CN105585256A - High-performance fiberglass winding yarn sizing agent and preparation method thereof - Google Patents
High-performance fiberglass winding yarn sizing agent and preparation method thereof Download PDFInfo
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- CN105585256A CN105585256A CN201510957917.5A CN201510957917A CN105585256A CN 105585256 A CN105585256 A CN 105585256A CN 201510957917 A CN201510957917 A CN 201510957917A CN 105585256 A CN105585256 A CN 105585256A
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- Prior art keywords
- sizing agent
- epoxy resin
- glass fiber
- wound around
- performance glass
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Classifications
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C25/00—Surface treatment of fibres or filaments made from glass, minerals or slags
- C03C25/10—Coating
- C03C25/24—Coatings containing organic materials
- C03C25/26—Macromolecular compounds or prepolymers
- C03C25/32—Macromolecular compounds or prepolymers obtained otherwise than by reactions involving only carbon-to-carbon unsaturated bonds
- C03C25/36—Epoxy resins
Abstract
The invention relates to a high-performance fiberglass winding yarn sizing agent. Solid containing substances of the sizing agent account for 5%-7% of the total mass of the sizing agent, and the rest is deionized water, wherein the solid containing substances of the sizing agent comprise, by mass, 55%-80% of epoxy resin emulsion, 10%-27% of a nonionic lubricant, 5%-18% of a silane coupling agent, 0.5%-2.5% of a wetting agent and 1%-5.5% of organic acid, and the total mass of the solid containing substances is 100%. The sizing agent enables fiberglass to achieve the excellent processability and less hairness and is good in compatibility with epoxy resin, polyester resin, vinyl resin and thermosetting resin and high in interfacial strength, and a composite material has the excellent wet-state shear strength retention rate.
Description
Technical field
The present invention relates to a kind of high-performance glass fiber and be wound around roving sizing agent, belong to glass fiber infiltration agent field.
Background technology
High-performance glass fiber refers to relative simple glass fiber, has higher mechanical property, stronger corrosion resistanceEnergy, higher heat resisting temperature, good dielectric and electrical insulation capability etc., it is as the enhancing base material of high-performance composite materials,Be mainly used in the national defence fields such as Aeronautics and Astronautics, weapons, nuclear industry. High-performance glass fiber reinforced composite key technologyOne of be the size technology that determines the performances such as material technology and composite material interface.
Size is a kind of fiberglass surface treating agent, and glass fibre conventionally needs the size of use from bushing flows outProcess, give textile process performance that glass fibre is good and the mechanical property of composite excellence thereof. Different infiltrationsThe performance difference of glass fibre that agent is given, various must have good weaving and make for weaving, weave the roving of useWith performance and and substrate resin between there is good compatibility and could meet various product demand. Therefore exploitation is suitableSize for high-performance glass fiber and composite thereof is most important.
US20050279140A1 discloses a kind of winding roving sizing agent formula, and this formula film forming agent contains a kind of epoxy resinEmulsion, one or more coupling agents, a kind of cationic lubricant and a kind of acid, the epoxide equivalent of epoxy emulsion is 175-190G/eq. The glass fibre reinforced composion that this formula is produced has better mechanical property and processing characteristics.
US20090075544A1 discloses a kind of for strengthening the size formula of thermosetting resin, and this formula film forming agent containsThere are a kind of epoxy resin latex, the combination of a kind of coupling agent, a kind of non-ionic lubricant and a kind of crystallization polyalcohol, epoxy emulsionThe preferred 180-195g/eq of epoxide equivalent. The glass fibre frictional resistance that this formula is produced is little, and epoxy resin, polyester treeFat and vinylite all have good compatibility, are mainly used in and are wound around and pultrude process.
US008129018B2 discloses a kind of high-performance glass fiber size formula, and this formula comprises a kind of epoxy and becomesFilm, a kind of polyurethane finishing agent, a kind of amino and the combination of epoxy radicals coupling agent, a kind of cation and non-ionic lubricant groupClose, a kind of antistatic additive and at least one acid, the epoxide equivalent of epoxy emulsion is preferably 185-192g/eq. Use this sizeGlass fibre have good processing characteristics as braiding, its composite has good mechanical property and breaking resistance.
