CN118240518A - Epoxy resin composition for adhesive, preparation method of epoxy resin composition and adhesive - Google Patents
Epoxy resin composition for adhesive, preparation method of epoxy resin composition and adhesive Download PDFInfo
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- CN118240518A CN118240518A CN202410502722.0A CN202410502722A CN118240518A CN 118240518 A CN118240518 A CN 118240518A CN 202410502722 A CN202410502722 A CN 202410502722A CN 118240518 A CN118240518 A CN 118240518A
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- 239000003822 epoxy resin Substances 0.000 title claims abstract description 51
- 229920000647 polyepoxide Polymers 0.000 title claims abstract description 51
- 239000000853 adhesive Substances 0.000 title claims abstract description 33
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 33
- 239000000203 mixture Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title abstract description 6
- 239000012745 toughening agent Substances 0.000 claims abstract description 18
- 229920005906 polyester polyol Polymers 0.000 claims abstract description 15
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims abstract description 14
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical group CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- 150000003077 polyols Chemical class 0.000 claims description 17
- 229920005862 polyol Polymers 0.000 claims description 15
- 150000001412 amines Chemical group 0.000 claims description 12
- -1 modified alicyclic amine Chemical class 0.000 claims description 10
- 239000004721 Polyphenylene oxide Substances 0.000 claims description 9
- 239000004841 bisphenol A epoxy resin Substances 0.000 claims description 9
- 229920000570 polyether Polymers 0.000 claims description 9
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 6
- 125000003118 aryl group Chemical group 0.000 claims description 6
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical compound C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- RNLHGQLZWXBQNY-UHFFFAOYSA-N 3-(aminomethyl)-3,5,5-trimethylcyclohexan-1-amine Chemical compound CC1(C)CC(N)CC(C)(CN)C1 RNLHGQLZWXBQNY-UHFFFAOYSA-N 0.000 claims description 4
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 claims description 4
- IMUDHTPIFIBORV-UHFFFAOYSA-N aminoethylpiperazine Chemical compound NCCN1CCNCC1 IMUDHTPIFIBORV-UHFFFAOYSA-N 0.000 claims description 4
- WERYXYBDKMZEQL-UHFFFAOYSA-N butane-1,4-diol Chemical compound OCCCCO WERYXYBDKMZEQL-UHFFFAOYSA-N 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 4
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical class OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 239000004698 Polyethylene Substances 0.000 claims description 3
- KEIQPMUPONZJJH-UHFFFAOYSA-N dicyclohexylmethanediamine Chemical compound C1CCCCC1C(N)(N)C1CCCCC1 KEIQPMUPONZJJH-UHFFFAOYSA-N 0.000 claims description 3
- 229920000768 polyamine Polymers 0.000 claims description 3
- 238000006068 polycondensation reaction Methods 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- LCZVSXRMYJUNFX-UHFFFAOYSA-N 2-[2-(2-hydroxypropoxy)propoxy]propan-1-ol Chemical compound CC(O)COC(C)COC(C)CO LCZVSXRMYJUNFX-UHFFFAOYSA-N 0.000 claims description 2
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 2
- 239000003085 diluting agent Substances 0.000 claims description 2
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical compound OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 claims description 2
- XXMIOPMDWAUFGU-UHFFFAOYSA-N hexane-1,6-diol Chemical compound OCCCCCCO XXMIOPMDWAUFGU-UHFFFAOYSA-N 0.000 claims description 2
