CN110003828A - Hot-fusible pressure-sensitive adhesive and preparation method thereof - Google Patents
Hot-fusible pressure-sensitive adhesive and preparation method thereof Download PDFInfo
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- CN110003828A CN110003828A CN201910328116.0A CN201910328116A CN110003828A CN 110003828 A CN110003828 A CN 110003828A CN 201910328116 A CN201910328116 A CN 201910328116A CN 110003828 A CN110003828 A CN 110003828A
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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
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/08—Macromolecular additives
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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
- C09J157/00—Adhesives based on unspecified polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C09J157/02—Copolymers of mineral oil hydrocarbons
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
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- Adhesives Or Adhesive Processes (AREA)
Abstract
The present invention relates to a kind of hot-fusible pressure-sensitive adhesives, and in particular to a kind of hot-fusible pressure-sensitive adhesive and preparation method thereof.Component including following parts by weight: 10-40 parts of thermoplastic elastomer (TPE), 1-8 parts of butadiene-styrene rubber, 1-20 parts of hollow glass micropearl, 40-60 parts of tackifying resin, 0.2-0.5 parts of antioxidant 1010,0.1-0.5 parts of irgasfos 168,10-20 parts of softening agent.Hot-fusible pressure-sensitive adhesive amalgamation is poor in the prior art, perimeter bond loosely (Yi Qiqiao, degumming), service life is short, ageing properties are poor, initial bonding strength is low, the disadvantages of initial bonding strength and holding power cannot have both simultaneously, and fusion performance is poor, poor air permeability and big density.Hot-fusible pressure-sensitive adhesive of the present invention has the characteristics that good anti-aging property, tack and holds that viscosity is excellent, amalgamation is good, good air permeability and light.
Description
Technical field
The present invention relates to a kind of hot-fusible pressure-sensitive adhesives, and in particular to a kind of hot-fusible pressure-sensitive adhesive and preparation method thereof.
Background technique
Hot-fusible pressure-sensitive adhesive combines the characteristics of hot melt adhesive and pressure sensitive adhesive, i.e., is at room temperature solid-state, heating melting at solid-state,
Coated, wetting adherend, slightly external force can bond after cooling, easily peelable.The positive Devoting Major Efforts To Developing heat molten type in countries in the world at present
Pressure sensitive adhesive, double faced adhesive tape, health care, woman article, label and in terms of be used widely.
Existing hot-fusible pressure-sensitive adhesive is by copolymer, tackifying resin, plasticizer, anti-aging agent and some other auxiliary agent groups
At, wherein copolymer mainly forms (SIS, SBS etc.) by triblock copolymer, although having both physical mechanical property and toughness, because
To contain a large amount of unsaturated bond in copolymer, polarity is smaller, causes the ageing-resistant performance of hot-fusible pressure-sensitive adhesive and heat resistance poor.
The softening point of hot-fusible pressure-sensitive adhesive is generally all relatively low (generally less than 100 DEG C), bonds loosely when encountering hot environment.Thermoplasticity
Elastomer and tackifying resin are easy to be dissolved by organic solvent or plasticizer, when hot-fusible pressure-sensitive adhesive is bonded in highly plasticized dose of PVC
Agent dissolution can be plasticized when upper.Traditional hot-fusible pressure-sensitive adhesive has significant deficiency in terms of gas permeability and raw materials consumption.By
Double bond is easy the attack by oxygen in air or other oxidation materials in the molecular structure of resin, generates free radical, and certainly
Macromolecular chain break can be further caused by base, cause the ageing properties of hot-fusible pressure-sensitive adhesive poor.
In order to overcome the existing disadvantage of hot-fusible pressure-sensitive adhesive, many researchs are modified hot-fusible pressure-sensitive adhesive, main by altogether
Mixed modification, sulfonation modifying and composite modified etc..Wherein, polyethylene (PE) is modified using benzoyl peroxide as initiator, is mixing
Object is chemically crosslinked, but with the increase of the degree of cross linking, the elongation at break and tensile strength of blend decline.Using poly-
Styrene (PS) is modified, so that hot-fusible pressure-sensitive adhesive impact strength reduces.In addition to this, the raw material of hot-fusible pressure-sensitive adhesive are expensive
Or what is taken is not easy, raw material supplier can not provide index close raw material, hot-fusible pressure-sensitive adhesive unstable quality etc. all at
For the obstruction in hot-fusible pressure-sensitive adhesive research.
