalt sulfate hexahydrate and ethyl alcohol into the solution A under the stirring condition, dropwise adding a mixed solution of chromium sulfate hexahydrate and ethyl alcohol into the solution B, refluxing for 12 hours at 75 ℃, cooling, filtering under negative pressure, washing the solid for 1 time by using absolute ethyl ether, and drying under vacuum to obtain a Schiff base imine complex cobalt compound and a Schiff base imine complex chromium compound respectively;
s3, under the protection of nitrogen, ultrasonically stirring nano silicon dioxide and absolute ethyl alcohol, dropwise adding an absolute ethyl alcohol solution of Schiff base imine complex cobalt matter and Schiff base imine complex chromium matter, and refluxing for 24 hours at 75 ℃ in nitrogen; cooling, filtering under negative pressure, washing with absolute ethyl alcohol for 2 times, and drying in vacuum to obtain a mixture of Schiff base imine covalent modification nano-silica loaded cobalt and Schiff base imine covalent modification nano-silica to obtain modified nano-silica;
the molar ratio of the 3-aminopropyltriethoxysilane to the salicylaldehyde is 5: 6; the molar ratio of the cobalt sulfate hexahydrate to the silane-bridged salicylaldimine ligand is 2: 1; the molar ratio of the chromium sulfate hexahydrate to the silane-bridged salicylaldehyde is 7: 8; the molar ratio of the chromium sulfate hexahydrate to the cobalt sulfate hexahydrate is 1: 3;
the molar weight of the salicylaldehyde is 6 mmol; the molar weight of the cobalt sulfate hexahydrate is 6 mmol; 5mmol of nano silicon dioxide and 100ml of absolute ethyl alcohol; 0.3mmol of Schiff base imine complex cobalt compound and 0.1mmol of Schiff base imine complex chromium compound;
(2) the method comprises the steps of coating glue on a release film in a coating mode, and adjusting the coating thickness to obtain the anti-aging substrate-free easily-pulled removable adhesive tape with the dry glue thickness of 100 micrometers.
Example 5
(1) Ultrasonically stirring tackifying resin, heat-resistant filler and toluene at 22 ℃, adding thermoplastic rubber for stirring after the tackifying resin, the heat-resistant filler and the toluene are completely dissolved, sequentially adding a softening agent, color paste and a crosslinking agent after the materials are uniformly stirred, and uniformly stirring to obtain glue;
the raw materials comprise the following components in parts by weight: 100 parts of thermoplastic rubber, 70 parts of tackifying resin, 170 parts of toluene, 10 parts of softener, 2.5 parts of color paste, 1 part of cross-linking agent and 2 parts of heat-resistant filler;
the thermoplastic rubber is a styrene-butadiene-styrene block copolymer;
the cross-linking agent is prepared from benzoyl peroxide and triallyl cyanurate according to the mass ratio of 1: 1;
the tackifying resin comprises the following components in parts by weight: 25 parts of Keteng B115 terpene resin, Y61235 parts of tin-free remote modified resin and 10 parts of Sichuan chemical liquid rosin ester;
the heat-resistant filler is obtained by compounding modified nano silicon dioxide and biomass silicon carbon according to the mass ratio of 2.4: 1; the preparation method of the modified nano silicon dioxide comprises the following steps:
s1, under the protection of nitrogen, ultrasonically stirring 3-aminopropyltriethoxysilane and absolute ethyl alcohol, then dropwise adding salicylaldehyde, continuously stirring for 8min, then heating to 78 ℃, carrying out reflux reaction for 3h under the protection of nitrogen, cooling to 20 ℃, heating to 60 ℃ by using a rotary evaporator, and carrying out rotary evaporation to obtain a silane bridging salicylaldehyde imine ligand;
