CN114806087A - Epoxy resin-anhydride system for vacuum infusion of wind power blade and preparation method thereof - Google Patents
Epoxy resin-anhydride system for vacuum infusion of wind power blade and preparation method thereof Download PDFInfo
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- CN114806087A CN114806087A CN202210292243.1A CN202210292243A CN114806087A CN 114806087 A CN114806087 A CN 114806087A CN 202210292243 A CN202210292243 A CN 202210292243A CN 114806087 A CN114806087 A CN 114806087A
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- epoxy resin
- anhydride
- curing agent
- vacuum infusion
- agent
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- 239000004593 Epoxy Substances 0.000 title claims abstract description 67
- 238000009755 vacuum infusion Methods 0.000 title claims abstract description 58
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 239000003822 epoxy resin Substances 0.000 claims abstract description 74
- 229920000647 polyepoxide Polymers 0.000 claims abstract description 74
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 67
- 150000008064 anhydrides Chemical class 0.000 claims abstract description 41
- 239000011159 matrix material Substances 0.000 claims abstract description 33
- 239000007787 solid Substances 0.000 claims abstract description 30
- 229920005989 resin Polymers 0.000 claims abstract description 29
- 239000011347 resin Substances 0.000 claims abstract description 29
- 239000000463 material Substances 0.000 claims abstract description 22
- 239000004850 liquid epoxy resins (LERs) Substances 0.000 claims abstract description 20
- 239000012745 toughening agent Substances 0.000 claims abstract description 19
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 17
- 239000003085 diluting agent Substances 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims description 53
- 238000010438 heat treatment Methods 0.000 claims description 22
- 229920001971 elastomer Polymers 0.000 claims description 14
- -1 glycidyl amines Chemical class 0.000 claims description 14
- RAXXELZNTBOGNW-UHFFFAOYSA-N imidazole Natural products C1=CNC=N1 RAXXELZNTBOGNW-UHFFFAOYSA-N 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 229920000642 polymer Polymers 0.000 claims description 12
- 239000007788 liquid Substances 0.000 claims description 11
- 239000002518 antifoaming agent Substances 0.000 claims description 10
- 239000005060 rubber Substances 0.000 claims description 9
- 150000005846 sugar alcohols Polymers 0.000 claims description 9
- 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 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 239000004843 novolac epoxy resin Substances 0.000 claims description 7
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 6
- 150000008065 acid anhydrides Chemical class 0.000 claims description 6
- PXKLMJQFEQBVLD-UHFFFAOYSA-N bisphenol F Chemical compound C1=CC(O)=CC=C1CC1=CC=C(O)C=C1 PXKLMJQFEQBVLD-UHFFFAOYSA-N 0.000 claims description 6
- 150000003839 salts Chemical class 0.000 claims description 6
- 150000003512 tertiary amines Chemical class 0.000 claims description 6
- 239000000806 elastomer Substances 0.000 claims description 5
- 229920000587 hyperbranched polymer Polymers 0.000 claims description 5
- 229920005992 thermoplastic resin Polymers 0.000 claims description 5
- 150000002460 imidazoles Chemical class 0.000 claims description 4
- 239000002253 acid Substances 0.000 claims description 3
- 125000002723 alicyclic group Chemical group 0.000 claims description 3
- 150000001336 alkenes Chemical class 0.000 claims description 3
- WPYMKLBDIGXBTP-UHFFFAOYSA-N benzoic acid Chemical compound OC(=O)C1=CC=CC=C1 WPYMKLBDIGXBTP-UHFFFAOYSA-N 0.000 claims description 3
- 150000007942 carboxylates Chemical class 0.000 claims description 3
- 239000011258 core-shell material Substances 0.000 claims description 3
- 239000007822 coupling agent Substances 0.000 claims description 3
- GYZLOYUZLJXAJU-UHFFFAOYSA-N diglycidyl ether Chemical class C1OC1COCC1CO1 GYZLOYUZLJXAJU-UHFFFAOYSA-N 0.000 claims description 3
- 239000000539 dimer Substances 0.000 claims description 3
- 125000003055 glycidyl group Chemical group C(C1CO1)* 0.000 claims description 3
- 229910052736 halogen Inorganic materials 0.000 claims description 3
- 150000002367 halogens Chemical class 0.000 claims description 3
- WJRBRSLFGCUECM-UHFFFAOYSA-N hydantoin Chemical compound O=C1CNC(=O)N1 WJRBRSLFGCUECM-UHFFFAOYSA-N 0.000 claims description 3