Chinese patent CN107603537A discloses a kind of hot-fusible pressure-sensitive adhesive and preparation method thereof, by butyl rubber, hydrogenation
Styrene butadiene block copolymer thermoplastic elastomer (TPE), hydrogenated synthetic resin, poly- α-methylstyrene hydrogenated resin, rubber increase
Mould agent, antioxidant is added mixing melting completely with certain proportion and sequence and vacuumizes without particle, exhaust bubble.The patent advantage is
Hot-fusible pressure-sensitive adhesive heat resistance difference and the low disadvantage of cohesive force are overcome, the disadvantage is that not accounting for due to the excessive bring work of density
Industry higher cost.
Chinese patent CN201810363425 discloses a kind of anti-oxidant Medical hot melt pressure-sensitive adhesive and preparation method thereof, by stone
Oily hydrogenated resin, thermoplastic elastomer (TPE) SBS/SIS, phenol antiager, peroxide decomposer, ultraviolet absorber, rosin change
Property resin with certain proportion and sequence mix completely melting, vacuumize, maintain outlet temperature.The patent advantage is to reach promotion doctor
With the effect of the cohesive force of hot-fusible pressure-sensitive adhesive, and Long Term Contact air does not allow oxidizable, can to consolidate bonding yet.The disadvantage is that thoroughly
Gas performance is poor, accelerates bacterial growth.
Chinese patent CN201810065733 discloses a kind of paper diaper hot-fusible pressure-sensitive adhesive and its production method, passes through rubber
Glue oil, hydrogenated resin, the compound of macromolecular elastomer SBS and SIS, polyolefin copolymer, anti-aging agent are with certain proportion and suitable
Sequence mixing, sufficiently reacts, filtering.The patent advantage is to be not easy to disengage, have certain flexibility, non-aging, mobility it is strong,
It is nontoxic, there is no irritation to human body, meet paper diaper production requirement, the disadvantage is that permeability can be poor.
Summary of the invention
In view of the deficiencies of the prior art, the object of the present invention is to provide a kind of hot-fusible pressure-sensitive adhesive, hot-fusible pressure-sensitive adhesive has anti-
Ageing properties are good, tack and hold that viscosity is excellent, amalgamation is good, good air permeability and light feature；The present invention also provides it
Preparation method.
Hot-fusible pressure-sensitive adhesive of the present invention, the component including following parts by weight:
Wherein:
Thermoplastic elastomer (TPE) is SIS thermoplastic elastomer (TPE), is a kind of triblock copolymer, styrene-content 16%-
20%, diblock content 15%-20%.Styrene-content and diblock content within this range, are able to maintain product fine
Holding power and initial bonding strength；If the excessively high holding power that can reduce hot-fusible pressure-sensitive adhesive of diblock content, if styrene-content mistake
Height can reduce the initial bonding strength of hot-fusible pressure-sensitive adhesive.
Hollow glass micropearl is a kind of hollow glass microballoon that micron-sized surface is smooth, and main chemical compositions are soda lime
Borosilicate glass is viewed as hollow transparent spherosome under Electronic Speculum.In the present invention, hollow glass micropearl D at normal temperature90≤50
μm, density 0.58g/cm3-0.63g/cm3。D90At≤50 μm, hollow glass micropearl is preferable in conjunction with matrix, non-breakable；
Density is 0.58g/cm3-0.63g/cm3, in this density range, the anti-pressure ability of hot-fusible pressure-sensitive adhesive can be enhanced.If partial size
Exceed this range with density, the light effect that will lead to hot-fusible pressure-sensitive adhesive is poor.Such hollow glass micropearl is added, was being produced
Cheng Zhongke reduces product density.
Butadiene-styrene rubber is SSBR solution polymerized butadiene styrene rubber, and styrene total amount is 20%-27%, and block styrene content is
15%-22%.Styrene enhances its cohesive force in solution polymerized butadiene styrene rubber, but reduces adhesion strength, and the SSBR that the present invention uses is molten
Styrene total amount is 20%-27%, block styrene content 15%-22%, the block benzene second of this content in poly- butadiene-styrene rubber
Alkene content can enhance adhesion strength, maintain the initial bonding strength, holding power and 180 ° of peeling forces of hot-fusible pressure-sensitive adhesive one higher
Level.