- 229920001451 polypropylene glycol Polymers 0.000 claims description 2
- 229960004063 propylene glycol Drugs 0.000 claims description 2
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000009477 glass transition Effects 0.000 abstract description 2
- 125000003277 amino group Chemical group 0.000 abstract 1
- 238000001723 curing Methods 0.000 description 17
- 239000004593 Epoxy Substances 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 description 4
- 229920000459 Nitrile rubber Polymers 0.000 description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 4
- LNEPOXFFQSENCJ-UHFFFAOYSA-N haloperidol Chemical compound C1CC(O)(C=2C=CC(Cl)=CC=2)CCN1CCCC(=O)C1=CC=C(F)C=C1 LNEPOXFFQSENCJ-UHFFFAOYSA-N 0.000 description 4
- 238000000034 method Methods 0.000 description 4
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 description 3
- 150000001299 aldehydes Chemical class 0.000 description 3
- 150000008064 anhydrides Chemical class 0.000 description 3
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- VILCJCGEZXAXTO-UHFFFAOYSA-N 2,2,2-tetramine Chemical compound NCCNCCNCCN VILCJCGEZXAXTO-UHFFFAOYSA-N 0.000 description 2
- PIICEJLVQHRZGT-UHFFFAOYSA-N Ethylenediamine Chemical compound NCCN PIICEJLVQHRZGT-UHFFFAOYSA-N 0.000 description 2
- FQYUMYWMJTYZTK-UHFFFAOYSA-N Phenyl glycidyl ether Chemical compound C1OC1COC1=CC=CC=C1 FQYUMYWMJTYZTK-UHFFFAOYSA-N 0.000 description 2
- FDLQZKYLHJJBHD-UHFFFAOYSA-N [3-(aminomethyl)phenyl]methanamine Chemical compound NCC1=CC=CC(CN)=C1 FDLQZKYLHJJBHD-UHFFFAOYSA-N 0.000 description 2
- IISBACLAFKSPIT-UHFFFAOYSA-N bisphenol A Chemical compound C=1C=C(O)C=CC=1C(C)(C)C1=CC=C(O)C=C1 IISBACLAFKSPIT-UHFFFAOYSA-N 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 239000012948 isocyanate Substances 0.000 description 2
- 150000002513 isocyanates Chemical class 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- QWVGKYWNOKOFNN-UHFFFAOYSA-N o-cresol Chemical compound CC1=CC=CC=C1O QWVGKYWNOKOFNN-UHFFFAOYSA-N 0.000 description 2
- 229920002635 polyurethane Polymers 0.000 description 2
- 239000004814 polyurethane Substances 0.000 description 2
- JOLVYUIAMRUBRK-UHFFFAOYSA-N 11',12',14',15'-Tetradehydro(Z,Z-)-3-(8-Pentadecenyl)phenol Natural products OC1=CC=CC(CCCCCCCC=CCC=CCC=C)=C1 JOLVYUIAMRUBRK-UHFFFAOYSA-N 0.000 description 1
- YLKVIMNNMLKUGJ-UHFFFAOYSA-N 3-Delta8-pentadecenylphenol Natural products CCCCCCC=CCCCCCCCC1=CC=CC(O)=C1 YLKVIMNNMLKUGJ-UHFFFAOYSA-N 0.000 description 1
- QHPQWRBYOIRBIT-UHFFFAOYSA-N 4-tert-butylphenol Chemical compound CC(C)(C)C1=CC=C(O)C=C1 QHPQWRBYOIRBIT-UHFFFAOYSA-N 0.000 description 1
- JOLVYUIAMRUBRK-UTOQUPLUSA-N Cardanol Chemical compound OC1=CC=CC(CCCCCCC\C=C/C\C=C/CC=C)=C1 JOLVYUIAMRUBRK-UTOQUPLUSA-N 0.000 description 1
- FAYVLNWNMNHXGA-UHFFFAOYSA-N Cardanoldiene Natural products CCCC=CCC=CCCCCCCCC1=CC=CC(O)=C1 FAYVLNWNMNHXGA-UHFFFAOYSA-N 0.000 description 1
- BRLQWZUYTZBJKN-UHFFFAOYSA-N Epichlorohydrin Chemical compound ClCC1CO1 BRLQWZUYTZBJKN-UHFFFAOYSA-N 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- PTFIPECGHSYQNR-UHFFFAOYSA-N cardanol Natural products CCCCCCCCCCCCCCCC1=CC=CC(O)=C1 PTFIPECGHSYQNR-UHFFFAOYSA-N 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007123 defense Effects 0.000 description 1
- 230000001627 detrimental effect Effects 0.000 description 1
- 125000003700 epoxy group Chemical group 0.000 description 1
- UYMKPFRHYYNDTL-UHFFFAOYSA-N ethenamine Chemical compound NC=C UYMKPFRHYYNDTL-UHFFFAOYSA-N 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000013007 heat curing Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000011159 matrix material Substances 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000010125 resin casting Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004154 testing of material Methods 0.000 description 1
