CN104194662A - Phenolphthalein polyaryletherketone modified epoxy structure adhesive film and preparation method thereof - Google Patents
Phenolphthalein polyaryletherketone modified epoxy structure adhesive film and preparation method thereof Download PDFInfo
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- CN104194662A CN104194662A CN201410491347.0A CN201410491347A CN104194662A CN 104194662 A CN104194662 A CN 104194662A CN 201410491347 A CN201410491347 A CN 201410491347A CN 104194662 A CN104194662 A CN 104194662A
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Abstract
The invention discloses a phenolphthalein polyaryletherketone modified epoxy structure adhesive film and a preparation method of the phenolphthalein polyaryletherketone modified epoxy structure adhesive film, and relates to an adhesive and a preparation method of the adhesive. The adhesive film and the preparation method of the adhesive film solve the problem that the temperature tolerance of an existing high-temperature cured epoxy structure adhesive is poor. The phenolphthalein polyaryletherketone modified epoxy structure adhesive film is prepared from a main resin, a main flexibilizer, an auxiliary flexibilizer, a curing agent and a coupling agent. The method comprises 1 weighing, 2 mixing the materials together, 3 preparing the adhesive; 4 preheating, calendaring and forming the film. The adhesive film has excellent heat resistance, damp-heat aging resistance, higher shearing strength, higher high temperature strength, and higher toughness. The method is used to prepare the phenolphthalein polyaryletherketone modified epoxy structure adhesive film, and is applied in the technical field of high polymer materials.
Description
Technical field
The present invention relates to sizing agent and preparation method thereof.
Background technology
Hot setting structural film adhesive is that a class solidification value is more than 175 DEG C, 121 DEG C of above sizing agents of use temperature, have under high strength, high-durability and hot conditions can life-time service feature, be important structural adhesive bonding material during the high temperature resistant load bearing structure part of Aeronautics and Astronautics aircraft is manufactured.The feature of this class sizing agent is that good toughness, intensity are high, but its thermotolerance is affected by toughening material and the stable on heating of Dyhard RU 100 curing system, and second-order transition temperature is 145 DEG C of left and right, and life-time service temperature is no more than 150 DEG C.In recent years, along with aerospace flight vehicle high speed development, the stable on heating requirement of epoxy construction gluing agent is improved constantly.The agent of existing epoxy construction gluing cannot meet the manufacture requirement of future aircraft high-temperature-resistant structure part.Therefore, development and existing hot setting structural adhesive intensity, tough similar temperament and to have the epoxy construction glued membrane of higher glass transition temperature significant, meet the manufacture requirement of future aircraft high-temperature-resistant structure part.
Summary of the invention
The present invention will solve the not high problem of existing hot setting epoxy construction gluing agent temperature tolerance, and a kind of phenolphthalein base polyaryletherketone modified epoxy structural film adhesive and preparation method thereof is provided.
A kind of phenolphthalein base polyaryletherketone modified epoxy structural film adhesive, is prepared from by the matrix resin of 70～100 parts, the main toughner of 20～50 parts, the auxiliary toughner of 5～15 parts, the solidifying agent of 10～20 parts and the coupling agent of 1～5 part according to mass fraction; Wherein matrix resin is by one or more mixing of pressing any ratio in bisphenol A type epoxy resin, 3～6 functionality epoxy resin and phenol aldehyde type epoxy resin.
A preparation method for phenolphthalein base polyaryletherketone modified epoxy structural film adhesive, specifically carries out according to following steps:
One, take the matrix resin of 70～100 parts, the main toughner of 20～50 parts, the auxiliary toughner of 5～15 parts, the solidifying agent of 10～20 parts and the coupling agent of 1～5 part according to mass fraction;
Two, the matrix resin taking in step 1 and main toughner are put into reactor, controlling temperature is 200 DEG C, and blend 30min～50min, obtains blending resin;
Three, the auxiliary toughner, solidifying agent and the coupling agent that in blending resin step 2 being obtained and step 1, take are put into kneader, and controlling temperature is 80 DEG C, mix 20min～40min, obtain sizing material;
Four, sizing material step 3 being obtained is under the condition of 60 DEG C～90 DEG C in temperature, preheating 20min～40min, then roller temperature be on the glued membrane rolling press of 70 DEG C～90 DEG C by carrier hot pressing film forming, obtain phenolphthalein base polyaryletherketone modified epoxy structural film adhesive.