Tackifying resin is C5 Petropols, and softening point is 95 DEG C -105 DEG C.Using the C5 Petropols of this softening point, make
Initial bonding strength, holding power and the 180 ° of peeling forces of product are in higher level.
Softening agent is Kelamayi naphthenic oil KN 4010.
The present invention using antioxidant 1010 (four [β-(3,5- di-tert-butyl-hydroxy phenyl) propionic acid] pentaerythritol esters) and
Irgasfos 168 (three [2.4- di-tert-butyl-phenyl] phosphite esters) improves ageing properties as combination antioxidant.
The preparation method of hot-fusible pressure-sensitive adhesive of the present invention, comprising the following steps:
(1) softening agent is put into agitating and heating in reaction vessel；
(2) tackifying resin, antioxidant are added in the reaction vessel in step (1), and is passed through nitrogen, heat temperature raising；
(3) part SIS thermoplastic elastomer (TPE) and part solution polymerized butadiene styrene rubber are added in the reaction vessel in step (2),
Heating a period of time, remaining SIS thermoplastic elastomer (TPE) and solution polymerized butadiene styrene rubber are then added, continues to heat；
(4) after completion of the reaction to step (3), hollow glass micropearl is disposably all put into reaction vessel, stirring；
(5) stop stirring after completion of the reaction, after reactive material is stablized, discharge, cooling, packaging.
Wherein:
Step (1) preferably by reaction vessel cleaning, drying, is packed into stirring rod, thermometer, softening agent and heats, clean
When, preferably elder generation wash with distilled water, then with ethyl alcohol is cleaned.
Heating temperature is to 140 DEG C -150 DEG C in step (1), stirring rate 150r/min.
It is 170 DEG C -180 DEG C that temperature is heated in step (2), and the rate of heat temperature raising is 2 DEG C -5 DEG C/min, is maintained
This temperature 15min-20min.
Step (3) are as follows: the 30%- for accounting for SIS thermoplastic elastomer (TPE) total weight first is added in the reaction vessel in step (2)
35% SIS thermoplastic elastomer (TPE) and and account for solution polymerized butadiene styrene rubber total weight 40%-50% solution polymerized butadiene styrene rubber, heating
20min-25min adds remaining SIS thermoplastic elastomer (TPE) and solution polymerized butadiene styrene rubber, vacuumizes the white bubble of removal, then permanent
Warm continuous heating 30min-35min.SIS thermoplastic elastomer (TPE) and solution polymerized butadiene styrene rubber are added portionwise, it is whole compared to disposable
The conversion ratio that more can be improved raw material is added, is conducive to being normally carried out for reaction, while reaction vessel stirring pressure can be slowed down,
System is in homogeneous transparent shape thick liquid after step (3) processing.
Mixing speed is that 175r/min is stirred evenly under this mixing speed in step (4), is otherwise easy to cause stirring
Unevenly.
The temperature of discharge port maintains 125 DEG C -150 DEG C when discharging in step (5), and at this temperature, discharging effect is best,
Otherwise it is easy to cause solidification, wastes product.
Compared with prior art, the invention has the following advantages that
(1) addition of hollow glass micropearl (HGS) occupies thermoplastic elastomer (TPE) in hot-fusible pressure-sensitive adhesive (SIS) and contains intermingle with fourth
Volume between benzene rubber (SSBR) strand, limits the movement of SIS strand and SSBR strand, reduces to a certain extent
The moulding of SIS, reduces the mobility of SSBR, therefore reduces the moulding and mobility of hot-fusible pressure-sensitive adhesive, makes hot-fusible pressure-sensitive adhesive
With better docile effect, the holding power of hot-fusible pressure-sensitive adhesive is improved.In the present invention, hollow glass micropearl D90 at normal temperature
It is≤50 μm, preferable and non-breakable using the hollow glass micropearl of the partial size and the interface cohesion of matrix, there is higher storage
It is bigger to spring back index for energy modulus after elastic deformation, and almost without particle agglomeration phenomenon.Solution polymerized butadiene styrene rubber by butadiene and
Styrene is as principal monomer, and wherein the styrene-content of SIS thermoplastic elastomer (TPE) is 16%-20%, and diblock content is
15%-20%, styrene-content and diblock content within this range, are able to maintain the holding power and initial bonding strength of product fine；
The styrene total amount of SSBR solution polymerized butadiene styrene rubber be 20%-27%, block styrene content 15%-22%, this content it is embedding
Section styrene-content can enhance adhesion strength, and the initial bonding strength, holding power and 180 ° of peeling forces of hot-fusible pressure-sensitive adhesive is made to maintain one
A higher level.Most of all, wherein isoprene also crosslinks in the styrene and SIS in solution polymerized butadiene styrene rubber,
Improve the compatibility of solution polymerized butadiene styrene rubber and SIS, so as to improve the cohesive force of system, make hot-fusible pressure-sensitive adhesive 180 ° of peeling forces and
Holding power is improved.
