CN111607344A - Oil-seepage-resistant low-temperature-resistant high-peeling-force hot-melt pressure-sensitive adhesive and preparation method thereof - Google Patents

Oil-seepage-resistant low-temperature-resistant high-peeling-force hot-melt pressure-sensitive adhesive and preparation method thereof Download PDF

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CN111607344A
CN111607344A CN202010368743.XA CN202010368743A CN111607344A CN 111607344 A CN111607344 A CN 111607344A CN 202010368743 A CN202010368743 A CN 202010368743A CN 111607344 A CN111607344 A CN 111607344A
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sensitive adhesive
melt pressure
thermoplastic elastomer
hot melt
pressure sensitive
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王泽洲
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Zhejiang Jinjia Technology Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J153/00Adhesives 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
    • C09J153/02Vinyl aromatic monomers and conjugated dienes
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J11/00Features of adhesives not provided for in group C09J9/00, e.g. additives
    • C09J11/08Macromolecular additives
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J145/00Adhesives based on homopolymers or copolymers of compounds having no unsaturated aliphatic radicals in a side chain, and having one or more carbon-to-carbon double bonds in a carbocyclic or in a heterocyclic system; Adhesives based on derivatives of such polymers
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J157/00Adhesives based on unspecified polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2207/00Properties characterising the ingredient of the composition
    • C08L2207/04Thermoplastic elastomer

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Abstract

The invention discloses an oil-seepage-resistant low-temperature-resistant high-peeling-force-resistant hot-melt pressure-sensitive adhesive and a preparation method thereof, wherein the hot-melt pressure-sensitive adhesive comprises the following raw materials in parts by weight: 5-30 parts of thermoplastic elastomer; 5-30 parts of a second thermoplastic elastomer; 5-30 parts of a thermoplastic elastomer; 0-5 parts of a plasticizer; 5-20 parts of low-molecular-weight synthetic liquid polybutadiene rubber; 20-40 parts of tackifying resin; 10-30 parts of a second tackifying resin; 0.2-2 parts of antioxidant; the oil-permeation-resistant low-temperature-resistant high-peeling-force-resistant hot-melt pressure-sensitive adhesive and the preparation method thereof disclosed by the invention meet the technical requirements of downstream application on oil permeation resistance, high peeling force and low temperature resistance, and effectively ensure the oil permeation resistance, high peeling force and low temperature resistance of a hot-melt pressure-sensitive adhesive product.

Description

Oil-seepage-resistant low-temperature-resistant high-peeling-force hot-melt pressure-sensitive adhesive and preparation method thereof
Technical Field
The invention belongs to the technical field of high-molecular adhesives, and particularly relates to an oil-seepage-resistant low-temperature-resistant high-peeling-force hot-melt pressure-sensitive adhesive and a preparation method thereof.
Background
The hot melt pressure sensitive adhesive is an adhesive which takes thermoplastic rubber as a base material, integrates the characteristics of heat collection melt adhesive and pressure sensitive adhesive, has no solvent, no pollution and convenient use. The adhesive is coated in a molten state, and can be quickly bonded by applying slight finger pressure after being cooled and hardened. At present, the hot melt pressure sensitive adhesive is widely applied to the aspects of automobiles, sanitary products, adhesive tapes, labels, medical treatment and health, surface protection films, wood processing, shoe making and the like.
In recent years, with the improvement of living standard of people, the requirements of the technical field of polymer bonding on various composite materials are higher and higher, and especially higher requirements are provided for the oil permeability resistance of hot melt pressure sensitive adhesives in the application of some paper labels. The paper material is used as a coating substrate of the hot-melt pressure-sensitive adhesive, and can easily absorb the plasticizer in the components of the hot-melt pressure-sensitive adhesive, so that the component proportion of the hot-melt pressure-sensitive adhesive is changed, and the bonding performance of the hot-melt pressure-sensitive adhesive after being stored for a period of time is unstable, such as initial adhesion, stripping force, low temperature resistance, high temperature resistance and the like. The above-described occurrence of unstable variations in adhesion properties is unacceptable for downstream product applications. If a hot melt pressure sensitive adhesive whose plasticizer does not migrate to the paper substrate is developed, it is hoped to solve the problem of unstable adhesive property.
