CN101851481B - Epoxy resin adhesive for manufacturing blades of wind driven generator and preparation method thereof - Google Patents
Epoxy resin adhesive for manufacturing blades of wind driven generator and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an epoxy resin adhesive for manufacturing blades of a wind driven generator and a preparation method thereof. The epoxy resin adhesive is prepared by combining a resin part and a curing agent part, wherein the resin part comprises epoxy resin, a dilutent, filler, a thixotropic agent and an auxiliary agent; the curing agent part comprises an amine curing agent, filler and a thixotropic agent; and the filler comprises a powdery filler part and a fibrous filler part. The epoxy resin adhesive prepared by using the general epoxy resin has high strength, particularly further improves the strength of materials by adding the fibrous filler, improves the anti-cracking performance of the materials, meets the special requirements of the blades of wind driven generators with megawatt or more on the materials and has low material cost and high economy.
Description
Technical field:
The present invention relates to a kind of preparation method of epoxyn and this tackiness agent for the manufacture of blade of wind-driven generator, it is particularly suitable for making blade of MW class wind turbine.
Background technology:
Wind-power electricity generation is pollution-free power-generating, is the clean energy that is full of vitality, and the high speed development of wind-powered electricity generation has become inexorable trend.The major equipment that wind-power electricity generation relies on is wind power generating set, the parts that aerogenerator is most important, the most expensive are impeller, single impeller accounts for 20% of whole aerogenerator cost, the key of impeller then is blade, and the quality of blade directly affects efficient, life-span and the performance of wind power generating set.What the blade of aerogenerator mainly adopted is matrix material, the above blade of wind-driven generator of MW class especially, and the blade of matrix material is supporting to be the critical material that blade of wind-driven generator prepares with epoxyn.
Epoxyn is since beginning to use the 1950's, and development is very fast, be performance comparatively comprehensively, use a quite widely class tackiness agent.Although China's epoxyn has developed for many years, be widely used in the industries such as electronics, potting, food, but still shortage high-end product, especially for the epoxyn of making blade of wind-driven generator, this is wherein especially supporting more outstanding with epoxyn with the blade of wind-driven generator more than the MW class.For a long time, produce the epoxyn of blade of wind-driven generator always by relevant major company monopolization abroad, its prescription and preparation technology externally maintain secrecy, so that China blade of wind-driven generator manufacturing concern has to rely on these major companies, the cost fancy price is from these major company's import epoxyns.Yet the import epoxyn is except price is high, and supply chain also quite is critical, and this has affected normal production and the profit level of China blade manufacturing concern to a great extent, thereby seriously restricts and affect the development of China's wind-powered electricity generation industry.In order to strengthen the manufacturing capacity of China's blade of wind-driven generator, promote fast the paces that China's wind-powered electricity generation cause is advanced, realize that the supporting production domesticization with epoxyn of blade of MW class wind turbine is extremely urgent.
In recent years, China is also at exploitation wind electricity blade epoxyn, mainly is conceived to solve the problem that the conventional epoxies tackiness agent exists at snappiness and anti-cracking performance.Chinese patent literature disclosed " a kind of wind-power class bi-component epoxy adhesive and preparation method thereof " (publication number: CN101550325A for example, on October 7th, 2009) and " a kind of modified epoxy and preparation method for structural adhesive of wind generating blades " (publication number: CN101525439A open day:, open day: on September 9th, 2009), they all are that (CN101550325A has introduced the vinylformic acid chain by introduce flexible segment in the Resins, epoxy molecule, CN101525439A has introduced polyurethane chain), to improve the snappiness of epoxyn, prevent the material cracking.But their problem is:
1. blade of wind-driven generator generally is to be made of upper half-shell, housing lower half and shear beam three parts, sticks with glue agent and makes their mutual bonding one-tenth as a whole.Blade of wind-driven generator is in operational process, and tack coat is subject to the effect of shearing force, peeling force etc., needs adhesive material to have higher intensity.In addition, tackiness agent also needs to exert all one's strength and effectively transmits between upper and lower half housing and shear beam, therefore needs adhesive material to have higher modulus.Blade is longer, and just larger to the strength and modulus requirement of adhesive material, the Megawatt fan blade generally all surpasses 30 meters, weighs several tons, and is high especially to the strength and modulus requirement of tackiness agent.CN101550325A has introduced the vinylformic acid chain in molecular resin, CN101525439A has introduced polyurethane chain in molecular resin, this can cause the decline of the strength of materials and modulus, do not reach the technical requirements of the above blade of wind-driven generator of MW class, can only little for the manufacture of size, lightweight small-sized wind power generator blade.