(2) naphthenic oil is good plasticizer, is had compared with high-solvency and excellent cryogenic property, use softening point for
95 DEG C -105 DEG C of C5 Petropols have excellent compatibility with Petropols and thermoplastic elastomer (TPE), with solution polymerized butylbenzene rubber
The good plasticising of glue and intersolubility, significantly reduce melt viscosity, become easy mixing and processing, reduce adhesive hardness, drop
Lower glass transition temperatures improve fusion performance, reduce alice.Styrene is total in the SSBR solution polymerized butadiene styrene rubber that the present invention uses
Amount is 20%-27%, and block styrene content 15%-22%, it is strong that the block styrene content of this content can enhance bonding
Degree, makes the initial bonding strength, holding power and 180 ° of peeling forces of hot-fusible pressure-sensitive adhesive maintain a higher level；Moreover, C5 petroleum tree
Rouge smell is small, and cohesive force is high and naphthenic oil is with thermoplastic elastomer (TPE) good compatibility, reduces alice caused by migrating and takes off
Glue.
(3) present invention is combined using antioxidant, due in the molecular structure of resin double bond be easy by oxygen in air or
The attack of other oxidation materials generates free radical, and free radical can further cause macromolecular chain break, in order to inhibit or prolong
Delay the process, the phenol antiager and phosphorons acid compound antioxidant of use can carry out anti-with the various free radicals of generation
It answers, generates stable compound, to prevent the further degradation of macromolecular chain.Irgasfos 168 belongs to phosphorous acid esters chemical combination
The intermediate product of oxidative degradation can be decomposed into non-free radical product by object, so that free radical be prevented to accelerate automatic oxidation reaction, antioxygen
The amount of 1010 substance of agent is minimum, but antioxidant effect is best, and antioxidant 1010 belongs to polyphenol type, there are four be obstructed phenol unit and
Phenolic hydroxyl group has the function of capture free radical, and therefore, antioxidant 1010 plays preferably the thermal oxide of pentalyn
Inhibiting effect.Antioxidant 1010 is as the primary antioxidant in composite antioxidant, and irgasfos 168 is as auxiliary antioxidant, the two
Due to radical reaction, stable compound can be formed, while improving antioxidant effect, secondly antioxidant 1010 and irgasfos 168
It is fabulous with other raw material compatibilities, it will not generate and be unevenly distributed or react incomplete phenomenon.
(4) solution polymerized butadiene styrene rubber SSBR is a kind of linear random block butadienestyrene copolymer, using organic lithiumation
Object is closed as initiator, causes anionic polymerisation and forms, have both good holding power and initial bonding strength.Product is anti-using non-polluting
Oxygen agent can be contacted with food.And substantially without gel, because of good compatibility, so color clarification is transparent.With it is good it is cold-resistant,
Heat-resisting, wear-resisting, ageing-resistant performance has skid resistance, and gas permeability, thermal conductivity, physical mechanical property is good.By solution polymerized butadiene styrene rubber
It is added in hot-fusible pressure-sensitive adhesive, because solution polymerized butadiene styrene rubber and naphthenic oil have good compatibility, the solution polymerized butylbenzene with gas permeability
Rubber can promote the gas permeability of hot-fusible pressure-sensitive adhesive, since solution polymerized butadiene styrene rubber styrene-content is maintained at and is involutory in the present invention
In the range of reason, the initial bonding strength and holding power for making hot-fusible pressure-sensitive adhesive are in higher level.And it according to similar compatibility principle, contains intermingle with
Butadiene-styrene rubber is similar with SIS polarity, and the two has good compatibility, enhances the stability of product.