- 229920005992 thermoplastic resin Polymers 0.000 description 1
- YXFVVABEGXRONW-UHFFFAOYSA-N toluene Substances CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 1
- DSROZUMNVRXZNO-UHFFFAOYSA-K tris[(1-naphthalen-1-yl-3-phenylnaphthalen-2-yl)oxy]alumane Chemical compound C=1C=CC=CC=1C=1C=C2C=CC=CC2=C(C=2C3=CC=CC=C3C=CC=2)C=1O[Al](OC=1C(=C2C=CC=CC2=CC=1C=1C=CC=CC=1)C=1C2=CC=CC=C2C=CC=1)OC(C(=C1C=CC=CC1=C1)C=2C3=CC=CC=C3C=CC=2)=C1C1=CC=CC=C1 DSROZUMNVRXZNO-UHFFFAOYSA-K 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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
- C09J163/00—Adhesives based on epoxy resins; Adhesives based on derivatives of epoxy resins
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Epoxy Resins (AREA)
- Adhesives Or Adhesive Processes (AREA)
Abstract
The invention relates to the technical field of adhesives, in particular to an epoxy resin composition for an adhesive, a preparation method of the epoxy resin composition and the adhesive. The epoxy resin composition for the adhesive comprises a component A and a component B; the component A comprises the following components in parts by weight: 100 parts of epoxy resin and 1-25 parts of toughening agent; the component B is an amine curing agent; wherein the toughening agent is phthalic anhydride polyester polyol. The epoxy resin composition provided by the invention can improve the elongation at break and tensile breaking energy, and has the advantages of higher glass transition temperature Tg and good comprehensive performance.
Description
Technical Field
The invention relates to the technical field of adhesives, in particular to an epoxy resin composition for an adhesive, a preparation method of the epoxy resin composition and the adhesive.
Background
Epoxy resins (EP) refer to the generic name for a class of polymers containing more than two epoxy groups in the molecule. It is the polycondensation product of epichlorohydrin with bisphenol a or a polyol. Due to the chemical activity of epoxy, the epoxy can be ring-opened by using various compounds containing active hydrogen, and is in a highly cross-linked three-dimensional network structure after curing, and the epoxy has excellent bonding strength, dielectric property, corrosion resistance, mechanical property and lower curing shrinkage rate, and is widely applied to the fields of paint, adhesive, insulating material, national defense, military industry, aerospace, construction, light industry and the like as an excellent matrix material. However, cured products thereof have disadvantages such as brittleness, poor toughness, poor heat resistance, poor impact resistance, and the like, which restrict the application thereof, and therefore, it is necessary to toughen and modify epoxy resins, and particularly, when used as adhesives, it is necessary to properly toughen and modify the epoxy resins so as to satisfy practical technical and cost requirements.
In general, toughening modification is to add a toughening agent into epoxy resin, and the toughening purpose is achieved through various toughening mechanisms, and related technicians perform a lot of researches on the toughening modification of the epoxy resin, wherein common toughening agents are as follows: reactive liquid nitrile rubbers such as carboxyl terminated nitrile rubber (CTBN) and amine terminated nitrile rubber (ABTN); thermoplastic resins such as polyvinyl butyral (PVB); blocked isocyanate or epoxy modified polyurethane tougheners; polyether polyols; polyester polyols.