The invention has the beneficial effects as follows: phenolphthalein base polyaryletherketone modified epoxy structural film adhesive of the present invention has good thermotolerance, wet and heat ageing resistant performance, its second-order transition temperature reaches 179.8 DEG C, 180 DEG C of thermal ageings strength degradation rate≤15% after 500 hours, 200 DEG C of thermal ageings strength degradation rate≤15% after 200 hours, strength degradation rate≤15% after hydrothermal aging 1000h under 55 DEG C, 98% humidity; There is higher shearing resistance and high temperature strength, more than normal temperature shearing resistance reaches 25MPa, more than 200 DEG C of shearing resistances reach 18MPa, more than climbing drum peel strength reaches 100Nmm/mm.
The present invention, for the preparation of phenolphthalein base polyaryletherketone modified epoxy structural film adhesive, is applied to technical field of polymer materials.
Embodiment
Technical solution of the present invention is not limited to following cited embodiment, also comprises the arbitrary combination between each embodiment.
Embodiment one: a kind of phenolphthalein base of present embodiment polyaryletherketone modified epoxy structural film adhesive, is prepared from by the matrix resin of 70～100 parts, the main toughner of 20～50 parts, the auxiliary toughner of 5～15 parts, the solidifying agent of 10～20 parts and the coupling agent of 1～5 part according to mass fraction; Wherein matrix resin is by one or more mixing of pressing any ratio in bisphenol A type epoxy resin, 3～6 functionality epoxy resin and phenol aldehyde type epoxy resin.
Embodiment two: present embodiment is different from embodiment one: this phenolphthalein base polyaryletherketone modified epoxy structural film adhesive is prepared from by the matrix resin of 75～95 parts, the main toughner of 30～45 parts, the auxiliary toughner of 8～15 parts, the solidifying agent of 13～18 parts and the coupling agent of 2～4 parts according to mass fraction.Other is identical with embodiment one.
Embodiment three: present embodiment is different from embodiment one: this phenolphthalein base polyaryletherketone modified epoxy structural film adhesive is prepared from by the matrix resin of 90 parts, the main toughner of 40 parts, the auxiliary toughner of 12 parts, the solidifying agent of 15 parts and the coupling agent of 3 parts according to mass fraction.Other is identical with embodiment one.
Embodiment four: present embodiment is different from embodiment one, two or three: main toughner is phenolphthalein base polyaryletherketone, auxiliary toughner is that one or more in core shell rubbers, solid nitrile rubber, epoxy group(ing) paracril and nbr carboxyl terminal are by the mixing of any ratio.Other is identical with embodiment one, two or three.
Embodiment five: present embodiment is different from embodiment one, two or three: solidifying agent is Dyhard RU 100 or 4,4-diaminodiphenylsulfone(DDS); Coupling agent is silane coupling agent.Other is identical with embodiment one, two or three.
Embodiment six: the preparation method of a kind of phenolphthalein base polyaryletherketone modified epoxy structural film adhesive described in embodiment one, specifically carries out according to following steps:
One, take the matrix resin of 70～100 parts, the main toughner of 20～50 parts, the auxiliary toughner of 5～15 parts, the solidifying agent of 10～20 parts and the coupling agent of 1～5 part according to mass fraction;
Two, the matrix resin taking in step 1 and main toughner are put into reactor, controlling temperature is 200 DEG C, and blend 30min～50min, obtains blending resin;
Three, the auxiliary toughner, solidifying agent and the coupling agent that in blending resin step 2 being obtained and step 1, take are put into kneader, and controlling temperature is 80 DEG C, mix 20min～40min, obtain sizing material;
Four, sizing material step 3 being obtained is under the condition of 60 DEG C～90 DEG C in temperature, preheating 20min～40min, then roller temperature be on the glued membrane rolling press of 70 DEG C～90 DEG C by carrier hot pressing film forming, obtain phenolphthalein base polyaryletherketone modified epoxy structural film adhesive.
Embodiment seven: present embodiment is different from embodiment six: blend 40min in step 2.Other is identical with embodiment six.
Embodiment eight: present embodiment is different from embodiment six: in step 4, sizing material is under the condition of 70 DEG C～80 DEG C in temperature, preheating 30min.Other is identical with embodiment six.
Embodiment nine: present embodiment is different from embodiment six: in step 4, the roller temperature of glued membrane rolling press is 75 DEG C～85 DEG C.Other is identical with embodiment six.
Embodiment ten: present embodiment is different from embodiment six: in step 4, carrier is polyester graticule cloth or nylon yarn screen cloth.Other is identical with embodiment six.