(5) hollow glass micropearl has high temperature resistant, acid and alkali-resistance, low thermally conductive, electrical isolation, light, high-intensitive, good flowing
A variety of excellent properties such as property.Since hollow glass micropearl is microspheres, than sheet, needle-shaped or irregular in liquid resin
The filler of shape has more preferable mobility；The addition of hollow glass micropearl, enable product have good crack resistance with
Cycling processability；The present invention uses hollow glass micropearl D at normal temperature90≤ 50 μm, density 0.58g/cm3-0.63g/cm3,
In this partial size and density range, the anti-pressure ability of hot-fusible pressure-sensitive adhesive can be enhanced.If partial size and density exceed this range, meeting
Cause the light effect of hot-fusible pressure-sensitive adhesive poor.Such hollow glass micropearl is added, product density can be reduced in process of production.
(6) hot-fusible pressure-sensitive adhesive is by materials systems such as thermoplastic elastomer (TPE), antioxidant, tackifier, plasticizer in the prior art
Form, amalgamation is poor, perimeter bond loosely (Yi Qiqiao, degumming), service life is short, ageing properties are poor, initial bonding strength is low, just
The disadvantages of viscous force and holding power cannot have both simultaneously, and fusion performance is poor, poor air permeability and big density.Hot-fusible pressure-sensitive adhesive tool of the present invention
There are good anti-aging property, tack and holds that viscosity is excellent, amalgamation is good, good air permeability and light.
(7) the present invention also provides preparation method, when reaction, adds SIS thermoplastic elastomer (TPE) and solution polymerized butadiene styrene rubber in batches
Enter, compared to the conversion ratio that disposable all additions more can be improved raw material, is conducive to being normally carried out for reaction, while can slow down
Reaction vessel stirs pressure, and system is in homogeneous transparent shape thick liquid after processing.Raw material are added in batches, make SIS, SSBR
Cross-linking reaction substep between hollow glass micropearl carries out, and contains unsaturated bond in SIS and tackifying resin, in step (2)
Antioxidant is added in advance, the intermediate product of oxidative degradation can be decomposed by the effective free radical captured in tackifying resin and SIS
Non-free radical product, reduces the oxidation of hot-fusible pressure-sensitive adhesive raw material during the preparation process, and the SIS being first added and SSBR occur one
Divide crosslinking, generates the macromolecule mixture of stable and uniform, when remaining SIS and SSBR is added, reduce between identical molecule
Interaction force, make between different molecular compatibility enhancing, react more complete.The enhancing of final products stability, it is anti-aging
Performance improves.
Specific embodiment
Below with reference to embodiment, the present invention will be further described.
Embodiment 1
A kind of hot-fusible pressure-sensitive adhesive, the component including following parts by weight:
Wherein:
The styrene-content of SIS thermoplastic elastomer (TPE) is 18%, diblock content 18%；
Hollow glass micropearl D at normal temperature90≤ 50, density 0.60g/cm3, heat resisting temperature≤350 DEG C；
The styrene total amount of SSBR solution polymerized butadiene styrene rubber is 22%, block styrene content 17%；
The softening point of C5 Petropols is 100 DEG C.
The hot-fusible pressure-sensitive adhesive the preparation method is as follows:
(1) reaction vessel is first wash with distilled water, then cleaned with ethyl alcohol, it is dry, it is packed into stirring rod, thermometer, carat
Ma is according to naphthenic oil KN 4010 and heats, and heating temperature is to 145 DEG C, stirring rate 150r/min；
(2) C5 Petropols, antioxidant 1010 and irgasfos 168 are added in the reaction vessel in step (1), and is passed through
Nitrogen, being heated to temperature is 175 DEG C, and the rate of heat temperature raising is 2 DEG C/m, maintains this temperature 18min；
(3) the 30% SIS heat for accounting for SIS thermoplastic elastomer (TPE) total weight is first added in the reaction vessel in step (2)
Thermoplastic elastic and and account for 40% solution polymerized butadiene styrene rubber of solution polymerized butadiene styrene rubber total weight, heat 20min, add remaining
SIS thermoplastic elastomer (TPE) and solution polymerized butadiene styrene rubber vacuumize the white bubble of removal, then constant temperature continuous heating 30min；
(4) after completion of the reaction to step (3), hollow glass micropearl is disposably all put into reaction vessel, stirring is stirred
Mixing speed is 175r/min；
(5) stop stirring after completion of the reaction, after reactive material is stablized, discharging, the temperature of discharge port is maintained when discharging
It is 125 DEG C, cooling, packaging.