However, the existing toughening agents still have the following defects: when the reactive liquid nitrile rubber is used with a curing agent at normal temperature, CTBN and excessive epoxy resin need to be reacted in advance to obtain modified epoxy resin, the viscosity is very large and the price is high, ATBN has poor compatibility with some high-polarity curing agents, and the viscosity is also very large and the price is high; PVB has a significant increase in viscosity due to its high molecular weight after it is added to the epoxy resin, which in some cases can lead to processing difficulties and can be detrimental to increasing filler loading; the viscosity of the blocked isocyanate or epoxy modified polyurethane toughener is also relatively high and is mostly used for improving flexibility; polyether polyol, chinese patent application CN102884100a mentions that low molecular weight polyether polyols, although low in viscosity and low in cost, greatly lower Tg of the cured product and are often used in heat-curable anhydride systems; the polyester polyol, chinese patent application CN103396536A, adopts aromatic trimethyl anhydride or tetramethyl anhydride to react with polyol to obtain the polyester polyol toughening agent, and the modified condensate maintains high heat distortion temperature and good impact resistance, but the viscosity of the modified condensate is more than 5000 centipoise at 25 ℃, and the modified condensate is an anhydride system for heat curing.
Therefore, it is highly desired to find a new way to improve the defects of the cured epoxy resin such as high brittleness, poor toughness and poor impact resistance.
Disclosure of Invention
In order to solve the technical problems in the prior art, the invention provides an epoxy resin composition for an adhesive, a preparation method thereof and the adhesive.
The technical scheme for solving the technical problems is as follows:
the first aspect of the invention provides an epoxy resin composition for an adhesive, which is characterized by comprising a component A and a component B;
the component A comprises the following components in parts by weight: 100 parts of epoxy resin and 1-25 parts of toughening agent;
the component B is an amine curing agent;
wherein the toughening agent is phthalic anhydride polyester polyol.
Based on the technical scheme, the invention can also make the following improvements:
Further, the phthalic anhydride polyester polyol is obtained by polycondensation of phthalic anhydride and a polyol selected from a small molecular polyol or a small molecular polyether polyol.
Further, the small molecular polyol is selected from any one or more of ethylene glycol, 1, 2-propylene glycol, 1, 4-butanediol, 1, 6-hexanediol, diethylene glycol, triethylene glycol, dipropylene glycol, tripropylene glycol, trimethylolpropane, glycerol and low molecular weight polyethylene glycol, and the small molecular weight polyether polyol is selected from polyethylene glycol or polypropylene glycol.
Further, the amine curing agent is modified alicyclic amine or modified aliphatic amine.
Further, the modified aliphatic amine is any one of an addition product of polyethylene polyamine and aromatic glycidyl ether, mannich base (phenolic amine) or polyether amine, preferably an addition product obtained by reacting diethylene triamine (DETA) with Phenyl Glycidyl Ether (PGE) or o-toluene glycidyl ether (CGE), and more preferably a polyethylene polyamine modified JH-5413-3M curing agent, so as to improve the compatibility with epoxy resin.
The Mannich base is a phenolic amine type curing agent and is obtained by reacting phenol, aldehyde and amine, wherein the phenol is generally phenol, and nonylphenol, o-cresol, p-tert-butylphenol and cardanol can also be adopted; the amine is usually vinylamine such as Ethylenediamine (EDA), diethylenetriamine (DETA), triethylenetetramine (TETA), and other amines such as m-xylylenediamine (MXDA), isophoronediamine (IPDA); formaldehyde is generally used as the aldehyde, and other aldehydes may be used.
Further, the modified alicyclic amine is any one of an adduct of isophorone diamine and bisphenol a epoxy resin, an adduct of diamino dicyclohexylmethane (PACM) and bisphenol a epoxy resin, an adduct of aminoethylpiperazine and aromatic glycidyl ether, and an adduct of aminoethylpiperazine and bisphenol a epoxy resin.
Further, the phthalic anhydride polyester polyol is STEPANOL PDP-70.
Further, the epoxy resin is bisphenol A type epoxy resin, preferably NPEL-128.
The beneficial effects of adopting the further technical scheme are that: the structure of the phthalic anhydride polyester polyol and the bisphenol A epoxy resin contains aromatic structural groups, and according to the similar compatibility principle, the phthalic anhydride polyester polyol and the bisphenol A epoxy resin have good compatibility, and the polarity of ester bonds contained in the phthalic anhydride polyester polyol structure is high, so that the compatibility of the phthalic anhydride polyester polyol and the bisphenol A epoxy resin is improved.