s2, under the protection of nitrogen, ultrasonically stirring silane-bridged salicylaldimine ligand and absolute ethyl alcohol, dividing a ligand solution into 2 parts, marking as a solution A and a solution B, then dropwise adding a mixed solution of cobalt sulfate hexahydrate and ethyl alcohol into the solution A under the stirring condition, dropwise adding a mixed solution of chromium sulfate hexahydrate and ethyl alcohol into the solution B, refluxing for 12 hours at 78 ℃, cooling, filtering under negative pressure, washing the solid for 2 times by using absolute ethyl ether, and drying under vacuum to obtain a Schiff base imine complex cobalt compound and a Schiff base imine complex chromium compound respectively;
s3, under the protection of nitrogen, ultrasonically stirring nano silicon dioxide and absolute ethyl alcohol, dropwise adding an absolute ethyl alcohol solution of Schiff base imine complex cobalt matter and Schiff base imine complex chromium matter, and refluxing for 24 hours at 78 ℃ in nitrogen; cooling, filtering under negative pressure, washing for 3 times by using absolute ethyl alcohol, and drying in vacuum to obtain a mixture of Schiff base imine covalent modified nano-silica supported cobalt and Schiff base imine covalent modified nano-silica, so as to obtain modified nano-silica;
the molar ratio of the 3-aminopropyltriethoxysilane to the salicylaldehyde is 5: 6; the molar ratio of the cobalt sulfate hexahydrate to the silane-bridged salicylaldimine ligand is 2: 1; the molar ratio of the chromium sulfate hexahydrate to the silane-bridged salicylaldehyde is 7: 8; the molar ratio of the chromium sulfate hexahydrate to the cobalt sulfate hexahydrate is 1: 3;
the molar weight of the salicylaldehyde is 6 mmol; the molar weight of the cobalt sulfate hexahydrate is 6 mmol; 5mmol of nano silicon dioxide and 100ml of absolute ethyl alcohol; 0.3mmol of Schiff base imine complex cobalt compound and 0.1mmol of Schiff base imine complex chromium compound;
(2) the glue is coated on the release film by adopting a coating mode, and the coating thickness is adjusted to obtain the anti-aging substrate-free easily-pulled removable adhesive tape with the dry glue thickness of 100 mu m.
Example 6
(1) Ultrasonically stirring tackifying resin, heat-resistant filler and toluene at 25 ℃, adding thermoplastic rubber for stirring after the tackifying resin, the heat-resistant filler and the toluene are completely dissolved, sequentially adding a softening agent, color paste and a crosslinking agent after the materials are uniformly stirred, and uniformly stirring to obtain glue;
the raw materials comprise the following components in parts by weight: 130 parts of thermoplastic rubber, 130 parts of tackifying resin, 300 parts of toluene, 20 parts of softener, 10 parts of color paste, 10 parts of cross-linking agent and 3 parts of heat-resistant filler;
the thermoplastic rubber is prepared from styrene-isoprene-styrene and styrene-butadiene-styrene block copolymers in a mass ratio of 1: 1;
the cross-linking agent is benzoyl peroxide;
the tackifying resin comprises the following components in parts by weight: 50 parts of Keteng B115 terpene resin, 50 parts of tin-free ytterbium modified resin Y61265 parts and 15 parts of crude Sichuan chemical liquid rosin ester;
the heat-resistant filler is obtained by compounding modified nano silicon dioxide and biomass silicon carbon in a mass ratio of 3.2: 1; the preparation method of the modified nano silicon dioxide comprises the following steps:
s1, under the protection of nitrogen, ultrasonically stirring 3-aminopropyltriethoxysilane and absolute ethyl alcohol, then dropwise adding salicylaldehyde, continuously stirring for 8min, then heating to 80 ℃, carrying out reflux reaction for 3h under the protection of nitrogen, cooling to 25 ℃, heating to 60 ℃ by using a rotary evaporator, and carrying out rotary evaporation to obtain a silane bridging salicylaldehyde imine ligand;