- 229940091173 hydantoin Drugs 0.000 claims description 3
- 239000012948 isocyanate Substances 0.000 claims description 3
- 150000002513 isocyanates Chemical class 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 150000003242 quaternary ammonium salts Chemical class 0.000 claims description 3
- 150000004023 quaternary phosphonium compounds Chemical class 0.000 claims description 3
- 239000000080 wetting agent Substances 0.000 claims description 3
- 239000003292 glue Substances 0.000 claims description 2
- VOOLKNUJNPZAHE-UHFFFAOYSA-N formaldehyde;2-methylphenol Chemical compound O=C.CC1=CC=CC=C1O VOOLKNUJNPZAHE-UHFFFAOYSA-N 0.000 claims 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims 1
- 239000000835 fiber Substances 0.000 abstract description 2
- 229920000459 Nitrile rubber Polymers 0.000 description 9
- RSWGJHLUYNHPMX-UHFFFAOYSA-N 1,4a-dimethyl-7-propan-2-yl-2,3,4,4b,5,6,10,10a-octahydrophenanthrene-1-carboxylic acid Chemical compound C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 description 8
- 238000004806 packaging method and process Methods 0.000 description 8
- 238000007789 sealing Methods 0.000 description 8
- 239000004721 Polyphenylene oxide Substances 0.000 description 6
- 229920000570 polyether Polymers 0.000 description 6
- OYBMVMAXKOGYDC-UHFFFAOYSA-N CTPB Chemical compound CCCCCCCCCCCCCCCC1=CC=CC(OCC)=C1C(=O)NC1=CC=C(Cl)C(C(F)(F)F)=C1 OYBMVMAXKOGYDC-UHFFFAOYSA-N 0.000 description 4
- 239000006087 Silane Coupling Agent Substances 0.000 description 4
- NTXGQCSETZTARF-UHFFFAOYSA-N buta-1,3-diene;prop-2-enenitrile Chemical compound C=CC=C.C=CC#N NTXGQCSETZTARF-UHFFFAOYSA-N 0.000 description 4
- QWVGKYWNOKOFNN-UHFFFAOYSA-N o-cresol Chemical compound CC1=CC=CC=C1O QWVGKYWNOKOFNN-UHFFFAOYSA-N 0.000 description 4
- 150000001412 amines Chemical class 0.000 description 3
- HPILSDOMLLYBQF-UHFFFAOYSA-N 2-[1-(oxiran-2-ylmethoxy)butoxymethyl]oxirane Chemical compound C1OC1COC(CCC)OCC1CO1 HPILSDOMLLYBQF-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 229920001083 polybutene Polymers 0.000 description 2
- 229920000728 polyester Polymers 0.000 description 2
- YSUQLAYJZDEMOT-UHFFFAOYSA-N 2-(butoxymethyl)oxirane Chemical compound CCCCOCC1CO1 YSUQLAYJZDEMOT-UHFFFAOYSA-N 0.000 description 1
- FQYUMYWMJTYZTK-UHFFFAOYSA-N Phenyl glycidyl ether Chemical compound C1OC1COC1=CC=CC=C1 FQYUMYWMJTYZTK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229920005862 polyol Polymers 0.000 description 1
- 150000003077 polyols Chemical class 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L63/00—Compositions of epoxy resins; Compositions of derivatives of epoxy resins
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/42—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
- C08G59/4207—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof aliphatic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/42—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
- C08G59/4215—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof cycloaliphatic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/42—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
- C08G59/4223—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof aromatic
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/42—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof
- C08G59/423—Polycarboxylic acids; Anhydrides, halides or low molecular weight esters thereof containing an atom other than oxygen belonging to a functional groups to C08G59/42, carbon and hydrogen
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Epoxy Resins (AREA)
Abstract
The invention relates to the technical field of epoxy resin materials, in particular to an epoxy resin-anhydride system for vacuum infusion of wind power blades and a preparation method thereof, wherein a resin matrix comprises the following components in parts by weight: 60-100 parts of liquid epoxy resin, 0-10 parts of solid epoxy resin, 0-20 parts of epoxy diluent, 0-20 parts of toughening agent and 0-1 part of auxiliary agent; the curing agent comprises the following components: 60-95 parts of anhydride curing agent, 0-30 parts of flexibilizer, 0.5-5.0 parts of accelerator and 0-1 part of auxiliary agent. The epoxy resin-anhydride system for vacuum infusion of the wind power blade can ensure that anhydride serving as a curing agent is cured at the medium temperature of 60-100 ℃ on the premise of good operable time and good fiber wettability.