Further, the component A also comprises 0-20 parts of diluent to reduce viscosity.
Further, the weight ratio of the component A to the component B is 100:25-50.
The weight ratio of the component A to the component B is calculated according to the epoxy equivalent of the component A and the active hydrogen equivalent of the component B and is obtained through experimental optimization.
The second aspect of the present invention provides a method for preparing the epoxy resin composition for adhesive, comprising the steps of:
(1) Heating the epoxy resin and the toughening agent to 60-80 ℃ according to parts by weight, stirring and mixing for 30-60 minutes, and then standing and cooling to room temperature to obtain a component A for later use;
(2) And uniformly mixing the component A and the component B at normal temperature, and curing to obtain the epoxy resin composition for the adhesive.
In another aspect, the present invention provides an adhesive comprising the epoxy resin composition for adhesive.
Compared with the prior art, the invention has the following technical effects:
The invention selects phthalic anhydride polyester polyol as the toughening agent of epoxy resin, and the main chain of the toughening agent contains rigid benzene ring structure and polar ester bond, and also contains flexible polyol chain segment, which has lower viscosity, the viscosity at 25 ℃ is 1000-5000 centipoise, and the toughening agent has good compatibility with epoxy resin and amine curing agent, low viscosity and high cost performance.
Drawings
FIG. 1 shows stress-strain curves for tensile strength testing of various examples and comparative examples of the present invention (0 PHR: comparative example, 5PHR: example 1, 10PHR: example 2, 15PHR: example 3).
Detailed Description
Further advantages and effects of the present invention will become apparent to those skilled in the art from the disclosure of the present specification, by describing the embodiments of the present invention with specific examples. While the description of the invention will be described in connection with the preferred embodiments, it is not intended to limit the inventive features to the implementation. Rather, the purpose of the invention described in connection with the embodiments is to cover other alternatives or modifications, which may be extended by the claims based on the invention. The following description contains many specific details for the purpose of providing a thorough understanding of the present invention. The invention may be practiced without these specific details. Furthermore, some specific details are omitted from the description in order to avoid obscuring the invention. It should be noted that, without conflict, the embodiments of the present invention and features of the embodiments may be combined with each other.
Example 1
The preparation process comprises the following steps:
(1) Weighing 100g NPEL-128 g of STEPANOL PDP-70, heating to 60 ℃, stirring and mixing for 30 minutes, and then cooling to room temperature to obtain an epoxy A component for later use;
(2) Adopting a modified fatty amine curing agent JH-5413-3M as a component B, wherein the dosage is 1/3 of NPEL-128;
(3) And uniformly mixing the component A and the component B at normal temperature, and then curing at 40 ℃ for 24 hours to obtain the epoxy resin composition of the example 1.
Example 2
STEPANOL PDP-70 was added in an amount of 10g, with the remainder being as in example 1.
Example 3
STEPANOL PDP-70 was added in an amount of 15g, the remainder being as in example 1.
Comparative example
Phthalic anhydride polyester polyol was not added, and the other was the same as in example 1.
Note that: examples 1-3 and comparative examples were each cured using a curing condition at 40℃for 24 hours, which had a curing effect equivalent to that of a curing at ordinary temperature for seven days, and the present invention shortened the curing time by increasing the curing temperature.
The epoxy resin compositions of examples 1 to 3 and comparative examples were subjected to performance test by the following methods:
the tensile property is detected according to GB/T2567-2008 method for testing the property of a resin casting body, and an electronic tensile machine is a LLOYD EZ20 material testing machine;
Shear strength was tested according to GB/T7124-2008 "determination of adhesive tensile shear Strength (rigid Material to rigid Material");
Tg was measured using DSC apparatus; solidifying at 40-250deg.C by heating rate of 10deg.C/min, cooling to 25deg.C, scanning at heating rate of 10deg.C/min, and measuring at 150deg.C by midpoint method.
The specific performance data are shown in Table 1.
Table 1 Performance data of epoxy resin compositions
Note that: fracture energy: the integrated area of the stress-strain plot of the tensile strength test (as shown in fig. 1) divided by the tensile spline fracture area (tensile spline fracture area 1.28 x 0.33cm 2).