Because the application field of the hot melt pressure sensitive adhesive is more and more extensive, the requirement on the stripping force of the hot melt adhesive is higher and higher. The hot melt pressure sensitive adhesive has the advantages that the higher peeling force can be achieved under the same adhesive coating amount, or the lower adhesive coating amount can be used for achieving the peeling force of the same level, so that the hot melt pressure sensitive adhesive is a new demand for hot melt pressure sensitive adhesive developers in the market.
In addition, with the continuous and strong market of the hot-melt pressure-sensitive adhesive, various performance requirements of the hot-melt pressure-sensitive adhesive are continuously refined, and a higher-end paper base material oil seepage resistant high-peeling force and low-temperature resistant hot-melt pressure-sensitive adhesive is needed to meet the increasingly high technical requirements of the market.
Disclosure of Invention
The invention aims to provide an oil-permeation-resistant low-temperature-resistant high-peeling-force hot-melt pressure-sensitive adhesive and a preparation method thereof, which can completely meet the technical requirements of downstream on oil permeation resistance, high peeling force and low temperature resistance, and effectively ensure the oil permeation resistance, high peeling force and low temperature resistance of hot-melt pressure-sensitive adhesive products.
Technical scheme
The hot-melt pressure-sensitive adhesive with oil permeation resistance, low temperature resistance and high peeling force is prepared from the following raw materials in parts by weight:
Figure BDA0002477457070000021
further preferably, the thermoplastic elastomer one is selected from styrene-isoprene-styrene copolymers; wherein the content of the styrene is 13.0 to 17.0 percent and the content of the styrene-isoprene diblock is 40.0 to 55.0 percent in percentage by weight.
Further preferably, the second thermoplastic elastomer is selected from styrene-isoprene-styrene copolymers; wherein, the content of the styrene block is between 28.0 and 32.0 percent and the content of the styrene block is between 17.0 and 21.0 percent in percentage by weight.
Further preferably, the thermoplastic elastomer is selected from styrene-butadiene-styrene copolymer; wherein, the content of the styrene block is 67.0 to 73.0 percent and the content of the styrene block is 33.0 to 37.0 percent in percentage by weight.
Preferably, the plasticizer is selected from at least one of liquid resin, low molecular weight polyisobutylene, hydrogenated naphthenic oil, paraffin oil, synthetic base oil or a mixture thereof.
Preferably, the plasticizer is selected from at least one of liquid resin, low molecular weight polyisobutylene, hydrogenated naphthenic oil, paraffin oil, synthetic base oil or a mixture thereof.
Further, the plasticizer is preferably at least one of hydrogenated naphthenic oil, paraffin oil, synthetic base oil, or a mixture thereof.
Preferably, the first tackifying resin and the second tackifying resin are at least one selected from C5 petroleum resin, C5/C9 petroleum resin, hydrogenated C5 petroleum resin, hydrogenated C5/C9 petroleum resin, hydrogenated C9 petroleum resin, hydrogenated dicyclopentadiene resin, hydrogenated terpene resin or a mixture thereof.
The antioxidant is at least one of aromatic amine antioxidant, hindered phenol antioxidant and auxiliary antioxidant.
A preparation method of an oil-seepage-resistant low-temperature-resistant high-peeling-force hot-melt pressure-sensitive adhesive specifically comprises the following steps:
step A, adding a plasticizer, low molecular weight synthetic liquid polybutadiene rubber, an antioxidant and 25-40% of tackifying resin I into a reaction kettle, stirring and heating, setting the rotating speed at 30-50rpm, controlling the material temperature at 140-150 ℃, sealing the reaction kettle, vacuumizing for 0.5-1.0 h, and controlling the reaction pressure to be less than or equal to-0.09 MPa;
step B, closing the vacuum, opening the reaction kettle, adding the first thermoplastic elastomer, the second thermoplastic elastomer and the third thermoplastic elastomer after the tackifying resin is completely melted and uniformly mixed with the plasticizer, the low-molecular-weight synthetic liquid polybutadiene rubber and the antioxidant, heating to 150-155 ℃, preserving heat, vacuumizing and stirring until the first thermoplastic elastomer, the second thermoplastic elastomer and the third thermoplastic elastomer are completely melted;
and C, finally adding the second tackifying resin and the first tackifying resin left in the step A, vacuumizing and stirring at 135-140 ℃, taking out of the kettle and packaging after 60min to obtain the finished product of the high-temperature-resistant high-peeling-force low-temperature-resistant hot-melt pressure-sensitive adhesive.