2. loaded down with trivial details to the technique of epoxy resin modification with vinylformic acid or urethane, plant investment is large, and preparation cycle is long, and the tackiness agent cost that makes is high, and is less economical.
Summary of the invention:
The purpose of this invention is to provide a kind of epoxyn for the manufacture of blade of wind-driven generator, especially for the epoxyn of making the above blade of wind-driven generator of MW class, and the preparation method of this epoxyn.
The objective of the invention is to adopt following technical proposals to realize:
A kind of epoxyn for the manufacture of blade of wind-driven generator, this epoxyn is combined by resin part and curing agent part, and described resin portion is divided and is comprised: Resins, epoxy, thinner, filler, thixotropic agent and auxiliary agent; Described curing agent part comprises amine curing agent, filler and thixotropic agent; Described filler comprises pulverulent filler and bat wool two portions.
The proportioning raw materials of described resin part is calculated by following weight ratio:
30～70 parts of Resins, epoxy
2～15 parts of thinners
10～45 parts of pulverulent filler
5～30 parts of bat wools
1～8 part of thixotropic agent
0～8 part of auxiliary agent
The proportioning raw materials of described curing agent part is calculated by following weight ratio:
35～65 parts of amine curing agents
10～45 parts of pulverulent filler
8～30 parts of bat wools
1～8 part of thixotropic agent
Described tackiness agent is that resin part and curing agent part are mixed, and its blending ratio is pressed following listed as parts by weight:
100 parts of resin parts
40～50 parts of curing agent part
Described bat wool is one or several the mixture in glass fibre, carbon fiber, aramid fiber, vinylon fibre, polyvinyl alcohol fiber, mullite fiber, basalt fibre, the Stainless Steel Fibre.
The length of described bat wool is 100～1000 microns.
Described pulverulent filler is one or several the mixture in nano silicon, nano titanium oxide, nano aluminium oxide, nanofiber wollastonite powder, nano-calcium carbonate, calcium carbonate crystal whisker, the ZnOw.
Described Resins, epoxy is one or several the mixture in bisphenol A type epoxy resin E-51, bisphenol A type epoxy resin E-44, bisphenol A type epoxy resin E-20, the bisphenol f type epoxy resin.
Described thinner is one or several the mixture in propylene oxide methyl ether, phenyl glycidyl ether, butanediol diglycidyl ether, glycidyl allyl ether, n-butyl glycidyl ether, glycidyl methacrylate, polypropylene glycol diglycidyl ether and the hexanediol diglycidyl ether.
Described amine curing agent is one or several the mixture in fat amine compound, aliphatic cyclic amine compounds and the aromatic amines compound.
Described amine curing agent is one or several the mixture in quadrol, hexanediamine, diethylenetriamine, triethylene tetramine, tetraethylene pentamine, diethylenetriamine-acrylonitrile copolymer, polyetheramine, mphenylenediamine, diaminodiphenyl-methane, isophorone diamine and the polymeric amide.
Described thixotropic agent is one or both the mixture in aerosil, the organobentonite.
Described auxiliary agent is toughner and/or coupling agent, and wherein, toughner is one or several the mixture in carboxyl end of the liquid acrylonitrile-butadiene rubber, hydroxyl terminated butyl nitrile (HTBN) rubber and the epoxy terminated liquid acrylonitrile butadiene rubber; Coupling agent is silane coupling agent.