Embodiment 2
A kind of hot-fusible pressure-sensitive adhesive, the component including following parts by weight:
Wherein:
The styrene-content of SIS thermoplastic elastomer (TPE) is 16%, diblock content 20%；
Hollow glass micropearl D at normal temperature90≤ 50, density 0.58g/cm3, heat resisting temperature≤350 DEG C；
The styrene total amount of SSBR solution polymerized butadiene styrene rubber is 20%, block styrene content 22%；
The softening point of C5 Petropols is 95 DEG C.
The hot-fusible pressure-sensitive adhesive the preparation method is as follows:
(1) reaction vessel is first wash with distilled water, then cleaned with ethyl alcohol, it is dry, it is packed into stirring rod, thermometer, carat
Ma is according to naphthenic oil KN 4010 and heats, and heating temperature is to 146 DEG C, stirring rate 150r/min；
(2) C5 Petropols, antioxidant 1010 and irgasfos 168 are added in the reaction vessel in step (1), and is passed through
Nitrogen, being heated to temperature is 175 DEG C, and the rate of heat temperature raising is 3 DEG C/min, maintains this temperature 15min；
(3) the 33% SIS heat for accounting for SIS thermoplastic elastomer (TPE) total weight is first added in the reaction vessel in step (2)
Thermoplastic elastic and and account for 45% solution polymerized butadiene styrene rubber of solution polymerized butadiene styrene rubber total weight, heat 22min, add remaining
SIS thermoplastic elastomer (TPE) and solution polymerized butadiene styrene rubber vacuumize the white bubble of removal, then constant temperature continuous heating 32min；
(4) after completion of the reaction to step (3), hollow glass micropearl is disposably all put into reaction vessel, stirring is stirred
Mixing speed is 175r/min；
(5) stop stirring after completion of the reaction, after reactive material is stablized, discharging, the temperature of discharge port is maintained when discharging
It is 135 DEG C, cooling, packaging.
Embodiment 3
A kind of hot-fusible pressure-sensitive adhesive, the component including following parts by weight:
Wherein: the styrene-content of SIS thermoplastic elastomer (TPE) is 19%, diblock content 15%；
Hollow glass micropearl D at normal temperature90≤ 50, density 0.62g/cm3, heat resisting temperature≤350 DEG C；
The styrene total amount of SSBR solution polymerized butadiene styrene rubber is 23%, block styrene content 18%；
The softening point of C5 Petropols is 97 DEG C.
The hot-fusible pressure-sensitive adhesive the preparation method is as follows:
(1) reaction vessel is first wash with distilled water, then cleaned with ethyl alcohol, it is dry, it is packed into stirring rod, thermometer, carat
Ma is according to naphthenic oil KN 4010 and heats, and heating temperature is to 144 DEG C, stirring rate 150r/min；
(2) C5 Petropols, antioxidant 1010 and irgasfos 168 are added in the reaction vessel in step (1), and is passed through
Nitrogen, being heated to temperature is 172 DEG C, and the rate of heat temperature raising is 5 DEG C/min, maintains this temperature 20min；
(3) the 33% SIS heat for accounting for SIS thermoplastic elastomer (TPE) total weight is first added in the reaction vessel in step (2)
Thermoplastic elastic and and account for 45% solution polymerized butadiene styrene rubber of solution polymerized butadiene styrene rubber total weight, heat 23min, add remaining
SIS thermoplastic elastomer (TPE) and solution polymerized butadiene styrene rubber vacuumize the white bubble of removal, then constant temperature continuous heating 32min；
(4) after completion of the reaction to step (3), hollow glass micropearl is disposably all put into reaction vessel, stirring is stirred
Mixing speed is 175r/min；
(5) stop stirring after completion of the reaction, after reactive material is stablized, discharging, the temperature of discharge port is maintained when discharging
It is 127 DEG C, cooling, packaging.
Embodiment 4
A kind of hot-fusible pressure-sensitive adhesive, the component including following parts by weight:
Wherein: the styrene-content of SIS thermoplastic elastomer (TPE) is 19%, diblock content 18%；
Hollow glass micropearl D at normal temperature90≤ 50, density 0.61g/cm3, heat resisting temperature≤350 DEG C；
The styrene total amount of SSBR solution polymerized butadiene styrene rubber is 26%, block styrene content 20%；
The softening point of C5 Petropols is 98 DEG C.