Advantageous effects
Compared with the prior art, the hot-melt pressure-sensitive adhesive uses three thermoplastic elastomers with different styrene contents and different diblock contents, so that the stripping force and the low-temperature resistance of the product are effectively balanced; 1 plasticizer and 1 low molecular weight synthetic liquid polybutadiene rubber are also used, the plasticizer can reduce the system viscosity and improve the wetting of the hot melt adhesive on the base material, and the low molecular weight synthetic liquid polybutadiene rubber has larger molecular weight and is more difficult to migrate to the paper base material compared with base mineral oil, so that the low molecular weight synthetic liquid polybutadiene rubber has better oil seepage resistance of the paper base material; on the other hand, the low molecular weight synthetic polybutadiene rubber has a low glass transition temperature, and can endow the hot melt pressure sensitive adhesive with good low-temperature adhesion. The first tackifying resin preferably hydrogenated dicyclopentadiene resin and the second tackifying resin preferably hydrogenated C5C9 petroleum resin have good compatibility with the three thermoplastic elastomers, and particularly the third tackifying resin preferably hydrogenated dicyclopentadiene resin has excellent compatibility with the thermoplastic elastomer, which is beneficial to helping the hot melt pressure sensitive adhesive formula to achieve better performance balance, including peeling force, annular initial adhesion, low temperature adhesion and the like. The higher peel force of the final product is due to the higher molecular weight of the low molecular weight polybutadiene rubber than the base mineral oil.
Detailed Description
In order to make the technical problems, technical solutions and advantages to be solved by the present invention clearer, the following detailed description is given with reference to specific embodiments. In the following description, characteristic details such as specific configurations and components are provided only to help the full understanding of the embodiments of the present invention, and it should be apparent to those skilled in the art that various changes and modifications may be made to the embodiments described herein without departing from the scope and spirit of the present invention.
The invention provides an oil-seepage-resistant low-temperature-resistant high-peeling-force hot-melt pressure-sensitive adhesive which comprises the following raw materials in parts by weight:
Figure BDA0002477457070000031
preferably, the first thermoplastic elastomer, the second thermoplastic elastomer and the third thermoplastic elastomer are at least one selected from solution polymerized styrene-butadiene rubber, styrene-butadiene-styrene copolymer, styrene-ethylene-butylene-styrene copolymer, styrene-isoprene-styrene copolymer, styrene-ethylene-propylene-styrene copolymer or their mixture.
Preferably, the plasticizer is selected from at least one of liquid resin, low molecular weight polyisobutylene, hydrogenated naphthenic oil, paraffin oil, synthetic base oil or a mixture thereof.
Further preferably, the plasticizer is preferably at least one of hydrogenated naphthenic oil, paraffin oil, synthetic base oil, or a mixture thereof.
Preferably, the first tackifying resin and the second tackifying resin are at least one selected from C5 petroleum resin, C5/C9 petroleum resin, hydrogenated C5 petroleum resin, hydrogenated C5/C9 petroleum resin, hydrogenated C9 petroleum resin, hydrogenated dicyclopentadiene resin, hydrogenated terpene resin, or a mixture thereof.
Preferably, the antioxidant is at least one selected from aromatic amine antioxidants, hindered phenol antioxidants and auxiliary antioxidants.
Preferably, the relative molecular mass of the low molecular weight synthetic liquid polybutadiene rubber is 2000-5000 g/mol.
The invention also discloses a preparation method of the oil-seepage-resistant low-temperature-resistant high-peeling-force hot-melt pressure-sensitive adhesive, which specifically comprises the following steps:
step A, adding a plasticizer, low molecular weight synthetic liquid polybutadiene rubber, an antioxidant and 25-40% of tackifying resin I into a reaction kettle, stirring and heating, setting the rotating speed at 30-50rpm, controlling the material temperature at 140-150 ℃, sealing the reaction kettle, vacuumizing for 0.5-1.0 h, and controlling the reaction pressure to be less than or equal to-0.09 MPa;
step B, closing the vacuum, opening the reaction kettle, adding the first thermoplastic elastomer, the second thermoplastic elastomer and the third thermoplastic elastomer after the first tackifying resin is completely melted and is uniformly mixed with the plasticizer and the antioxidant, heating to 150-155 ℃, preserving the temperature, vacuumizing and stirring until the first thermoplastic elastomer, the second thermoplastic elastomer and the third thermoplastic elastomer are completely melted;
and C, finally adding a second tackifying resin and the first tackifying resin left in the step A, vacuumizing and stirring at 135-140 ℃, taking out of the kettle and packaging after 60min to obtain the finished product of the high-temperature-resistant high-peeling-force low-temperature-resistant hot-melt pressure-sensitive adhesive.