As can be seen from Table 1, the toughening agent content increased from 0 to 15 parts by weight, and the tensile break energy increased from 4.41J/cm 2 to 7.15J/cm 2 by 62.1%; elongation at break increased from 2.62% to 4.13%; and the glass transition temperature Tg is only slightly reduced from 70.4 ℃ to 64.41 ℃, the degree of reduction of the tensile strength is not very high and is maintained at a higher level, which shows that the toughening agent has good toughening effect and low viscosity (2000 centipoise, 25 ℃).
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (10)
1. An epoxy resin composition for an adhesive is characterized by comprising a component A and a component B;
the component A comprises the following components in parts by weight: 100 parts of epoxy resin and 1-25 parts of toughening agent;
the component B is an amine curing agent;
wherein the toughening agent is phthalic anhydride polyester polyol.
2. The epoxy resin composition for adhesives according to claim 1, wherein the phthalic anhydride polyester polyol is obtained by polycondensation of phthalic anhydride and a polyol selected from a small molecular polyol or a small molecular polyether polyol.
3. The epoxy resin composition for an adhesive according to claim 2, wherein the small molecular weight polyol is selected from any one or more of ethylene glycol, 1, 2-propylene glycol, 1, 4-butanediol, 1, 6-hexanediol, diethylene glycol, triethylene glycol, dipropylene glycol, tripropylene glycol, trimethylolpropane, glycerol, and low molecular weight polyethylene glycol, and the small molecular weight polyether polyol is selected from polyethylene glycol or polypropylene glycol.
4. The epoxy resin composition for adhesives according to claim 1, wherein the amine curing agent is a modified alicyclic amine or a modified aliphatic amine.
5. The epoxy resin composition for an adhesive according to claim 4, wherein the modified aliphatic amine is any one of an addition product of polyethylene polyamine and aromatic glycidyl ether, mannich base, and polyether amine; the modified alicyclic amine is any one of an adduct of isophorone diamine and bisphenol A epoxy resin, an adduct of diamino dicyclohexylmethane and bisphenol A epoxy resin, an adduct of aminoethylpiperazine and aromatic glycidyl ether, and an adduct of aminoethylpiperazine and bisphenol A epoxy resin.
6. The epoxy resin composition for an adhesive according to claim 1, wherein the epoxy resin is a bisphenol a type epoxy resin.
7. The epoxy resin composition for an adhesive according to claim 1, wherein the a component further comprises 0 to 20 parts of a diluent.
8. The epoxy resin composition for adhesive according to claim 1, wherein the weight ratio of the a component to the B component is 100:25-50.
9. A method for producing the epoxy resin composition for adhesive according to any one of claims 1 to 8, comprising the steps of:
(1) Heating the epoxy resin and the toughening agent to 60-80 ℃ according to parts by weight, stirring and mixing for 30-60 minutes, and then standing and cooling to room temperature to obtain a component A for later use;
(2) And uniformly mixing the component A and the component B at normal temperature, and curing to obtain the epoxy resin composition for the adhesive.
10. An adhesive comprising the epoxy resin composition for adhesive according to any one of claims 1 to 8.
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| CN202410502722.0A CN118240518B (en) | 2024-04-25 | Epoxy resin composition for adhesive, preparation method of epoxy resin composition and adhesive |
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| CN202410502722.0A CN118240518B (en) | 2024-04-25 | Epoxy resin composition for adhesive, preparation method of epoxy resin composition and adhesive |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101709208A (en) * | 2009-12-22 | 2010-05-19 | 大连凯华新技术工程有限公司 | Building structure adhesive with high impact and peeling strength |
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101709208A (en) * | 2009-12-22 | 2010-05-19 | 大连凯华新技术工程有限公司 | Building structure adhesive with high impact and peeling strength |
Non-Patent Citations (1)
| Title |
|---|
| 刘业强 等: "聚酯增韧环氧树脂灌封胶的研究", 刘业强 等, vol. 40, no. 2, 28 February 2007 (2007-02-28) * |
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