s2, under the protection of nitrogen, ultrasonically stirring silane-bridged salicylaldimine ligand and absolute ethyl alcohol, dividing a ligand solution into 2 parts, recording as a solution A and a solution B, then dropwise adding a mixed solution of cobalt sulfate hexahydrate and ethyl alcohol into the solution A under the stirring condition, dropwise adding a mixed solution of chromium sulfate hexahydrate and ethyl alcohol into the solution B, refluxing for 12 hours at 80 ℃, cooling, filtering under negative pressure, washing the solid for 3 times by using absolute ethyl ether, and drying under vacuum to respectively obtain a Schiff base imine complex cobalt substance and a Schiff base imine complex chromium substance;
s3, under the protection of nitrogen, ultrasonically stirring nano silicon dioxide and absolute ethyl alcohol, dropwise adding an absolute ethyl alcohol solution of Schiff base imine complex cobalt matter and Schiff base imine complex chromium matter, and refluxing for 24 hours at 80 ℃ in nitrogen; cooling, filtering under negative pressure, washing with absolute ethyl alcohol for 2-3 times, and drying in vacuum to obtain a mixture of Schiff base imine covalent modified nano-silica supported cobalt and Schiff base imine covalent modified nano-silica, so as to obtain modified nano-silica;
the molar ratio of the 3-aminopropyltriethoxysilane to the salicylaldehyde is 5: 6; the molar ratio of the cobalt sulfate hexahydrate to the silane-bridged salicylaldimine ligand is 2: 1; the molar ratio of the chromium sulfate hexahydrate to the silane-bridged salicylaldehyde is 7: 8; the molar ratio of the chromium sulfate hexahydrate to the cobalt sulfate hexahydrate is 1: 3;
the molar weight of the salicylaldehyde is 6 mmol; the molar weight of the cobalt sulfate hexahydrate is 6 mmol; 5mmol of nano silicon dioxide and 100ml of absolute ethyl alcohol; 0.3mmol of Schiff base imine complex cobalt compound and 0.1mmol of Schiff base imine complex chromium compound;
(2) the method comprises the steps of coating glue on a release film in a coating mode, and adjusting the coating thickness to obtain the anti-aging substrate-free easily-pulled removable adhesive tape with the dry glue thickness of 100 micrometers.
Comparative example 1
(1) Ultrasonically stirring tackifying resin, heat-resistant filler and toluene at 25 ℃, adding thermoplastic rubber for stirring after the tackifying resin, the heat-resistant filler and the toluene are completely dissolved, sequentially adding a softening agent, color paste and a crosslinking agent after the materials are uniformly stirred, and uniformly stirring to obtain glue;
the raw materials comprise the following components in parts by weight: 130 parts of thermoplastic rubber, 130 parts of tackifying resin, 300 parts of toluene, 20 parts of softener, 10 parts of color paste, 10 parts of cross-linking agent and 3 parts of heat-resistant filler;
the thermoplastic rubber is prepared from styrene-isoprene-styrene and styrene-butadiene-styrene block copolymers in a mass ratio of 1: 1;
the cross-linking agent is benzoyl peroxide;
the tackifying resin comprises the following components in parts by weight: 50 parts of Keteng B115 terpene resin, 50 parts of tin-free remote modified resin Y61265 parts of Siberian ytterbium and Sichuan chemical liquid rosin ester and 15 parts of Siberian ytterbium and Siberian ytterbium chemical liquid rosin ester;
the heat-resistant filler is modified nano silicon dioxide; the preparation method of the modified nano silicon dioxide comprises the following steps:
s1, under the protection of nitrogen, ultrasonically stirring 3-aminopropyltriethoxysilane and absolute ethyl alcohol, then dropwise adding salicylaldehyde, continuously stirring for 8min, then heating to 80 ℃, carrying out reflux reaction for 3h under the protection of nitrogen, cooling to 25 ℃, heating to 60 ℃ by using a rotary evaporator, and carrying out rotary evaporation to obtain a silane-bridged salicylaldimine ligand;