Specifically, the present invention provides the following 4 sets of examples:
example 1
In this example, the following raw materials were taken in parts by weight:
Figure BDA0002477457070000041
Figure BDA0002477457070000051
in the preparation step of this embodiment, preferably, the thermoplastic elastomer is selected from styrene-isoprene-styrene copolymer; the styrene content is between 13.0% and 17.0% (preferably 17%) by weight, and the styrene-isoprene diblock content is between 40.0% and 55.0% (preferably 55%).
The second thermoplastic elastomer is selected from styrene-isoprene-styrene copolymer; wherein the styrene content is 17.0-21.0% (preferably 21%) and the styrene block content is 28.0-32.0% (preferably 32%) by weight percentage.
The thermoplastic elastomer III is selected from styrene-butadiene-styrene copolymer; wherein the styrene content is 33.0-37.0% (preferably 37%) and the styrene block content is 67.0-73.0% (preferably 73%) by weight percentage.
The plasticizer is preferably a synthetic base oil.
The tackifying resin-preferably a hydrogenated dicyclopentadiene resin.
The tackifying resin II is preferably hydrogenated C5/C9 petroleum resin.
The antioxidant is selected from hindered phenol antioxidants.
Low molecular weight synthetic liquid polybutadiene rubbers with a relative molecular mass of 5000g/mol are preferred.
Further, according to the raw materials in the corresponding parts by weight, the preparation method of the hot melt pressure sensitive adhesive provided by the invention comprises the following preparation steps:
step A, adding the plasticizer, the low molecular weight synthetic liquid polybutadiene rubber, the antioxidant and 40% of tackifying resin I (namely 16 parts) into a reaction kettle in corresponding parts by weight, stirring and heating, setting the rotating speed at 50rpm, controlling the material temperature at 150 ℃, sealing the reaction kettle, vacuumizing for 1.0h, and controlling the reaction pressure at-0.09 MPa;
step B, closing vacuum, opening the reaction kettle, respectively adding 15 parts by weight of a first thermoplastic elastomer, 15 parts by weight of a second thermoplastic elastomer and 10 parts by weight of a third thermoplastic elastomer after 40% of the first tackifying resin in the step A is completely melted and uniformly mixed with the plasticizer and the antioxidant, heating to 155 ℃, preserving heat, vacuumizing and stirring until the first thermoplastic elastomer, the second thermoplastic elastomer and the third thermoplastic elastomer are completely melted;
and C, finally adding a second tackifying resin and the first tackifying resin (namely 24 parts) left in the step A, vacuumizing and stirring at 140 ℃, taking out of the kettle and packaging after 60min to obtain the finished product of the high-temperature-resistant high-peeling-force low-temperature-resistant hot-melt pressure-sensitive adhesive.
According to the invention, three thermoplastic elastomers with different styrene contents and different diblock contents are used in the hot-melt pressure-sensitive adhesive, so that the stripping force and the low-temperature resistance of the product are effectively balanced; 1 plasticizer and 1 low molecular weight synthetic liquid polybutadiene rubber are also used, the plasticizer can reduce the system viscosity and improve the wetting of the hot melt adhesive on the base material, and the low molecular weight synthetic liquid polybutadiene rubber has larger molecular weight and is more difficult to migrate to the paper base material compared with base mineral oil, so that the low molecular weight synthetic liquid polybutadiene rubber has better oil seepage resistance of the paper base material; on the other hand, the low molecular weight synthetic polybutadiene rubber has a low glass transition temperature, and can endow the hot melt pressure sensitive adhesive with good low-temperature adhesion. The first tackifying resin preferably hydrogenated dicyclopentadiene resin and the second tackifying resin preferably hydrogenated C5C9 petroleum resin have good compatibility with the three thermoplastic elastomers, and particularly the third tackifying resin preferably hydrogenated dicyclopentadiene resin has excellent compatibility with the thermoplastic elastomer, which is beneficial to helping the hot melt pressure sensitive adhesive formula to achieve better performance balance, including peeling force, annular initial adhesion, low temperature adhesion and the like. The higher peel force of the final product is due to the higher molecular weight of the low molecular weight polybutadiene rubber than the base mineral oil.