Description
Technical Field
The invention relates to the technical field of epoxy resin materials, in particular to a preparation method of an epoxy resin-acid anhydride system for vacuum infusion of wind power blades.
Background
The epoxy resin vacuum infusion system is a composite system consisting of epoxy resin and a curing agent system, and amines are generally used as curing agents in epoxy resin compositions for vacuum infusion at present. The prior art does not disclose an unlimited epoxy resin-anhydride system suitable for vacuum infusion of wind power blades.
Disclosure of Invention
The invention aims to provide an epoxy resin-anhydride system for vacuum infusion of wind power blades and a preparation method thereof, and aims to solve the problem that the existing anhydride used as an epoxy resin curing agent can be cured only by heating at high temperature.
The invention provides an epoxy resin-anhydride system for vacuum infusion of wind power blades, which comprises the following components in parts by weight:
resin matrix part A:
b curing agent moiety
Further, the epoxy resin includes one or more of glycidyl ethers (including but not limited to bisphenol a type liquid epoxy resin, bisphenol F type epoxy resin, liquid novolac epoxy resin), glycidyl esters, glycidyl amines, alicyclic epoxy resin, epoxidized olefins or hydantoin epoxy resin.
Further, the solid epoxy resin comprises one or more of bisphenol A type solid epoxy resin, solid novolac epoxy resin or o-cresol novolac epoxy resin.
Further, the toughening agent comprises one or more of polyalcohol, hydroxyl-terminated polymer, rubber elastomer, thermoplastic resin, core-shell polymer, dimer acid modified epoxy resin, isocyanate modified epoxy resin or hyperbranched polymer.
Optionally, the rubber elastomer comprises CTBN, CTPB, HTBN, or the like.
Wherein CTBN refers to carboxyl-terminated butadiene-acrylonitrile rubber; CTPB refers to carboxyl-terminated liquid polybutene dirubber; HTBN (carboxylic-terminated nitrile rubber) refers to hydroxyl terminated liquid nitrile rubbers.
Optionally, the thermoplastic resin comprises a polyoxy resin or a polyether.
Optionally, the hyperbranched polymer comprises a polyester-based hyperbranched epoxy resin or a polyether-based hyperbranched epoxy resin.
Further, the acid anhydride comprises one or a mixture of several of aromatic acid anhydride, alicyclic acid anhydride, aliphatic acid anhydride and halogen-containing acid anhydride.
Further, the accelerator comprises one or a mixture of more of tertiary amine and salt thereof, acetylacetone metal salt, organic carboxylate and complex thereof, quaternary ammonium salt, quaternary phosphonium compound, imidazole or modified imidazole.
Further, the auxiliary agent comprises several or a mixture of several of a coupling agent, a defoaming agent and a wetting agent.
In a second aspect, the invention provides a preparation method of the epoxy resin-anhydride system for vacuum infusion of the wind power blade, which comprises the following steps:
preparing a resin matrix intermediate material: adding the solid epoxy resin into the liquid epoxy resin according to the weight part ratio of 1-3:1-3, fully dissolving the solid epoxy resin at the temperature of 100-130 ℃, uniformly stirring, and reducing the temperature to room temperature to obtain a resin matrix intermediate material;
preparing an anhydride curing agent intermediate material: adding the anhydride into the polyalcohol and the hydroxyl-terminated polymer according to the weight part ratio of 1-3:1-3, fully and uniformly stirring the anhydride at the temperature of 100-130 ℃, and then reducing the temperature to room temperature to obtain an anhydride curing agent intermediate material;
step method for preparing epoxy resin-anhydride system for vacuum infusion wind power blade
a) Epoxy resin matrix part: and if no solid resin is used, heating the liquid epoxy resin to 50-80 ℃, adding the epoxy diluent, the toughening agent and the auxiliary agent into the liquid epoxy resin, keeping the stirring speed of 120-150rpm, and stirring for 30-45min to obtain the epoxy resin matrix part of the epoxy resin-anhydride system for the vacuum infusion wind power blade.