s2, under the protection of nitrogen, ultrasonically stirring silane-bridged salicylaldimine ligand and absolute ethyl alcohol, dividing a ligand solution into 2 parts, marking as a solution A and a solution B, then dropwise adding a mixed solution of cobalt sulfate hexahydrate and ethyl alcohol into the solution A under the stirring condition, dropwise adding a mixed solution of chromium sulfate hexahydrate and ethyl alcohol into the solution B, refluxing for 12 hours at 80 ℃, cooling, filtering under negative pressure, washing the solid for 3 times by using absolute ethyl ether, and drying under vacuum to obtain a Schiff base imine complex cobalt compound and a Schiff base imine complex chromium compound respectively;
s3, under the protection of nitrogen, ultrasonically stirring nano silicon dioxide and absolute ethyl alcohol, dropwise adding an absolute ethyl alcohol solution of a Schiff base imine complex cobalt substance and a Schiff base imine complex chromium substance, and refluxing for 24 hours at 80 ℃ in nitrogen; cooling, filtering under negative pressure, washing with absolute ethyl alcohol for 3 times, and drying in vacuum to obtain a mixture of Schiff base imine covalent modification nano-silica loaded cobalt and Schiff base imine covalent modification nano-silica to obtain modified nano-silica;
the molar ratio of the 3-aminopropyltriethoxysilane to the salicylaldehyde is 5: 6; the molar ratio of the cobalt sulfate hexahydrate to the silane-bridged salicylaldimine ligand is 2: 1; the molar ratio of the chromium sulfate hexahydrate to the silane-bridged salicylaldehyde is 7: 8; the molar ratio of the chromium sulfate hexahydrate to the cobalt sulfate hexahydrate is 1: 3;
the molar weight of the salicylaldehyde is 6 mmol; the molar weight of the cobalt sulfate hexahydrate is 6 mmol; 5mmol of nano silicon dioxide and 100ml of absolute ethyl alcohol; 0.3mmol of Schiff base imine complex cobalt compound and 0.1mmol of Schiff base imine complex chromium compound;
(2) the glue is coated on the release film by adopting a coating mode, and the coating thickness is adjusted to obtain the anti-aging substrate-free easily-pulled removable adhesive tape with the dry glue thickness of 100 mu m.
Comparative example 2
(1) Ultrasonically stirring tackifying resin, heat-resistant filler and toluene at 25 ℃, adding thermoplastic rubber for stirring after the tackifying resin, the heat-resistant filler and the toluene are completely dissolved, sequentially adding a softening agent, color paste and a crosslinking agent after the materials are uniformly stirred, and uniformly stirring to obtain glue;
the raw materials comprise the following components in parts by weight: 130 parts of thermoplastic rubber, 130 parts of tackifying resin, 300 parts of toluene, 20 parts of softener, 10 parts of color paste, 10 parts of cross-linking agent and 3 parts of heat-resistant filler;
the thermoplastic rubber is prepared from styrene-isoprene-styrene and styrene-butadiene-styrene block copolymers in a mass ratio of 1: 1;
the cross-linking agent is benzoyl peroxide;
the tackifying resin comprises the following components in parts by weight: 50 parts of Keteng B115 terpene resin, 50 parts of tin-free remote modified resin Y61265 parts of Siberian ytterbium and Sichuan chemical liquid rosin ester and 15 parts of Siberian ytterbium and Siberian ytterbium chemical liquid rosin ester; the heat-resistant filler is biomass silicon carbon;
(2) the method comprises the steps of coating glue on a release film in a coating mode, and adjusting the coating thickness to obtain the anti-aging substrate-free easily-pulled removable adhesive tape with the dry glue thickness of 100 micrometers.