Embodiment 11: present embodiment is different from embodiment six: in step 1, main toughner is phenolphthalein base polyaryletherketone, auxiliary toughner is that one or more in core shell rubbers, solid nitrile rubber, epoxy group(ing) paracril and nbr carboxyl terminal are by the mixing of any ratio; Solidifying agent is Dyhard RU 100 or 4,4-diaminodiphenylsulfone(DDS).Other is identical with embodiment six.
Adopt following examples to verify beneficial effect of the present invention:
Embodiment mono-:
The preparation method of a kind of phenolphthalein base of the present embodiment polyaryletherketone modified epoxy structural film adhesive, specifically carries out according to following steps:
One, according to mass fraction take the bisphenol A type epoxy resin of 60 parts, 30 parts of phenol aldehyde type epoxy resins, the phenolphthalein base polyaryletherketone of 40 parts, 3 parts of epoxy group(ing) paracrils, 5 parts of core shell rubbers, 2 parts of nbr carboxyl terminals, 8 parts 4,4-diaminodiphenylsulfone(DDS), the Dyhard RU 100 of 2 parts and the silane coupling agent of 3 parts;
Two, the bisphenol A type epoxy resin taking in step 1, phenol aldehyde type epoxy resin and phenolphthalein base polyaryletherketone are put into reactor, controlling temperature is 200 DEG C, and blend 40min, obtains blending resin;
Three, the epoxy group(ing) paracril, core shell rubbers, the nbr carboxyl terminal, 4 that in blending resin step 2 being obtained and step 1, take, 4-diaminodiphenylsulfone(DDS), Dyhard RU 100 and silane coupling agent are put into kneader, controlling temperature is 80 DEG C, mixes 30min, obtains sizing material;
Four, sizing material step 3 being obtained is under the condition of 80 DEG C in temperature, preheating 30min, then roller temperature be on the glued membrane rolling press of 85 DEG C by carrier hot pressing film forming, obtain phenolphthalein base polyaryletherketone modified epoxy structural film adhesive, wherein, carrier is polyester graticule cloth.
Bisphenol A type epoxy resin in the present embodiment is bought in Xingchen Synthetic Matrials Co., Ltd., Nantong; Phenol aldehyde type epoxy resin is bought in Xingchen Synthetic Matrials Co., Ltd., Nantong; Phenolphthalein base polyaryletherketone is bought in Xuzhou engineering plastics factory; Epoxy group(ing) paracril is self-control; Core shell rubbers is bought in Mitsui; Nbr carboxyl terminal is bought in Lanzhou Petrochemical petrochemical industry research institute; 4,4-diaminodiphenylsulfone(DDS) is bought in Shanghai Nuo Tai Chemical Co., Ltd.; Dyhard RU 100 is bought in Shanxi Zhi Cheng Chemical Co., Ltd.; Silane coupling agent is bought in dawn chemical plant, Nanjing; Polyester graticule cloth is bought in top sieve silk screen Manufacturing Co., Ltd.
The phenolphthalein base polyaryletherketone modified epoxy structural film adhesive of the present embodiment has good thermotolerance, wet and heat ageing resistant performance, its second-order transition temperature reaches 179.8 DEG C, 180 DEG C of thermal ageings strength degradation rate≤15% after 500 hours, 200 DEG C of thermal ageings strength degradation rate≤15% after 200 hours, strength degradation rate≤15% after hydrothermal aging 1000h under 55 DEG C, 98% humidity.Under the condition that is 0.15～0.20mm at film thickness, according to GB7124-2008 (normal temperature shearing resistance standard) and GJB444-88 (shear at high temperature strength criterion), the shearing resistance of glued membrane adhesiveproperties is tested, shearing test piece is aluminium alloy, and phosphoric acid processing is carried out on surface.Its normal temperature shearing resistance is 33.83MPa, and 200 DEG C of shearing resistances are 21.42MPa.Therefore the phenolphthalein base polyaryletherketone modified epoxy structural film adhesive shearing resistance of the present embodiment is high, high temperature strength good.Under the condition that is 0.35～0.40mm at film thickness, according to GBT1457-2005 test, the phenolphthalein base polyaryletherketone modified epoxy structural film adhesive of the present embodiment is carried out to climbing drum peel strength test, more than climbing drum peel strength reaches 100Nmm/mm, there is higher toughness.