If solid resin is used, firstly, heating the liquid epoxy resin to 95-105 ℃, adding the solid epoxy resin into the liquid epoxy resin, continuously heating to 120-;
secondly, reducing the heating temperature to 70-75 ℃, adding the epoxy diluent, the toughening agent and the auxiliary agent, and continuing stirring for 15-30min at the stirring speed of 120-150 rpm;
finally, reducing the heating temperature to 20-35 ℃ to obtain an epoxy resin matrix part of the epoxy resin-anhydride system for the vacuum infusion wind power blade;
b) curing agent part: if the anhydride curing agent intermediate is not used, adding the toughening agent, the accelerator and the auxiliary agent into the anhydride, keeping the stirring speed of 120-150rpm, and stirring for 30-45min to obtain the curing agent part of the epoxy resin-anhydride system for the vacuum infusion wind power blade;
if an anhydride curing agent intermediate is used, firstly heating the toughening agent polyalcohol and the hydroxyl-terminated polymer to 95-105 ℃, adding the solid or liquid anhydride, continuously heating to 110-130 ℃, keeping the constant temperature for 2-3h, and keeping the stirring speed of 120-150rpm to fully dissolve the solid anhydride, cooling to room temperature for later use (or cooling to 30-40 ℃, adding the anhydride, the toughening agent, the accelerator and the auxiliary agent, and continuously stirring uniformly to obtain the curing agent part), thereby obtaining the anhydride curing agent intermediate;
secondly, reducing the temperature of the anhydride curing agent intermediate to 30-40 ℃, adding the anhydride, the toughening agent, the accelerant and the auxiliary agent, keeping the stirring speed of 120-150rpm, and stirring for 30-45min to obtain the curing agent part of the epoxy resin-anhydride system for the vacuum-poured wind power blade;
c) the epoxy resin-anhydride system for vacuum infusion of the wind power blade is prepared by automatically and uniformly mixing an epoxy resin matrix part and a curing agent part in proportion by a glue mixer to obtain the epoxy resin-anhydride system for vacuum infusion of the wind power blade, wherein the epoxy resin matrix part and the curing agent part are mixed according to the proportion of 100: 90-120 ℃, and the temperature of the feed liquid is 25-40 ℃.
Further, in the preparation method, the epoxy resin-anhydride system for vacuum infusion of the wind power blade comprises the following components in parts by weight:
resin matrix part A:
b curing agent moiety
Further, the liquid epoxy resin includes one or more of glycidyl ethers (including but not limited to bisphenol a type liquid epoxy resin, bisphenol F type epoxy resin, liquid novolac epoxy resin), glycidyl esters, glycidyl amines, alicyclic epoxy resin, epoxidized olefins or hydantoin epoxy resin.
Further, the solid epoxy resin comprises one or more of bisphenol A type solid epoxy resin, solid novolac epoxy resin or o-cresol novolac epoxy resin.
Further, the toughening agent comprises one or more of polyalcohol, hydroxyl-terminated polymer, rubber elastomer, thermoplastic resin, core-shell polymer, dimer acid modified epoxy resin, isocyanate modified epoxy resin or hyperbranched polymer.
Optionally, the rubber elastomer comprises CTBN, CTPB, HTBN, or the like.
Wherein CTBN refers to carboxyl-terminated butadiene-acrylonitrile rubber; CTPB refers to carboxyl-terminated liquid polybutene dirubber; HTBN (carboxylic-terminated nitrile rubber) refers to hydroxyl terminated liquid nitrile rubbers.
Optionally, the thermoplastic resin comprises a polyoxy resin or a polyether.