The preparation method of above-mentioned used for blades of wind driven generator epoxyn may further comprise the steps:
(1) prepares respectively raw material by the formula ratio of resin part and curing agent part; Prepare mixing equipment;
(2) resin part and curing agent part are prepared respectively;
1. resin part
A. the component with the resin part joins in the mixing equipment, is fully mixed to evenly;
B. vacuumize the air pocket of eliminating in the compound, leave standstill;
C. the resin that mixes partly is expressed in the product bucket sealing, lucifuge, room temperature preservation;
2. curing agent part
A. curing agent part is joined in the mixing equipment, be fully mixed to evenly;
B. vacuumize the air pocket of eliminating in the compound, leave standstill;
C. the solidifying agent component that mixes is expressed in the product bucket sealing, lucifuge, room temperature preservation;
(3) preparation epoxyn
During use resin part and curing agent part are mixed by proportioning, get final product.
The invention has the beneficial effects as follows:
The resin part of main material adopts the universal epoxy resin, bisphenol A type epoxy resin for example, and its structural formula is:
Compared with prior art, after adding solidifying agent, easier ring-opening polymerization forms closely spacial framework, therefore has higher strength and modulus, by adding bat wool, further improved the strength and modulus of material, and improved the anti-cracking performance of material, satisfied the particular requirement of the above blade of wind-driven generator of MW class to material, and the cost of material is low, preparation technology is simple, good economy performance.
The below is the performance data of the test of this tackiness agent:
Performance comparison before and after table 1 bat wool is introduced
Annotate: condition of cure is room temperature 24h+70 ℃/8h.
From table 1, can learn, the present invention is by the introducing of bat wool, body tensile strength, body tensile modulus, shearing resistance and the stripping strength of tackiness agent have effectively been improved, also improved anti-cracking behavior and the fatigue performance of tackiness agent, prepared epoxyn comprehensive technical performance is superior.
The present invention compares with CN101525439A with CN101550325A: by the introducing of bat wool, overcome the defective on technique, cost and the performance of bringing by the method for in the Resins, epoxy molecule, introducing soft segment, the epoxyn of preparation has superior intensity, modulus, anti-cracking performance, more can be suitable for making the above blade of wind-driven generator of MW class, and raw material obtains easily, prepares simple, cheap.
The present invention has broken for a long time abroad to producing the monopolization of used for blades of wind driven generator epoxyn, cheap, finish China blade of wind-driven generator manufacturing concern to the dependence of external major company, thereby can promote fast the paces that China's wind-powered electricity generation cause is advanced.
Embodiment:
Epoxyn of the present invention comprises resin part and curing agent part, and two portions prepare respectively.
Embodiment one:
The raw material of resin part: bisphenol A type epoxy resin E-51-55 part; 1,6-hexanediol diglycidyl ether-6 part, glycidyl allyl ether-2 part, glycidyl methacrylate-2 part; Nano-calcium carbonate-20 part; Vinylon fibre-6 part, staple length is 300 microns; Epoxy terminated liquid acrylonitrile butadiene rubber-3 part, silane coupling agent KH560-1 part; Organobentonite-5 part.
The raw material of curing agent part: polyetheramine D230-45 part; Nano-calcium carbonate-28 part; Vinylon fibre-8 part, staple length is 300 microns; Organobentonite-4 part.
The nano-calcium carbonate calcium powder plays a part to fill and anti-settling, and vinylon fibre mainly plays a part to strengthen, prevents the adhesive matrix cracking, also plays filling effect simultaneously.
