CN107254023B - Preparation method and application of graft modified tackifying resin - Google Patents
Preparation method and application of graft modified tackifying resin Download PDFInfo
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- CN107254023B CN107254023B CN201710492287.8A CN201710492287A CN107254023B CN 107254023 B CN107254023 B CN 107254023B CN 201710492287 A CN201710492287 A CN 201710492287A CN 107254023 B CN107254023 B CN 107254023B
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- tackifying resin
- rosin
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F289/00—Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds not provided for in groups C08F251/00 - C08F287/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F277/00—Macromolecular compounds obtained by polymerising monomers on to polymers of carbocyclic or heterocyclic monomers as defined respectively in group C08F32/00 or in group C08F34/00
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F291/00—Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds according to more than one of the groups C08F251/00 - C08F289/00
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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
- C08L51/00—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers
- C08L51/003—Compositions of graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Compositions of derivatives of such polymers grafted on to macromolecular compounds obtained by reactions only involving unsaturated carbon-to-carbon bonds
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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
- C09J151/00—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
- C09J151/003—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers grafted on to macromolecular compounds obtained by reactions only involving unsaturated carbon-to-carbon bonds
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- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Adhesives Or Adhesive Processes (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention relates to a preparation method and application of graft modified tackifying resin, which comprises the following steps: (1) weighing the following raw materials in parts by weight: 3.5-90 parts of rosin resin, 1-90 parts of other resins, 3.5-90 parts of grafting monomers, 0.2-0.4 part of initiator and 0.3-0.6 part of antioxidant, wherein the grafting monomers comprise acrylic acid series monomers; (2) crushing rosin resin, adding the crushed rosin resin and other resins into a reaction kettle, adding 40% of grafting monomer, adding an antioxidant, stirring for dissolving, and heating until the mixture is completely dissolved; (3) adding an initiator and dispersing for 5 minutes; (4) dropwise adding the remaining grafting monomers to start grafting reaction; (5) and (5) cooling and discharging. The graft modified tackifying resin prepared by the method can be independently used as a hot melt adhesive resin, can be added into other hot melt adhesive systems to be used as a tackifier for blending, and can also be used as a compatilizer in the hot melt adhesive systems.
Description
Technical field
The present invention relates to field of polymer material preparing technology, more particularly to a kind of preparation of graft modification tackifying resin
Method and application.
Background technology
Because of its environmental protection characteristic, the development and application of hot melt adhesive is more and more, and a variety of thermoplastic resins and additive are used for
The formula system of hot melt adhesive.The natural resin that rosin is pine tree or conifer trunk secrets out of can obtain rosin after refinement, and rosin is again
Become rosin resin after being chemically modified.Rosin resin is one of most popular tackifying resin, market in hot melt adhesive system
On also commonly use acrylic resin as tackifying resin, acrylic resin is directly added as tackifying resin in hot melt adhesive system, though
So improve the bonding force of system, but bring poor compatibility, it is of high cost the shortcomings of, influence to be widely applied.And using third
Olefin(e) acid series monomers fusion-grafting prepares tackifying resin to the method for the modification of rosin resin and has not been reported.
Invention content
The purpose of the present invention is to provide a kind of environmental-friendly, based on renewable resource graft modification tackifying resins
Preparation method.This method using rosin resin as basis material, esters of acrylic acid, styrene, maleic anhydride be grafted monomers, peroxide
Compound is initiator, is graft-polymerized using ontology smelting process.Graft modification tackifying resin obtained can in this way
It is used separately as hot melt gum resin, can be also added in other hot melt adhesive systems and be blended to use as tackifier, also may be used
It is used as the compatilizer in hot melt adhesive system.