Optionally, the hyperbranched polymer comprises a polyester-based hyperbranched epoxy resin or a polyether-based hyperbranched epoxy resin.
Further, the acid anhydride comprises one or a mixture of more of aromatic acid anhydride, alicyclic acid anhydride, aliphatic acid anhydride and halogen-containing acid anhydride.
Further, the accelerator comprises one or a mixture of more of tertiary amine and salt thereof, acetylacetone metal salt, organic carboxylate and complex thereof, quaternary ammonium salt, quaternary phosphonium compound, imidazole or modified imidazole.
Further, the auxiliary agent comprises several or a mixture of several of a coupling agent, a defoaming agent and a wetting agent.
Compared with the prior art, the invention has the following beneficial effects:
the epoxy resin-anhydride system for the vacuum infusion wind power blade is obtained by selecting specific components and proportions, and the anhydride is used as the curing agent to be cured at the medium temperature of 60-100 ℃ on the premise of good operable time and fiber wettability because the anhydride curing agent is used instead of amines as the curing agent.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "comprises" and "comprising," and any variations thereof, of embodiments of the present invention are intended to cover non-exclusive inclusions, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
In the invention, the raw material components such as liquid epoxy resin, solid epoxy resin, epoxy diluent, toughening agent, anhydride curing agent, accelerator, auxiliary agent and the like can be obtained by commercial purchase.
Example one
The embodiment provides an epoxy resin-anhydride system for vacuum infusion of a wind power blade, which comprises the following components in parts by weight:
resin matrix part A:
b curing agent moiety
The preparation method of the epoxy resin-anhydride system for the vacuum infusion wind power blade comprises the following steps:
preparing the components in parts by weight;
a) preparing a resin matrix intermediate material: under the condition that the stirring speed is 100-300rpm, the weight portion ratio of 1:3, slowly adding the E20 solid resin into the E51 epoxy resin, stirring and heating, controlling the temperature to be less than or equal to 150 ℃, stirring and dispersing for 45-60 minutes until the solid resin is completely dissolved, and cooling to room temperature to obtain the resin matrix intermediate material.
Preparation of the epoxy resin part:
heating the rest E51 epoxy resin to 60-70 ℃, adding the resin matrix intermediate, adding the phenyl glycidyl ether diluent, the silane coupling agent and the defoaming agent, and continuously stirring for 45-60min at the stirring speed of 120-150 rpm; and obtaining the epoxy resin part of the epoxy resin-acid anhydride system for vacuum infusion of the wind power blade.
Packaging the obtained epoxy resin part with ton barrel, sealing, and storing at 2-43 deg.C.
b) Preparing a curing agent intermediate material: under the condition of stirring speed of 100-300rpm, slowly adding polyether polyol into anhydride according to the weight part ratio of 1:3, stirring and heating, controlling the temperature to be less than or equal to 130 ℃, stirring and dispersing for 45-60 minutes, and cooling to room temperature to obtain the curing agent intermediate material.
Preparation of the curing agent part:
pouring the residual anhydride into a container, adding a curing agent intermediate into the container, adding an imidazole modified accelerator and a defoaming agent, and continuously stirring for 45-60min at a stirring speed of 120-150 rpm; and obtaining the curing agent part of the epoxy resin-anhydride system for vacuum infusion of the wind power blade.
Packaging the obtained curing agent part with a ton bucket, sealing and storing at 2-43 deg.C.
Example two
The embodiment provides an epoxy resin-anhydride system for vacuum infusion of a wind power blade, which comprises the following components in parts by weight:
resin matrix part A:
b curing agent moiety
The preparation method of the epoxy resin-anhydride system for the vacuum infusion wind power blade comprises the following steps:
preparing the components in parts by weight;
a) preparing a resin matrix intermediate material: under the condition of stirring speed of 100-300rpm, slowly adding the carboxyl-terminated butadiene-acrylonitrile rubber into E51 epoxy resin according to the weight part ratio of 1:3, stirring and heating, controlling the temperature to be less than or equal to 90 ℃, stirring and dispersing for 45-60 minutes until the carboxyl-terminated butadiene-acrylonitrile rubber is completely and uniformly dispersed, and cooling the temperature to room temperature to obtain the resin matrix intermediate material.