Example 2
In this example, the following raw materials were taken in parts by weight:
Figure BDA0002477457070000061
among them, it is preferable that the thermoplastic elastomer one is selected from styrene-isoprene-styrene copolymers; the styrene content is between 13.0% and 17.0% (preferably 15%) by weight, the styrene-isoprene diblock content is between 40.0% and 55.0% (preferably 53%).
The second thermoplastic elastomer is selected from styrene-isoprene-styrene copolymer; wherein the styrene content is 17.0-21.0% (preferably 19%) and the styrene block content is 28.0-32.0% (preferably 30%) by weight percentage.
The thermoplastic elastomer III is selected from styrene-butadiene-styrene copolymer; wherein the styrene content is 33.0-37.0% (preferably 35%) and the styrene block content is 67.0-73.0% (preferably 70%) by weight.
The plasticizer is preferably hydrogenated naphthenic oil.
The tackifying resin-preferably a hydrogenated C9 petroleum resin.
The tackifying resin II is preferably a hydrogenated C5 petroleum resin.
The antioxidant is selected from aromatic amine antioxidants.
Low molecular weight synthetic liquid polybutadiene rubbers with a relative molecular mass of 2000g/mol are preferred.
Further, in this embodiment, according to the above raw materials in parts by weight, the following preparation steps are performed according to the preparation method of the hot melt pressure sensitive adhesive provided by the present invention:
step A, adding the plasticizer, the low molecular weight synthetic liquid polybutadiene rubber, the antioxidant and 25 wt% of tackifying resin I (5 parts) into a reaction kettle, stirring and heating, setting the rotating speed at 30rpm, controlling the material temperature at 140 ℃, sealing the reaction kettle, vacuumizing for 0.5h, and controlling the reaction pressure at-1.0 MPa;
step B, closing vacuum, opening the reaction kettle, respectively adding the first thermoplastic elastomer, the second thermoplastic elastomer and the third thermoplastic elastomer again after the tackifying resin I added into the reaction kettle in the step A is completely melted and is uniformly mixed with the plasticizer and the antioxidant, heating to 150 ℃, preserving heat, vacuumizing and stirring until the first thermoplastic elastomer, the second thermoplastic elastomer and the third thermoplastic elastomer are completely melted;
and C, finally adding a second tackifying resin and the 15 parts of the first tackifying resin in the rest parts by weight in the step A, vacuumizing and stirring at 135 ℃, taking out of the kettle and packaging after 60min to obtain the finished product of the high-temperature-resistant high-peeling-force low-temperature-resistant hot-melt pressure-sensitive adhesive.
Example 3
In this example, the following raw materials were taken in parts by weight:
Figure BDA0002477457070000071
among them, it is preferable that the thermoplastic elastomer one is selected from styrene-isoprene-styrene copolymers; the styrene content is between 13.0% and 17.0% (preferably 15%) by weight, the styrene-isoprene diblock content is between 40.0% and 55.0% (preferably 50%).
The thermoplastic elastomer III is selected from styrene-butadiene-styrene copolymer; wherein the styrene content is 33.0-37.0% (preferably 35%) and the styrene block content is 67.0-73.0% (preferably 68%) by weight.
The plasticizer is preferably hydrogenated naphthenic oil.
The tackifying resin is preferably C5/C9 petroleum resin.
The tackifying resin II is preferably hydrogenated C5/C9 petroleum resin.
The antioxidant is selected from a mixture of hindered phenolic antioxidants and secondary antioxidants.
A low molecular weight synthetic liquid polybutadiene rubber with a relative molecular mass of 3000g/mol is preferred.