The hot-fusible pressure-sensitive adhesive the preparation method is as follows:
(1) reaction vessel is first wash with distilled water, then cleaned with ethyl alcohol, it is dry, it is packed into stirring rod, thermometer, carat
Ma is according to naphthenic oil KN 4010 and heats, and heating temperature is to 144 DEG C, stirring rate 150r/min；
(2) C5 Petropols, antioxidant 1010 and irgasfos 168 are added in the reaction vessel in step (1), and is passed through
Nitrogen, being heated to temperature is 172 DEG C, and the rate of heat temperature raising is 4 DEG C/min, maintains this temperature 18min；
(3) the 31% SIS heat for accounting for SIS thermoplastic elastomer (TPE) total weight is first added in the reaction vessel in step (2)
Thermoplastic elastic and and account for 46% solution polymerized butadiene styrene rubber of solution polymerized butadiene styrene rubber total weight, heat 23min, add remaining
SIS thermoplastic elastomer (TPE) and solution polymerized butadiene styrene rubber vacuumize the white bubble of removal, then constant temperature continuous heating 33min；
(4) after completion of the reaction to step (3), hollow glass micropearl is disposably all put into reaction vessel, stirring is stirred
Mixing speed is 175r/min；
(5) stop stirring after completion of the reaction, after reactive material is stablized, discharging, the temperature of discharge port is maintained when discharging
It is 135 DEG C, cooling, packaging.
Comparative example 1
A kind of hot-fusible pressure-sensitive adhesive, the component and preparation method of use are same as Example 1, only difference is that step
(3) are as follows: be added at one time SIS thermoplastic elastomer (TPE) and solution polymerized butadiene styrene rubber in the reaction vessel in step (2), vacuumize
Except white bubble, then constant temperature continuous heating 50min.
Comparative example 2
A kind of hot-fusible pressure-sensitive adhesive, the component and preparation method of use are same as Example 1, only difference is that: it is not added
Hollow glass micropearl.
Comparative example 3
A kind of hot-fusible pressure-sensitive adhesive, the component including following parts by weight:
Preparation method: rising to 175 DEG C for reaction kettle oil temperature, and naphthenic oil is added in reaction kettle, 20min is then stirred, and rises
SIS thermoplastic elastomer (TPE) is added to 200 DEG C in temperature, continues to stir 30-50min, then by pentaerythritol ester, Petropols, antioxygen
Agent, rosin glyceride are put into reaction kettle, and reaction kettle oil temperature is adjusted to 160 DEG C, stirs 15-30min；Mixture is cooled to often
Temperature, mixture are hot-fusible pressure-sensitive adhesive finished product.
Embodiment 1-4 and comparative example the 1-3 hot-fusible pressure-sensitive adhesive being prepared are tested for the property:
(1) detection method: annular initial bonding strength proved recipe method is based on GB/T 31125-2014, and peel strength test method is
Based on GB/T 2790-1995, holding power test method is based on GB/T 4851-2014, GB/T 17146-2015 " Building wood
Material and its product water vapo(u)r transmission energy test method ", the steam penetrating capacity of test material, units/kg/(sm2), lightweight
Change effect=(m0-m1)/m0。(m0: adhesive quality when hollow glass micropearl is not yet added, m1: adhesive after hollow glass is added
Quality)
(2) pass through the quality of numerical value measurement technology effect in table.
In table 1, annular initial bonding strength value is bigger, illustrates that initial bonding strength is better；180 ° of removing force value are bigger, illustrate that peeling force is got over
It is good；Holding power value is bigger, illustrates that holding power is better；Gas permeability: it is compared with comparative example 2, gas permeability is less than compared to rising value
10% is chosen as difference, and gas permeability rising value is 10%~20% to be chosen as, and gas permeability rising value is 20%~30% to be chosen as good, breathes freely
Property rising value value be greater than 30% be chosen as it is excellent；Light percentage is bigger, illustrates that light effect is better.