Preparation of the epoxy resin part:
heating the rest E51 epoxy resin to 60-70 ℃, adding the resin matrix intermediate, adding butyl glycidyl ether diluent, silane coupling agent and defoaming agent, and continuously stirring for 45-60min at the stirring speed of 120-150 rpm; and obtaining the epoxy resin part of the epoxy resin-acid anhydride system for vacuum infusion of the wind power blade.
Packaging the obtained epoxy resin part with ton barrel, sealing, and storing at 2-43 deg.C.
b) Preparation of the curing agent part:
pouring anhydride into a container, adding an organic carboxylic acid complex, adding a tertiary amine accelerator and a defoaming agent, and continuously stirring for 45-60min at the stirring speed of 120-150 rpm; and obtaining the curing agent part of the epoxy resin-anhydride system for vacuum infusion of the wind power blade.
Packaging the obtained curing agent part with a ton bucket, sealing and storing at 2-43 deg.C.
EXAMPLE III
The embodiment provides an epoxy resin-acid anhydride system for vacuum infusion of wind power blades, which comprises the following components in parts by weight:
resin matrix part A:
b curing agent moiety
The preparation method of the epoxy resin-acid anhydride system for the vacuum infusion wind power blade comprises the following steps:
preparing the components in parts by weight;
a) preparation of the epoxy resin part:
heating E51 epoxy resin to 60-70 ℃, adding butanediol diglycidyl ether diluent, silane coupling agent and defoaming agent, and continuously stirring for 45-60min at the stirring speed of 120-150 rpm; and obtaining the epoxy resin part of the epoxy resin-acid anhydride system for vacuum infusion of the wind power blade.
Packaging the obtained epoxy resin part with ton barrel, sealing, and storing at 2-43 deg.C.
b) Preparation of the curing agent part:
pouring anhydride into a container, adding the hydroxyl-terminated nitrile rubber into the container, adding the modified imidazole accelerator and the defoaming agent, and continuously stirring for 45-60min at the stirring speed of 120-150 rpm; and obtaining the curing agent part of the epoxy resin-anhydride system for vacuum infusion of the wind power blade.
Packaging the obtained curing agent part with a ton bucket, sealing and storing at 2-43 deg.C.
Comparative example 1
The comparative example provides an epoxy resin-amine curing agent system for vacuum infusion of wind power blades, which comprises the following components in parts by weight:
resin matrix part A:
b curing agent moiety
Polyetheramine curing agent 50
Alicyclic amine curing agent 50
Tertiary amine, accelerator 0.5
The preparation method of the epoxy resin-amine curing agent system for the vacuum infusion wind power blade comprises the following steps:
preparing the components in parts by weight;
a) preparation of the epoxy resin part:
heating the E51 epoxy resin to 60-70 ℃, adding a butanediol diglycidyl ether diluent, a silane coupling agent and an antifoaming agent, and continuously stirring for 45-60min at the stirring speed of 120-150 rpm; and obtaining the epoxy resin part of the epoxy resin-acid anhydride system for vacuum infusion of the wind power blade.
Packaging the obtained epoxy resin part with ton barrel, sealing, and storing at 2-43 deg.C.
b) Preparation of the curing agent part:
pouring the polyether amine into a container, adding alicyclic amine into the container, adding a tertiary amine accelerator, and continuously stirring for 45-60min at the stirring speed of 120-150 rpm; and obtaining the curing agent part of the epoxy resin-amine curing agent system for vacuum infusion of the wind power blade.
Packaging the obtained curing agent part with a ton bucket, sealing and storing at 2-43 deg.C.