Further, according to the raw materials in the corresponding parts by weight, the preparation method of the hot melt pressure sensitive adhesive provided by the invention comprises the following preparation steps:
a, adding a plasticizer, low-molecular-weight synthetic liquid polybutadiene rubber, an antioxidant and 30% of tackifying resin I in corresponding parts by weight into a reaction kettle, heating while stirring, controlling the material temperature at 145 ℃ and sealing the reaction kettle, vacuumizing for 0.6 h, and controlling the reaction pressure to be-1.05 MPa;
b, closing the vacuum, opening the reaction kettle, adding the first thermoplastic elastomer and the third thermoplastic elastomer after the first tackifying resin is completely melted and is uniformly mixed with the plasticizer, the low-molecular-weight synthetic liquid polybutadiene rubber and the antioxidant, heating to 155 ℃, preserving heat, vacuumizing and stirring until the first thermoplastic elastomer and the third thermoplastic elastomer are completely melted;
and C, finally adding a second tackifying resin and 70% of the first tackifying resin in the step A, vacuumizing and stirring at 140 ℃, taking out of the kettle and packaging after 60min to obtain a finished product of the paper base material oil-seepage-resistant high-peeling-force low-temperature-resistant hot-melt pressure-sensitive adhesive.
Example 4:
in this example, the following raw materials were taken in parts by weight:
Figure BDA0002477457070000081
among them, the thermoplastic elastomer II is preferably selected from styrene-isoprene-styrene copolymers; wherein the styrene content is 17.0-21.0% (preferably 17%) and the styrene block content is 28.0-32.0% (preferably 28%) by weight percentage.
The thermoplastic elastomer III is selected from styrene-butadiene-styrene copolymer; wherein the styrene content is 33.0-37.0% (preferably 33%) and the styrene block content is 67.0-73.0% (preferably 67%) by weight percentage.
The plasticizer is preferably a paraffin oil.
The tackifying resin is preferably C5 petroleum resin.
The tackifier resin II is preferably hydrogenated terpene resin.
The antioxidant is selected from hindered phenol antioxidants.
Low molecular weight synthetic liquid polybutadiene rubbers with a relative molecular mass of 4000g/mol are preferred.
In this embodiment, according to the above raw materials in parts by weight, the following preparation steps are performed according to the preparation method of the hot melt pressure sensitive adhesive provided by the present invention:
a, adding a plasticizer, low-molecular-weight synthetic liquid polybutadiene rubber, an antioxidant and 40% of tackifying resin I (namely 14 parts) in corresponding parts by weight into a reaction kettle, heating while stirring at a rotating speed set to be 45rpm, controlling the material temperature to be 145 ℃, sealing the reaction kettle, vacuumizing for 0.8 hour, and controlling the reaction pressure to be-0.12 MPa;
b, closing the vacuum, opening the reaction kettle, adding the second thermoplastic elastomer and the third thermoplastic elastomer after the first tackifying resin is completely melted and is uniformly mixed with the plasticizer, the low-molecular-weight synthetic liquid polybutadiene rubber and the antioxidant, heating to 155 ℃, preserving heat, vacuumizing and stirring until the second thermoplastic elastomer and the third thermoplastic elastomer are completely melted;
and C, finally adding a second tackifying resin and the 60% by weight of the first tackifying resin (namely 21 parts) which is remained in the step A, vacuumizing and stirring at 140 ℃, taking out of the kettle and packaging after 60min to obtain the paper base material oil seepage resistant high-peeling force low-temperature resistant hot-melt pressure-sensitive adhesive.
The results of comparing examples 1-4 with conventional hot melt adhesives are shown in the following table:
Figure BDA0002477457070000091
the above test criteria are briefly described as follows:
a. the peel strength test standard is GB/T2792-1998 (the coating substrate is coated paper, and the coating weight is 45-50g/m2);
b. Initial adhesion strength test standard FINAT FTM9-2003 (coated substrate is coated paper, coating weight is 45-50g/m2) 。

Claims (10)

1. The hot-melt pressure-sensitive adhesive with oil permeation resistance, low temperature resistance and high peeling force is characterized in that: the composition is characterized by comprising the following raw materials in parts by weight:
Figure FDA0002477457060000011
2. the hot melt pressure sensitive adhesive of claim 1, wherein the hot melt pressure sensitive adhesive is characterized in that: the thermoplastic elastomer is selected from styrene-isoprene-styrene copolymer; wherein the content of the styrene is 13.0 to 17.0 percent and the content of the styrene-isoprene diblock is 40.0 to 55.0 percent in percentage by weight.