Claims (10)
1. a phenolphthalein base polyaryletherketone modified epoxy structural film adhesive, is characterized in that this phenolphthalein base polyaryletherketone modified epoxy structural film adhesive is prepared from by the matrix resin of 70～100 parts, the main toughner of 20～50 parts, the auxiliary toughner of 5～15 parts, the solidifying agent of 10～20 parts and the coupling agent of 1～5 part according to mass fraction; Wherein matrix resin is by one or more mixing of pressing any ratio in bisphenol A type epoxy resin, 3～6 functionality epoxy resin and phenol aldehyde type epoxy resin.
2. a kind of phenolphthalein base polyaryletherketone modified epoxy structural film adhesive according to claim 1, is characterized in that this phenolphthalein base polyaryletherketone modified epoxy structural film adhesive is prepared from by the matrix resin of 75～95 parts, the main toughner of 30～45 parts, the auxiliary toughner of 8～15 parts, the solidifying agent of 13～18 parts and the coupling agent of 2～4 parts according to mass fraction.
3. a kind of phenolphthalein base polyaryletherketone modified epoxy structural film adhesive according to claim 1, is characterized in that this phenolphthalein base polyaryletherketone modified epoxy structural film adhesive is prepared from by the matrix resin of 90 parts, the main toughner of 40 parts, the auxiliary toughner of 12 parts, the solidifying agent of 15 parts and the coupling agent of 3 parts according to mass fraction.
4. according to a kind of phenolphthalein base polyaryletherketone modified epoxy structural film adhesive described in claim 1,2 or 3, it is characterized in that main toughner is phenolphthalein base polyaryletherketone, auxiliary toughner is that one or more in core shell rubbers, solid nitrile rubber, epoxy group(ing) paracril and nbr carboxyl terminal are by the mixing of any ratio.
5. according to a kind of phenolphthalein base polyaryletherketone modified epoxy structural film adhesive described in claim 1,2 or 3, it is characterized in that solidifying agent is Dyhard RU 100 or 4,4-diaminodiphenylsulfone(DDS); Coupling agent is silane coupling agent.
6. the preparation method of a kind of phenolphthalein base polyaryletherketone modified epoxy structural film adhesive as claimed in claim 1, is characterized in that specifically carrying out according to following steps:
One, take the matrix resin of 70～100 parts, the main toughner of 20～50 parts, the auxiliary toughner of 5～15 parts, the solidifying agent of 10～20 parts and the coupling agent of 1～5 part according to mass fraction;
Two, the matrix resin taking in step 1 and main toughner are put into reactor, controlling temperature is 200 DEG C, and blend 30min～50min, obtains blending resin;
Three, the auxiliary toughner, solidifying agent and the coupling agent that in blending resin step 2 being obtained and step 1, take are put into kneader, and controlling temperature is 80 DEG C, mix 20min～40min, obtain sizing material;
Four, sizing material step 3 being obtained is under the condition of 60 DEG C～90 DEG C in temperature, preheating 20min～40min, then roller temperature be on the glued membrane rolling press of 70 DEG C～90 DEG C by carrier hot pressing film forming, obtain phenolphthalein base polyaryletherketone modified epoxy structural film adhesive.
7. the preparation method of a kind of phenolphthalein base polyaryletherketone modified epoxy structural film adhesive according to claim 6, is characterized in that blend 40min in step 2.
8. the preparation method of a kind of phenolphthalein base polyaryletherketone modified epoxy structural film adhesive according to claim 6, is characterized in that sizing material in step 4 is under the condition of 70 DEG C～80 DEG C in temperature, preheating 30min.
9. the preparation method of a kind of phenolphthalein base polyaryletherketone modified epoxy structural film adhesive according to claim 6, the roller temperature that it is characterized in that glued membrane rolling press in step 4 is 75 DEG C～85 DEG C.
10. the preparation method of a kind of phenolphthalein base polyaryletherketone modified epoxy structural film adhesive according to claim 6, is characterized in that in step 4, carrier is polyester graticule cloth or nylon yarn screen cloth.
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| CN109023966A (en) * | 2018-06-25 | 2018-12-18 | 黑龙江省科学院石油化学研究院 | A kind of wet removing cloth of hot setting epoxy group and preparation method thereof |
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| CN105237958A (en) * | 2015-11-18 | 2016-01-13 | 江西洪都航空工业集团有限责任公司 | Preparation method of high-performance epoxy resin based carbon fiber composite material |
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| CN114015371A (en) * | 2021-11-24 | 2022-02-08 | 辛格顿(常州)新材料科技有限公司 | Insulating adhesive tape |
| CN114015371B (en) * | 2021-11-24 | 2023-04-18 | 辛格顿(常州)新材料科技有限公司 | Insulating adhesive tape |
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Application publication date: 20141210 |