1 the performance test results of table
Claims (10)
1. a kind of hot-fusible pressure-sensitive adhesive, it is characterised in that: the component including following parts by weight:
2. hot-fusible pressure-sensitive adhesive according to claim 1, it is characterised in that: thermoplastic elastomer (TPE) is SIS thermoplastic elastomer (TPE),
Styrene-content is 16%-20%, diblock content 15%-20%.
3. hot-fusible pressure-sensitive adhesive according to claim 1, it is characterised in that: hollow glass micropearl D at normal temperature90≤ 50, it is close
Degree is 0.58g/cm3-0.63g/cm3, heat resisting temperature≤350 DEG C.
4. hot-fusible pressure-sensitive adhesive according to claim 1, it is characterised in that: butadiene-styrene rubber is SSBR solution polymerized butadiene styrene rubber, benzene
Ethylene total amount is 20%-27%, block styrene content 15%-22%.
5. hot-fusible pressure-sensitive adhesive according to claim 1, it is characterised in that: tackifying resin is C5 Petropols, and softening point
It is 95 DEG C -105 DEG C.
6. hot-fusible pressure-sensitive adhesive according to claim 1, it is characterised in that: softening agent is Kelamayi naphthenic oil KN 4010.
7. a kind of preparation method of any hot-fusible pressure-sensitive adhesive of claim 1-6, it is characterised in that: the following steps are included:
(1) softening agent is put into agitating and heating in reaction vessel；
(2) tackifying resin, antioxidant are added in the reaction vessel in step (1), and is passed through nitrogen, heat temperature raising；
(3) part SIS thermoplastic elastomer (TPE) and part solution polymerized butadiene styrene rubber, heating are added in the reaction vessel in step (2)
For a period of time, remaining SIS thermoplastic elastomer (TPE) and solution polymerized butadiene styrene rubber are then added, continues to heat；
(4) after completion of the reaction to step (3), hollow glass micropearl is disposably all put into reaction vessel, stirring；
(5) stop stirring after completion of the reaction, after reactive material is stablized, discharge, cooling, packaging.
8. the preparation method of hot-fusible pressure-sensitive adhesive according to claim 7, it is characterised in that:
Heating temperature is to 140 DEG C -150 DEG C in step (1), stirring rate 150r/min；
It is 170 DEG C -180 DEG C that temperature is heated in step (2), and the rate of heat temperature raising is 2 DEG C -5 DEG C/min, maintains this temperature
Spend 15min-20min.
9. the preparation method of hot-fusible pressure-sensitive adhesive according to claim 7, it is characterised in that: step (3) are as follows: first to step
(2) in the reaction vessel in be added account for SIS thermoplastic elastomer (TPE) total weight 30%-35% SIS thermoplastic elastomer (TPE) and and
The solution polymerized butadiene styrene rubber of the 40%-50% of solution polymerized butadiene styrene rubber total weight is accounted for, 20min-25min is heated, adds remaining SIS
Thermoplastic elastomer (TPE) and solution polymerized butadiene styrene rubber vacuumize the white bubble of removal, then constant temperature continuous heating 30min-35min.
10. the preparation method of hot-fusible pressure-sensitive adhesive according to claim 7, it is characterised in that:
Mixing speed is 175r/min in step (4)；
The temperature of discharge port maintains 125 DEG C -150 DEG C when discharging in step (5).
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| CN111690354B (en) * | 2020-07-23 | 2022-07-01 | 佛山南宝高盛高新材料有限公司 | Hot melt adhesive for self-crosslinking label and preparation method thereof |
| CN111808562A (en) * | 2020-07-23 | 2020-10-23 | 佛山南宝高盛高新材料有限公司 | Hot melt adhesive for ultraviolet curing label and preparation method and application thereof |
| CN111808562B (en) * | 2020-07-23 | 2022-04-12 | 佛山南宝高盛高新材料有限公司 | Hot melt adhesive for ultraviolet curing label and preparation method and application thereof |
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| CN113249066A (en) * | 2021-06-30 | 2021-08-13 | 佛山南宝高盛高新材料有限公司 | High-temperature removable label hot melt adhesive and preparation method thereof |
| CN113249066B (en) * | 2021-06-30 | 2022-09-06 | 佛山南宝高盛高新材料有限公司 | High-temperature removable label hot melt adhesive and preparation method thereof |
| CN114958213A (en) * | 2022-06-01 | 2022-08-30 | 山东理工大学 | Novel self-adhesive rubber SBS modified asphalt crack plaster and preparation method thereof |
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