The present invention is achieved by the following technical solutions：
A kind of preparation method of graft modification tackifying resin, it is characterised in that：Include the following steps：
(1) raw material of following parts by weight is weighed：
3.5~90 parts of rosin resin,
Other 1~90 part of resins, other resins are terpene resin, C5 Petropols, C9 Petropols, C5-C9 common
Poly- Petropols, hydrogenation C5 Petropols, hydrogenation C9 Petropols, hydrogenation C5-C9 copolymerized petroleum resins or SBS (styrene-
Butadiene-styrene triblock copolymer), SIS (styrene-isoprene-styrene block copolymer), SEBS (styrene
One or more of block copolymer),
3.5~90 parts of grafted monomers, the grafted monomers include oleic series monomer,
0.2~0.4 part of initiator,
0.3~0.6 part of antioxidant；
(2) rosin resin is crushed and other resins is added in reaction kettle together, add in 40% grafted monomers, then
Antioxidant stirring and dissolving is added in, is heated to melting completely；
(3) initiator redisperse is added in 5 minutes；
(4) remaining grafted monomers are added dropwise and start graft reaction；
(5) cooling discharge.
Further, temperature control is 70-80 DEG C after the step (2) melts completely.
Further, at 80-120 DEG C, time for adding is at least 3 hours, is protected for step (4) the graft reaction temperature control
Temperature at least 1 hour.
Further, the rosin resin is rosin, rosin glycerides, hydrogenated rosin, disproportionated rosin, maleic rosin, gathers
Close the one or more of rosin.
Further, the oleic series monomer is acrylic acid, methacrylic acid, methyl acrylate, methacrylic acid
Methyl esters, ethyl acrylate, ethyl methacrylate, hydroxy-ethyl acrylate, hydroxyethyl methacrylate, hydroxypropyl acrylate, first
One in base hydroxypropyl acrylate, butyl acrylate, butyl methacrylate, Isooctyl acrylate monomer, isooctyl methacrylate
Kind is several.
Preferably, the grafted monomers further include one or both of styrene, maleic anhydride.The addition of styrene is not
Effect is more preferable when rosin resin can only dissolved with grafted monomers, can also improve the high temperature resistance of product, maleic anhydride
Addition can make product have better adhesive force.
Further, the initiator is benzoyl peroxide, the benzoyl peroxide tert-butyl ester, methyl ethyl ketone peroxide, mistake
Aoxidize one kind in diisopropylbenzene (DIPB), azodiisobutyronitrile.
Further, the antioxidant for BASF Irganox 565, Irganox 1010, Irganox 1076,
Irganox1425、Irganox1520、Irganox B551、Irganox B561、Irganox 1520、Irganox 1035、:
Irgafos 168, Sumitomo Sumilizer AO-80, Sumilizer TP-D, AKEMA rosin resin antioxidant ROSINOX one
Kind is several.
The present invention also provides a kind of graft modification tackifying resins, which is characterized in that is obtained by above-mentioned preparation method.
The present invention also provides a kind of applications of graft modification tackifying resin, which is characterized in that it is direct that melting connects rosin resin
Compatilizer as hot melt adhesive or as the tackifier of hot melt adhesive or as hot melt adhesive system.
The preparation method of the graft modification tackifying resin of the present invention, has the advantages that：
(1) graft copolymer prepared using this method, grafting rate>90%；
(2) this preparation method has selected environmental-friendly and based on renewable resource raw material to prepare；
(3) present invention utilizes contains double bond on rosin resin, the method pair for passing through graft polymerization with oleic series monomer
Rosin resin is modified, and is added directly into hot melt adhesive system with acrylic resin in the prior art or directly and rosin resin
It is mixed to get tackifying resin to compare, not only compatibility is more preferable, and excellent to the Efficient Adhesive Promotion of hot melt adhesive system, especially to low table
The adhesive effect of face energy material such as OPP, PE are good；It can be with the common APAO of the partial alternative prior art, polyolefin on adhesive effect
Materials are waited, reduce cost；
(4) the graft modification tackifying resin being prepared can not only be used directly as hot melt adhesive, can be also added to it
It is blended to use as tackifier in its hot melt adhesive system, can also be used as the compatilizer in hot melt adhesive system.