And (3) performance testing: the tapes prepared in examples 1 to 6 and comparative examples 1 to 2 were tested for thickness, peel force, tensile strength, elongation at break, aged white fog, and aged property, and the test results are shown in table 1;
1. the peel force of the prepared tape was measured with reference to the method of ASTM-D3330; after the sample is cured, standing for 48h in an environment of 23 ℃/50% RH; cutting an adhesive tape to prepare samples, wherein the length and the width are respectively 15cm multiplied by 2cm, tearing off a light release film, covering PET with the thickness of 23um, tearing off the other side of the light release film, sticking the heavy release film on a steel plate, grinding an adhered body which is an SUS304 steel plate by 280 # waterproof abrasive paper, after sticking, pressing back for 3 times by using a 2kg rubber roller, standing for 20min, peeling at 180 degrees at the speed of 300mm/min, and measuring the measured peeling strength as peeling force (gf/20 mm);
2. tensile strength, elongation at break, were tested with reference to ASTM-D3759; cutting the adhesive tape to prepare samples, wherein the length and the width are respectively 80mm multiplied by 15mm, and the gauge length is 20 mm;
3. aging white fog: after the sample is cured, standing for 24h in an environment of 23 ℃/50% RH; flatly attaching the tested adhesive tape to a clean glass plate, placing the glass plate in a constant temperature and humidity box with the temperature of 85 ℃/85% RH, taking out the glass plate after 15 days, standing the glass plate for 2.0 hours, tearing off the adhesive tape, and observing whether the surface of the glass plate appears white fog or not at different angles under a color comparison box;
4. aging performance: after the sample is cured, standing for 24h in an environment of 23 ℃/50% RH; then placing the adhesive tape in a constant temperature and humidity box with the temperature of 85 ℃/85% RH, taking out after 15d, standing for 2.0h to observe whether the surface of the adhesive tape is intact and has no holes, and testing the stripping force and the tensile strength; the test results are shown in table 1;
Figure RE-GDA0003516213730000111
TABLE 1
As can be seen from examples 1 to 3, the adhesive tape prepared according to the present invention did not decrease in peel force under long-term high temperature and high humidity; as can be seen from comparison between the example 5 and the example 2, when the added heat-resistant filler is modified silica and biomass silicon carbon, the peeling force is large enough and cannot be reduced along with the increase of time, the peeling force cannot be reduced under long-term high temperature and high humidity, pollution such as residual glue and the like cannot be generated, the temperature resistance of the adhesive tape can be enhanced, and the adhesive tape is soft and cannot rebound to cause adverse effect on shaping when needing to be bent; the comparison between example 6 and comparative examples 1 and 2 shows that the addition amounts of the modified silica and the biomass silicon carbon are limited, and the additive amount has a synergistic effect on the improvement of the mechanical property in the adhesive tape.
The anti-aging substrate-free easy-to-pull removable adhesive tape prepared by the invention can realize the connection of different objects by applying pressure, and when the adhesive tape needs to be removed, the adhesive tape can generate serious yield deformation as long as one end of the adhesive tape is held to keep a certain angle with a bonding interface and is forcibly stretched along the length direction, so that the adhesive tape can be smoothly pulled out and removed from the interface of the adhered object, the use is convenient and simple, and no residual adhesive is left; the adhesive tape prepared by the invention is complete, resistant to high temperature and ageing, and can keep a complete adhesive surface after 15 days in an ageing-resistant experiment at the temperature of 85 ℃ and the relative humidity of 85%, so that the viscosity is reduced, and the defects of the existing commercial products in the ageing resistance aspect are overcome.
The above description is only an example of the present invention, and is not intended to limit the scope of the present invention, and all modifications and equivalents of the present invention, which are made by the present specification and directly/indirectly applied to other related technical fields, are included in the scope of the present invention.

Claims (10)

1. An anti-aging non-substrate easy-to-pull removable adhesive tape is characterized in that the adhesive tape comprises the following components in parts by weight: 70-130 parts of thermoplastic rubber, 50-130 parts of tackifying resin, 300 parts of toluene, 1-20 parts of softening agent, 1-10 parts of color paste, 0.1-10 parts of cross-linking agent and 1-3 parts of heat-resistant filler.
2. The aging-resistant substrate-free easy-to-open removable adhesive tape according to claim 1, wherein the thermoplastic rubber is one or a combination of styrene-isoprene-styrene and styrene-butadiene-styrene block copolymers.
3. The aging-resistant substrate-free easy-to-draw removable adhesive tape as claimed in claim 1, wherein the tackifying resin is prepared from terpene resin, modified resin and liquid rosin in a proportion, and the tackifying resin comprises the following components in parts by weight: 25-50 parts of terpene resin, 10-50 parts of modified resin and 10-15 parts of liquid rosin ester.
4. The aging-resistant substrate-free easy open removable tape of claim 1, wherein the tackifying resin has a softening point of 60 to 150 ℃.