Test example-physical Properties of epoxy resin-acid anhydride System for vacuum infusion of wind turbine blades
The performance test of the epoxy resin-anhydride system for vacuum infusion wind power blades obtained in the first embodiment, the second embodiment and the third embodiment of the present invention and the epoxy resin-amine curing agent system for vacuum infusion wind power blades obtained in the first embodiment of the present invention shows that the epoxy resin-anhydride system for vacuum infusion wind power blades obtained in the present invention has more excellent physical properties, which are specifically shown in the following table 1:
table 1: physical property test of epoxy resin-anhydride system for vacuum infusion of wind power blade and epoxy resin-amine curing agent system for vacuum infusion of wind power blade
The epoxy resin-anhydride system for vacuum infusion wind turbine blades disclosed by the embodiment of the invention and the preparation method and application thereof are described in detail, a specific example is applied in the detailed description to explain the principle and the implementation mode of the invention, and the description of the embodiment is only used for helping to understand the method and the core idea of the invention; meanwhile, for a person skilled in the art, according to the idea of the present invention, there may be variations in the specific embodiments and the application scope, and in summary, the content of the present specification should not be construed as a limitation to the present invention.
Claims (10)
1. An epoxy resin-anhydride system for vacuum infusion of wind power blades is characterized by comprising the following components in parts by weight:
resin matrix part A:
b curing agent moiety
2. The epoxy resin-anhydride system for vacuum infusion of wind blades according to claim 1, wherein: the liquid epoxy resin comprises one or more of glycidyl ethers (including but not limited to bisphenol A type liquid epoxy resin, bisphenol F type epoxy resin and liquid novolac epoxy resin), glycidyl esters, glycidyl amines, alicyclic epoxy resin, epoxidized olefins or hydantoin epoxy resin.
3. The epoxy resin-anhydride system for vacuum infusion of wind blades according to claim 1, wherein: the solid epoxy resin comprises one or more of bisphenol A type solid epoxy resin, solid phenolic epoxy resin or o-cresol formaldehyde epoxy resin.
4. The epoxy resin-anhydride system for vacuum infusion of wind blades according to claim 1, wherein: the toughening agent comprises one or more of polyalcohol, hydroxyl-terminated polymer, rubber elastomer, thermoplastic resin, core-shell polymer, dimer acid modified epoxy resin, isocyanate modified epoxy resin or hyperbranched polymer.
5. The epoxy resin-anhydride system for vacuum infusion of wind blades according to claim 1, wherein: the acid anhydride comprises one or a mixture of more of aromatic acid anhydride, alicyclic acid anhydride, aliphatic acid anhydride and halogen-containing acid anhydride.
6. The epoxy resin-anhydride system for vacuum infusion of wind blades according to claim 1, wherein: the accelerator comprises one or a mixture of more of tertiary amine and salt thereof, acetylacetone metal salt, organic carboxylate and complex thereof, quaternary ammonium salt, quaternary phosphonium compound, imidazole or modified imidazole.
7. The epoxy resin-anhydride system for vacuum infusion of wind blades according to claim 1, wherein: the auxiliary agent comprises several or a mixture of several of a coupling agent, a defoaming agent and a wetting agent.
8. The preparation method of the epoxy resin-anhydride system for the vacuum infusion wind turbine blade according to any one of claims 1 to 7, characterized by comprising the following steps:
preparing a resin matrix intermediate material: adding the solid epoxy resin into the liquid epoxy resin according to the weight part ratio of 1-3:1-3, fully dissolving the solid epoxy resin at the temperature of 100-130 ℃, uniformly stirring, and reducing the temperature to room temperature to obtain a resin matrix intermediate material;
preparing an anhydride curing agent intermediate material: adding the anhydride into the polyalcohol and the hydroxyl-terminated polymer according to the weight part ratio of 1-3:1-3, fully and uniformly stirring the anhydride at the temperature of 100-130 ℃, and then reducing the temperature to room temperature to obtain an anhydride curing agent intermediate material;
preparing the epoxy resin-anhydride system for the vacuum infusion wind power blade: mixing the solid-liquid epoxy resin, the epoxy diluent and the toughening agent in parts by weight, adding the auxiliary agent and the resin matrix intermediate material in parts by weight, and stirring in vacuum to obtain an epoxy resin matrix part of the epoxy resin-anhydride system;
preparing the epoxy resin-anhydride system for the vacuum infusion wind power blade: mixing the anhydride, the toughening agent and the accelerator according to parts by weight, adding the auxiliary and the anhydride curing agent matrix intermediate material according to parts by weight, and stirring in vacuum to obtain a curing agent part of the epoxy resin-anhydride system;
preparing the epoxy resin-anhydride system for the vacuum infusion wind power blade: the epoxy resin matrix part and the curing agent part are automatically and uniformly mixed in proportion through a glue mixer to obtain an epoxy resin-anhydride system for vacuum infusion of the wind power blade, wherein the proportion of the epoxy resin matrix part to the curing agent part is 100: 90-120 ℃, and the temperature of the feed liquid is 25-40 ℃.