The preparation method:
Prepare mixing equipment, two portions material resin, solidifying agent are prepared respectively, above-mentioned resin raw material is partly joined in the mixing equipment, be fully mixed to evenly; Vacuumize the bubble of eliminating in the compound, leave standstill; The resin that mixes partly is expressed in the product bucket of resin part, seals lucifuge, room temperature preservation.The raw material of above-mentioned curing agent part is joined in the mixing equipment, be fully mixed to evenly; Vacuumize the air pocket of eliminating in the compound, leave standstill; The curing agent part that mixes is expressed in the solidifying agent product bucket, seals, lucifuge, room temperature preservation.In use, resin part and curing agent part are mixed by 100: 40～50 weight part, get final product.
The present invention has improved intensity, modulus, toughness and the anti-cracking performance of adhesive material effectively by the introducing of bat wool.
Embodiment two:
The raw material of resin part: bisphenol A type epoxy resin E-51-35 part, bisphenol f type epoxy resin-15 part; Polypropylene glycol diglycidyl ether-3.5 part, propylene oxide methyl ether-2 part; Calcium carbonate crystal whisker-13 part, nanofiber wollastonite powder-10 part; Glass fibre-10 part, staple length is 350 microns; Carboxyl end of the liquid acrylonitrile-butadiene rubber-4 part, silane coupling agent KH560-1.5 part; Aerosil-6 part.
The raw material of curing agent part: polyetheramine D230-40 part, isophorone diamine-10 part, tetraethylene pentamine-3 part; Calcium carbonate crystal whisker-27 part; Glass fibre-10 part, staple length is 350 microns; Aerosil-5 part.
The preparation method is identical with embodiment 1.
Embodiment three
The raw material of resin part: bisphenol f type epoxy resin standard type-32 part; Butanediol diglycidyl ether-3 part; Nano silicon-10 part; Carbon fiber-8 part, staple length is 180 microns; Aerosil-3 part.
The raw material of curing agent part: polymeric amide D230-40 part; Nano silicon-8 part, ZnOw-2 part; Carbon fiber-20 part, staple length is 180 microns; Aerosil-2 part.
The preparation method is identical with embodiment 1.
Embodiment four:
The raw material of resin part: bisphenol A type epoxy resin E-51-30 part, bisphenol f type epoxy resin standard type-16 part; Hexanediol diglycidyl ether-4 part, phenyl glycidyl ether-5 part, propylene oxide methyl ether-5 part; Carboxyl end of the liquid acrylonitrile-butadiene rubber-4 part, hydroxyl terminated butyl nitrile (HTBN) rubber-4 part; Nano titanium oxide-39 part; Stainless Steel Fibre-28 part, staple length is 400 microns; Organobentonite-2 part.
The raw material of curing agent part: polymeric amide-45 part; Nano titanium oxide-25 part; Stainless Steel Fibre-16 part, staple length is 400 microns; Organobentonite-7 part.
The preparation method is identical with embodiment 1.
Embodiment five:
The raw material of resin part: type bisphenol A epoxide resin E-20-30 part, bisphenol f type epoxy resin standard type-20 part; N-butyl glycidyl ether-5 part, phenyl glycidyl ether-5 part; Carboxyl end of the liquid acrylonitrile-butadiene rubber-2 part, hydroxyl terminated butyl nitrile (HTBN) rubber-2 part, epoxy terminated liquid acrylonitrile butadiene rubber-2 part, silane coupling agent KH560-2 part; Mullite fiber-20 part, basalt fibre-5 part, staple length is 120 microns; Calcium carbonate crystal whisker-20 part; Organobentonite-2 part.
The raw material of curing agent part: polyetheramine D230-27 part, quadrol-3 part, diaminodiphenyl-methane-2.5 part, hexanediamine-5 part; Mullite fiber-30 part, staple length is 120 microns; Calcium carbonate crystal whisker-32 part; Aerosil-5.5 part.
The preparation method is identical with embodiment 1.
Embodiment six:
The raw material of resin part: bisphenol A type epoxy resin E-51-68 part; Hexanediol diglycidyl ether-4 part; Nano titanium oxide-3 part, nano aluminium oxide-7 part; Carbon fiber-13 part, aramid fiber-3 part, staple length is 900 microns; Carboxyl end of the liquid acrylonitrile-butadiene rubber-0.5 part, hydroxyl terminated butyl nitrile (HTBN) rubber-0.5 part; Aerosil-4 part.