5. The aging-resistant substrate-free easy-to-open removable adhesive tape as claimed in claim 3, wherein the modified resin is prepared by polymerizing pure aromatic petroleum monomers, and the pure aromatic petroleum monomers are prepared by polymerizing styrene monomers and alpha-methyl styrene monomers; the modified resin has a softening point of 100-130 ℃.
6. An aging-resistant substrate-free easy open removable adhesive tape according to claim 1, wherein the crosslinking agent is one or more of dicumyl peroxide, benzoyl peroxide, di-tert-butyl peroxide, dicumyl peroxide, 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane, and triallyl cyanurate.
7. A preparation method of an anti-aging substrate-free easy-to-draw removable adhesive tape is characterized by comprising the following steps:
(1) ultrasonically stirring tackifying resin, heat-resistant filler and toluene at 20-25 ℃, adding thermoplastic rubber for stirring after the tackifying resin, the heat-resistant filler and the toluene are completely dissolved, sequentially adding a softening agent, color paste and a crosslinking agent after the mixture is uniformly stirred, and uniformly stirring to obtain glue;
(2) the method is characterized in that glue is coated on a release film or release paper in a coating mode, and the coating thickness is adjusted to obtain the anti-aging substrate-free easily-pulled removable adhesive tape with the dry glue thickness of 10-200 mu m.
8. The preparation method of the aging-resistant substrate-free easy-to-draw removable adhesive tape as claimed in claim 7, wherein the heat-resistant filler is prepared by compounding modified nano silica and biomass silicon carbon in a mass ratio of (1.8-3.2): 1.
9. The preparation method of the aging-resistant substrate-free easy-to-draw removable adhesive tape as claimed in claim 8, wherein the preparation method of the modified nano silica comprises the following steps:
s1, under the protection of nitrogen, ultrasonically stirring 3-aminopropyltriethoxysilane and absolute ethyl alcohol, then dropwise adding salicylaldehyde, continuously stirring for 8min, then heating to 75-80 ℃, carrying out reflux reaction for 3h under the protection of nitrogen, cooling to 15-25 ℃, heating to 60 ℃ by using a rotary evaporator, and carrying out rotary evaporation to obtain a silane-bridged salicylaldimine ligand;
s2, under the protection of nitrogen, ultrasonically stirring silane-bridged salicylaldimine ligand and absolute ethyl alcohol, dividing a ligand solution into 2 parts, marking as a solution A and a solution B, then dropwise adding a mixed solution of cobalt sulfate hexahydrate and ethyl alcohol into the solution A under the stirring condition, dropwise adding a mixed solution of chromium sulfate hexahydrate and ethyl alcohol into the solution B, refluxing for 12 hours at 75-80 ℃, cooling, filtering under negative pressure, washing the solid with absolute ethyl ether for 1-3 times, and drying under vacuum to obtain a Schiff base imine complex cobalt compound and a Schiff base imine complex chromium compound respectively;
s3, under the protection of nitrogen, ultrasonically stirring nano silicon dioxide and absolute ethyl alcohol, dropwise adding an absolute ethyl alcohol solution of a Schiff base imine complex cobalt substance and a Schiff base imine complex chromium substance, and refluxing for 24 hours at 75-80 ℃ in nitrogen; and (3) cooling, filtering under negative pressure, washing with absolute ethyl alcohol for 2-3 times, and drying in vacuum to obtain the modified nano silicon dioxide.
10. The method of claim 9, wherein the molar ratio of 3-aminopropyltriethoxysilane to salicylaldehyde is 5: 6; the molar ratio of the cobalt sulfate hexahydrate to the silane-bridged salicylaldimine ligand is 2: 1; the molar ratio of the chromium sulfate hexahydrate to the silane-bridged salicylaldehyde is 7: 8; the molar ratio of the chromium sulfate hexahydrate to the cobalt sulfate hexahydrate is 1: 3.
CN202111446855.3A 2021-11-30 2021-11-30 Anti-aging substrate-free easy-to-pull removable adhesive tape and preparation method thereof Pending CN115109529A (en)

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