3. The hot melt pressure sensitive adhesive of claim 1, wherein the hot melt pressure sensitive adhesive is characterized in that: the second thermoplastic elastomer is selected from styrene-isoprene-styrene copolymer; wherein, the content of the styrene block is between 28.0 and 32.0 percent and the content of the styrene block is between 17.0 and 21.0 percent in percentage by weight.
4. The hot melt pressure sensitive adhesive of claim 1, wherein the hot melt pressure sensitive adhesive is characterized in that: the thermoplastic elastomer III is selected from styrene-butadiene-styrene copolymer; wherein, the content of the styrene block is 67.0 to 73.0 percent and the content of the styrene block is 33.0 to 37.0 percent in percentage by weight.
5. The hot melt pressure sensitive adhesive of claim 1, wherein the hot melt pressure sensitive adhesive is characterized in that: the plasticizer is selected from at least one of liquid resin, low molecular weight polyisobutylene, hydrogenated naphthenic oil, paraffin oil and synthetic base oil or a mixture thereof.
6. The hot melt pressure sensitive adhesive of claim 5, wherein the hot melt pressure sensitive adhesive is characterized in that: wherein, the plasticizer is preferably at least one of hydrogenated naphthenic oil, paraffin oil and synthetic base oil or a mixture thereof.
7. The hot melt pressure sensitive adhesive of claim 1, wherein the hot melt pressure sensitive adhesive is characterized in that: the first tackifying resin and the second tackifying resin are selected from at least one of C5 petroleum resin, C5/C9 petroleum resin, hydrogenated C5 petroleum resin, hydrogenated C5/C9 petroleum resin, hydrogenated C9 petroleum resin, hydrogenated dicyclopentadiene resin, hydrogenated terpene resin or a mixture thereof.
8. The hot melt pressure sensitive adhesive of claim 7, wherein the hot melt pressure sensitive adhesive is characterized in that: the first tackifying resin is preferably hydrogenated dicyclopentadiene resin, and the second tackifying resin is preferably hydrogenated C5/C9 petroleum resin.
9. The hot melt pressure sensitive adhesive of claim 1, wherein the hot melt pressure sensitive adhesive is characterized in that: the antioxidant is at least one of aromatic amine antioxidant, hindered phenol antioxidant and auxiliary antioxidant.
10. A preparation method of an oil-seepage-resistant low-temperature-resistant high-peeling-force hot-melt pressure-sensitive adhesive is characterized by comprising the following steps:
step A, adding a plasticizer, low molecular weight synthetic liquid polybutadiene rubber, an antioxidant and 25-40% of tackifying resin I into a reaction kettle, stirring and heating, setting the rotating speed at 30-50rpm, controlling the material temperature at 140-150 ℃, sealing the reaction kettle, vacuumizing for 0.5-1.0 h, and controlling the reaction pressure to be less than or equal to-0.09 MPa;
step B, closing the vacuum, opening the reaction kettle, adding the first thermoplastic elastomer, the second thermoplastic elastomer and the third thermoplastic elastomer after the first tackifying resin is completely melted and is uniformly mixed with the plasticizer and the antioxidant, heating to 150-155 ℃, preserving the temperature, vacuumizing and stirring until the first thermoplastic elastomer, the second thermoplastic elastomer and the third thermoplastic elastomer are completely melted;
and C, finally adding a second tackifying resin and the residual first tackifying resin in the step A, vacuumizing and stirring for 60min at 135-140 ℃, taking out of the kettle and packaging to obtain a finished product of the high-temperature-resistant high-peeling-force low-temperature-resistant hot-melt pressure-sensitive adhesive.
CN202010368743.XA 2020-05-02 2020-05-02 Oil-seepage-resistant low-temperature-resistant high-peeling-force hot-melt pressure-sensitive adhesive and preparation method thereof Pending CN111607344A (en)

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CN114163975A (en) * 2021-12-21 2022-03-11 佛山市本嘉新材料科技有限公司 Hot-melt pressure-sensitive adhesive and preparation method and use method thereof
CN114350290A (en) * 2022-01-10 2022-04-15 广州鹿山新材料股份有限公司 Low-temperature-resistant glue and preparation method and application thereof
CN114381226A (en) * 2021-12-28 2022-04-22 佛山南宝高盛高新材料有限公司 Hot melt adhesive for decoration and pasting and preparation method thereof
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Application publication date: 20200901