Specific embodiment
Embodiment 1
The graft modification tackifying resin of the present embodiment, preparation method according to the following steps obtain：
(1) raw material of following parts by weight is weighed：
(2) rosin resin is crushed, equipped with thermometer, blender, reflux condenser dry reaction kettle in add in powder
Broken good rosin resin and other resins add in 40% grafted monomers and antioxidant stirring and dissolving, are heated to melting completely；
(3) it adds in initiator redisperse 5 minutes, keeps the temperature 1 hour；
(4) remaining grafted monomers are added dropwise and start graft reaction, temperature is controlled at 80-90 DEG C, is added dropwise within 4 hours, is protected
Temperature 1.5 hours；
(5) cooling discharge.
Graft modification tackifying resin manufactured in the present embodiment can be directly used as hot melt adhesive or the tackifier as hot melt adhesive
To use or the compatilizer as hot melt adhesive system.
Embodiment 2
The graft modification tackifying resin of the present embodiment, preparation method according to the following steps obtain：
(1) raw material of following parts by weight is weighed
(2) rosin resin is crushed, equipped with thermometer, blender, reflux condenser dry reaction kettle in add in powder
Broken good rosin resin and other resins add in 40% grafted monomers and antioxidant stirring and dissolving, are heated to melting completely, so
Temperature control is 70-80 DEG C afterwards；
(3) initiator redisperse is added in 5 minutes；
(4) remaining grafted monomers are added dropwise and start graft reaction, temperature is controlled at 80-90 DEG C, is added dropwise within 3 hours, is protected
Temperature 1.5 hours；
(5) cooling discharge.
Graft modification tackifying resin manufactured in the present embodiment can be directly used as hot melt adhesive or the tackifier as hot melt adhesive
To use or the compatilizer as hot melt adhesive system.
Embodiment 3
The graft modification tackifying resin of the present embodiment, preparation method according to the following steps obtain：
(1) raw material of following parts by weight is weighed
(2) rosin resin is crushed, equipped with thermometer, blender, reflux condenser dry reaction kettle in add in powder
Broken good rosin resin and other resins add in 40% grafted monomers and antioxidant stirring and dissolving, are heated to melting completely, so
Temperature control is 70-80 DEG C afterwards；
(3) it adds in initiator redisperse 5 minutes, keeps the temperature 1 hour；
(4) remaining grafted monomers are added dropwise and start graft reaction, temperature is controlled at 90-110 DEG C, is added dropwise within 4.5 hours,
Heat preservation 1 hour；
(5) cooling discharge.
Graft modification tackifying resin manufactured in the present embodiment can be directly used as hot melt adhesive or the tackifier as hot melt adhesive
To use or the compatilizer as hot melt adhesive system.
Embodiment 4
The graft modification tackifying resin of the present embodiment, preparation method according to the following steps obtain：
(1) raw material of following parts by weight is weighed
(2) rosin resin is crushed, equipped with thermometer, blender, reflux condenser dry reaction kettle in add in powder
Broken good rosin resin and other resins add in 40% grafted monomers and antioxidant stirring and dissolving, are heated to melting completely；
(3) it adds in initiator redisperse 5 minutes, keeps the temperature 1 hour；
(4) remaining grafted monomers are added dropwise and start graft reaction, temperature is controlled at 110-120 DEG C, dripped within 3.5 hours
Finish, keep the temperature 1 hour；
(5) cooling discharge.
Graft modification tackifying resin manufactured in the present embodiment can be directly used as hot melt adhesive or the tackifier as hot melt adhesive
To use or the compatilizer as hot melt adhesive system.
Embodiment described above only expresses the several embodiments of the present invention, and description is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that those of ordinary skill in the art are come
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to the protection of the present invention
Range.