9. The method of claim 8, wherein: the step of preparing the resin matrix intermediate material is specifically that under the condition that the stirring speed is 100-300rpm, the liquid epoxy resin is added into the solid epoxy resin, the solid epoxy resin is stirred and heated, the temperature is controlled to be less than or equal to 150 ℃, after the liquid epoxy resin is completely added, the solid epoxy resin is stirred for 40-60 minutes, and then the temperature is reduced to 20-30 ℃ to obtain the resin matrix intermediate material;
the step of preparing the intermediate material of the anhydride curing agent is specifically that the polyalcohol and the hydroxyl-terminated polymer are added into the anhydride under the condition that the stirring speed is 100-300rpm, the mixture is stirred and heated, the temperature is controlled to be less than or equal to 130 ℃, after the polyalcohol and the hydroxyl-terminated polymer are all added, the mixture is stirred for 40-60 minutes, and then the temperature is reduced to 20-30 ℃ to obtain the intermediate material of the anhydride curing agent.
10. The preparation method according to claim 8, wherein the step of preparing the epoxy resin-anhydride system for vacuum infusion of the wind turbine blade specifically comprises:
a) epoxy resin matrix part: if no solid resin is used, heating the liquid epoxy resin to 50-80 ℃, adding the epoxy diluent, the toughening agent and the auxiliary agent into the liquid epoxy resin, keeping the stirring speed of 120-150rpm, and stirring for 30-45min to obtain the epoxy resin matrix part of the epoxy resin-anhydride system for the vacuum infusion wind power blade;
if solid resin is used, firstly, heating the liquid epoxy resin to 95-105 ℃, adding the solid epoxy resin into the liquid epoxy resin, continuously heating to 120-;
secondly, reducing the heating temperature to 70-75 ℃, adding the epoxy diluent, the toughening agent and the auxiliary agent, and continuing stirring for 15-30min at the stirring speed of 120-150 rpm;
finally, reducing the heating temperature to 20-35 ℃ to obtain an epoxy resin matrix part of the epoxy resin-anhydride system for the vacuum infusion wind power blade;
b) curing agent part: if the anhydride curing agent intermediate is not used, adding the toughening agent, the accelerator and the auxiliary agent into the anhydride, keeping the stirring speed of 120-150rpm, and stirring for 30-45min to obtain the curing agent part of the epoxy resin-anhydride system for the vacuum infusion wind power blade;
if an anhydride curing agent intermediate is used, firstly heating the toughening agent polyalcohol and the hydroxyl-terminated polymer to 95-105 ℃, adding the solid or liquid anhydride, continuously heating to 110-130 ℃, keeping the constant temperature for 2-3h, and keeping the stirring speed of 120-150rpm to fully dissolve the solid anhydride, cooling to room temperature for later use (or cooling to 30-40 ℃, adding the anhydride, the toughening agent, the accelerator and the auxiliary agent, and continuously stirring uniformly to obtain the curing agent part), thereby obtaining the anhydride curing agent intermediate;
and secondly, reducing the temperature of the anhydride curing agent intermediate to 30-40 ℃, adding the anhydride, the toughening agent, the accelerator and the auxiliary agent, keeping the stirring speed of 120-150rpm, and stirring for 30-45min to obtain the curing agent part of the epoxy resin-anhydride system for the vacuum-infused wind power blade.
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| CN116515253A (en) * | 2023-06-28 | 2023-08-01 | 北京玻钢院复合材料有限公司 | Epoxy resin curing agent, epoxy resin composition, glass fiber reinforced plastic pavement panel and preparation method thereof |
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| CN102040802A (en) * | 2010-10-14 | 2011-05-04 | 天津联美化学工业有限公司 | Epoxy resin system and application thereof |
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