The raw material of curing agent part: polyetheramine D230-35 part, diethylenetriamine-acrylonitrile copolymer-5 part; Carbon fiber-8 part, staple length is 900 microns; Nano aluminium oxide-15 part; Organobentonite-3 part.
The preparation method is identical with embodiment 1.
Embodiment seven:
The raw material of resin part: bisphenol A type epoxy resin E-51-20 part, bisphenol f type epoxy resin-15 part; 1,6-hexanediol diglycidyl ether-4 part; Nano-calcium carbonate-20 part; Vinylon fibre-25 part, staple length is 200 microns; Organobentonite-1 part.
The raw material of curing agent part: polyetheramine D230-45 part, triethylene tetramine-5 part, polymeric amide-10 part; Nano-calcium carbonate-45 part; Vinylon fibre-12 part, staple length is 200 microns; Organobentonite-2 part.
The preparation method is identical with embodiment 1.
Embodiment eight:
The raw material of resin part: bisphenol f type epoxy resin-30 part; Polypropylene glycol diglycidyl ether-3.5 part; Calcium carbonate crystal whisker-13 part, nanofiber wollastonite powder-2 part; Glass fibre-15 part, staple length is 750 microns; Carboxyl end of the liquid acrylonitrile-butadiene rubber-3 part, silane coupling agent KH560-1.5 part; Aerosil-4 part.
The raw material of curing agent part: polyetheramine D230-38 part; Calcium carbonate crystal whisker-30 part, nanofiber wollastonite powder-8 part; Glass fibre-12 part, staple length is 750 microns; Aerosil-3 part.
The preparation method is identical with embodiment 1.
Embodiment nine:
The raw material of resin part: bisphenol A type epoxy resin E-51-30 part; Phenyl glycidyl ether-3 part; Carboxyl end of the liquid acrylonitrile-butadiene rubber-0.5 part, hydroxyl terminated butyl nitrile (HTBN) rubber-1 part; Nano titanium oxide-10 part; Stainless Steel Fibre-13 part, staple length is 600 microns; Organobentonite-3.5 part.
The raw material of curing agent part: polyetheramine D230-35 part; Nano titanium oxide-20 part; Stainless Steel Fibre-22 part, 600 microns of staple lengths; Organobentonite-3.5 part.
The preparation method is identical with embodiment 1.
Embodiment ten:
The raw material of resin part: bisphenol A type epoxy resin E-51-19 part, bisphenol f type epoxy resin standard type-19 part; N-butyl glycidyl ether-3.5 part; Carboxyl end of the liquid acrylonitrile-butadiene rubber-2 part; Polyvinyl alcohol fiber-20 part, basalt fibre-5 part, staple length is 550 microns; Calcium carbonate crystal whisker-20 part; Organobentonite-1.5 part.
The raw material of curing agent part: polyetheramine D23030 part, diaminodiphenyl-methane-7 part; Polyvinyl alcohol fiber-30 part, staple length is 550 microns; Calcium carbonate crystal whisker-26 part; Aerosil-7 part.
The preparation method is identical with embodiment 1.
Embodiment 11:
The raw material of resin part: bisphenol A type epoxy resin E-51-43 part; Hexanediol diglycidyl ether-6 part; Nano titanium oxide-3 part, nano aluminium oxide-15 part; Carbon fiber-3 part, aramid fiber-4 part, staple length is 450 microns; Carboxyl end of the liquid acrylonitrile-butadiene rubber-0.5 part, hydroxyl terminated butyl nitrile (HTBN) rubber-0.5 part; Aerosil-2 part.
The raw material of curing agent part: polyetheramine-30 part, diethylenetriamine-acrylonitrile copolymer-5 part; Aramid fiber-9 part, staple length is 450 microns; Nano aluminium oxide-15 part; Organobentonite-6 part.