Claims (8)
1. a kind of preparation method of graft modification tackifying resin, it is characterised in that：Include the following steps：
(1) raw material of following parts by weight is weighed：
3.5~90 parts of rosin resin,
Other 1~90 part of resins, other resins are terpene resin, C5 Petropols, C9 Petropols, C5-C9 copolymerization stones
In oleoresin, hydrogenation C5 Petropols, hydrogenation C9 Petropols, hydrogenation C5-C9 copolymerized petroleum resins or SBS, SIS, SEBS
One or more,
3.5~90 parts of grafted monomers, the grafted monomers include oleic series monomer,
0.2~0.4 part of initiator,
0.3~0.6 part of antioxidant；
(2) rosin resin is crushed and other resins is added in reaction kettle together, added in 40% grafted monomers, add
Antioxidant stirring and dissolving is heated to melting completely, and then temperature control is 70-80 DEG C；
(3) initiator redisperse is added in 5 minutes；
(4) remaining grafted monomers are added dropwise and start graft reaction, reaction temperature is controlled at 80-120 DEG C, and time for adding is at least 3
Hour, keep the temperature at least 1 hour；
(5) cooling discharge.
2. the preparation method of graft modification tackifying resin according to claim 1, it is characterised in that：The rosin resin is
Rosin, rosin glycerides, hydrogenated rosin, disproportionated rosin, maleic rosin, newtrex one or more.
3. the preparation method of graft modification tackifying resin according to claim 1, it is characterised in that：The oleic series
Monomer be acrylic acid, methacrylic acid, methyl acrylate, methyl methacrylate, ethyl acrylate, ethyl methacrylate,
Hydroxy-ethyl acrylate, hydroxyethyl methacrylate, hydroxypropyl acrylate, hydroxy propyl methacrylate, butyl acrylate, methyl-prop
One or more of olefin(e) acid butyl ester, Isooctyl acrylate monomer, isooctyl methacrylate.
4. the preparation method of graft modification tackifying resin according to claim 1, it is characterised in that：The grafted monomers are also
Including one or both of styrene, maleic anhydride.
5. the preparation method of graft modification tackifying resin according to claim 1, which is characterized in that the initiator was
One in Benzoyl Oxide, the benzoyl peroxide tert-butyl ester, methyl ethyl ketone peroxide, cumyl peroxide, azodiisobutyronitrile
Kind.
6. the preparation method of graft modification tackifying resin according to claim 1, which is characterized in that the antioxidant is bar
This husband Irganox 565, Irganox 1010, Irganox 1076, Irganox1425, Irganox1520, Irganox
B551、Irganox B561、Irganox 1520、Irganox 1035、Irgafos 168、Sumilizer TP-D、AKEMA
The one or more of rosin resin antioxidant ROSINOX.
7. a kind of graft modification tackifying resin, which is characterized in that obtained by any preparation method of claim 1~6.
8. the application of the graft modification tackifying resin described in claim 7, which is characterized in that graft modification tackifying resin is directly used
Make hot melt adhesive or the compatilizer as the tackifying resin of hot melt adhesive or as hot melt adhesive system.
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| CN201710492287.8A CN107254023B (en) | 2017-06-26 | 2017-06-26 | Preparation method and application of graft modified tackifying resin |
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| CN201710492287.8A CN107254023B (en) | 2017-06-26 | 2017-06-26 | Preparation method and application of graft modified tackifying resin |
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| CN107254023B true CN107254023B (en) | 2018-06-29 |
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| CN113528065B (en) | 2020-04-16 | 2023-02-17 | 3M创新有限公司 | Acrylic pressure-sensitive adhesive composition, product thereof and related preparation method |
| KR102315705B1 (en) * | 2020-06-17 | 2021-10-21 | 주식회사 켐코 | Manufacturing method of adhesive composition with improved heat-resistance |
| CN112552828A (en) * | 2020-11-09 | 2021-03-26 | 宁波启合新材料科技有限公司 | High-temperature-resistant hot-melt pressure-sensitive adhesive and preparation method thereof |
| CN115537159B (en) * | 2022-12-02 | 2023-03-21 | 广州鹿山新材料股份有限公司 | Weather-resistant waterproof coiled material hot-melt pressure-sensitive adhesive and preparation method and application thereof |
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| EP1295926A1 (en) * | 2001-09-19 | 2003-03-26 | ExxonMobil Chemical Patents Inc. | Components for adhesive compositions and process for manufacture |
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