The preparation method is identical with embodiment 1.
Embodiment 12:
The raw material of resin part: bisphenol A-type diglycidylether E-44-35 part, bisphenol f type epoxy resin standard type-22 part; Butanediol diglycidyl ether-5 part; Nano silicon-10 part, ZnOw-10 part; Carbon fiber-10 part, staple length is 1000 microns; Silane coupling agent KH550-1 part, epoxy terminated liquid acrylonitrile butadiene rubber-4 part; Aerosil-3 part.
The raw material of curing agent part: polyetheramine D230-40 part, isophorone diamine-10 part; Nano silicon-10 part, ZnOw-10 part; Carbon fiber-27 part, staple length is 1000 microns; Aerosil-3 part.
The preparation method is identical with embodiment 1.
The prescription of the various embodiments described above is weight part, and staple length refers to mean length.
This material also can be used for making the blade of wind-driven generator of small dimension in other.
Claims (5)
1. epoxyn for the manufacture of blade of wind-driven generator, this epoxyn is combined by resin part and curing agent part, and described resin portion is divided and is comprised: Resins, epoxy, thinner, filler, thixotropic agent and auxiliary agent; Described curing agent part comprises amine curing agent, filler and thixotropic agent; It is characterized in that described filler comprises pulverulent filler and bat wool two portions; The proportioning raw materials of described resin part is calculated by following weight ratio:
The proportioning raw materials of described curing agent part is calculated by following weight ratio:
Described tackiness agent is that resin part and curing agent part are mixed, and its blending ratio is pressed following listed as parts by weight:
100 parts of resin parts
40～50 parts of curing agent part
Described Resins, epoxy is a kind of in bisphenol A type epoxy resin, the bisphenol f type epoxy resin or their mixture;
Described pulverulent filler is one or several the mixture in nano silicon, nano titanium oxide, nano aluminium oxide, nano-calcium carbonate, calcium carbonate crystal whisker, the ZnOw;
Described bat wool is one or several the mixture in glass fibre, carbon fiber, aramid fiber, vinylon fibre, polyvinyl alcohol fiber, mullite fiber, basalt fibre, the Stainless Steel Fibre;
Described auxiliary agent is toughner and/or coupling agent, and wherein, toughner is one or several the mixture in carboxyl end of the liquid acrylonitrile-butadiene rubber, hydroxyl terminated butyl nitrile (HTBN) rubber and the epoxy terminated liquid acrylonitrile butadiene rubber; Coupling agent is silane coupling agent;
Described amine curing agent is one or several the mixture in fat amine compound, aliphatic cyclic amine compounds and the aromatic amines compound.
2. described epoxyn for the manufacture of blade of wind-driven generator according to claim 1 is characterized in that the length of described bat wool is 100～1000 microns.
3. described epoxyn for the manufacture of blade of wind-driven generator according to claim 1, it is characterized in that described thinner is one or several the mixture in propylene oxide methyl ether, phenyl glycidyl ether, butanediol diglycidyl ether, glycidyl allyl ether, n-butyl glycidyl ether, glycidyl methacrylate, polypropylene glycol diglycidyl ether and the hexanediol diglycidyl ether.
4. described epoxyn for the manufacture of blade of wind-driven generator according to claim 1, it is characterized in that described amine curing agent is one or several the mixture in quadrol, hexanediamine, diethylenetriamine, triethylene tetramine, tetraethylene pentamine, diethylenetriamine-acrylonitrile copolymer, polyetheramine, mphenylenediamine, diaminodiphenyl-methane, isophorone diamine and the polymeric amide.
5. described epoxyn for the manufacture of blade of wind-driven generator according to claim 1 is characterized in that, described thixotropic agent is one or both the mixture in aerosil, the organobentonite.
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| CN 201010186132 CN101851481B (en) | 2010-05-22 | 2010-05-22 | Epoxy resin adhesive for manufacturing blades of wind driven generator and preparation method thereof |
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