In above-mentioned winding roving sizing agent formula, generally only to select epoxide equivalent be the low-molecular-weight ring of 175～200g/eq to film forming agentEpoxy resins emulsion, or select the epoxy resin latex of 175～200g/eq to add the combination of 1～2 kind of water-soluble resin, only makeCannot meet processing characteristics with the epoxy resin latex of 175～200g/eq, glass precursor produces more in following process processFiloplume, and add water-soluble epoxy resin formula produce glass fiber product storage stability poor, the easy hardening of yarn, noBe beneficial to processing and the mechanical property thereof of composite. Therefore from improve glass processing characteristics and composite mechanical strength this twoAspect effect, is still necessary to develop the winding roving sizing agent formula of new high-performance glass, and glass and fluoropolymer resin are hadGood compatibility, gives composite more excellent mechanical property.
Summary of the invention
The object of the invention is to solve the deficiencies in the prior art, provide a kind of high-performance glass fiber to be wound around roving sizing agent, not onlyThe textile process performance of glass fibre can be improved, and the mechanical property of its composite can be improved.
Another object of the present invention is also to provide the preparation method of above-mentioned size.
For achieving the above object, the present invention is by the following technical solutions:
A kind of high-performance glass fiber is wound around roving sizing agent, and the thing that admittedly contains of described size accounts for 5～7% of size gross mass,All the other are deionized water, and the thing that admittedly contains of described size comprises following component: the gross mass that admittedly contains thing taking size is as 100%Meter, contains 55～80% epoxy resin latex, 10～27% non-ionic lubricant, the silane coupler of 5-18%, 0.5～2.5%Wetting agent, 1～5.5% organic acid.
Further, described size admittedly comprise following component containing thing: taking size admittedly containing the gross mass of thing as 100%,Contain 60～72% epoxy resin latex, 15～25% non-ionic lubricant, 8～14% silane coupler, 1～1.5%Wetting agent, 2～5% organic acids.
Described epoxy resin latex be low-molecular-weight liquid bisphenol A epoxy resin through surfactant emulsification preparation andBecome, epoxy resin epoxide equivalent is 180～250g/eq, preferably 210～240g/eq, the known skill that preparation method is this areaArt, dosage of surfactant is resin quality 8～20%, is preferably 10～15%. The surfactant adopting is nonionicSurfactant (providing by BASF), includes but are not limited to PLURONICP103, a kind of ethylene oxide/oxidationThe copolymer of propylene; PLURONICF77, the copolymer of ethylene oxide/propylene oxide; PLURONIC10R5, oneThe copolymer of ethylene oxide/propylene oxide; PLURONICL101, PLURONICP105 etc. Epoxy resin latex becomesFilm, the Main Function in size is for avoiding damage and give fiber and matrix in protection fiber Hou road manufacturing procedureThe compatibility that interlaminar resin is good, film forming agent also provides the caking property between monofilament in addition, increases the convergence of precursor, and raising addsWork performance reduces the generation of filoplume.
Non-ionic lubricant in size component of the present invention is as " moistening cunning " and provide fiber at winding processIn Additional Protection effect. Non-ionic lubricant can also reduce the generation of lousiness. Non-ionic lubricant of the present inventionBe selected from PEG400 monoleate, PEG600 monoleate, PEG200 monolaurate, PEG600 monostearate orThe mixture of one or more arbitrary proportions in PEG600 laurate, is preferably PEG400 monoleate.
Silane coupler of the present invention, is selected from A-1100 (gamma-aminopropyl-triethoxy-silane), A-1120 (N-β (ammoniaEthyl-γ-aminopropyltrimethoxysilane), A-187 (γ-glycidyl ether propane trimethoxy silane), A-174 (γ-(methacryloxypropyl) propyl trimethoxy silicane) or A172 (vinyl-tri-(2-methoxy ethoxy) silane) inAny one. The function of silane coupler is the cementability that is enhanced to film and glass fibre, can reduce fiber in processIn lousiness amount and broken end; Give glass surface the compatibility good with matrix resin, improve composite property.
Wetting agent of the present invention is a kind of low molecular crystalline polyalcohol, contains crystallization polyalcohol and can promote list in sizeFiber surface contacts with thermosetting resin, thereby improves the impregnability of fiber, and a small amount of crystallization polyalcohol can improve glass in additionThe cycle-index of glass fiber winding pipe. Described crystallization polyalcohol wetting agent is preferably monopentaerythritol.
Organic acid of the present invention is selected from any one in acetic acid, formic acid, butanedioic acid, boric acid or citric acid, preferably vinegarAcid or citric acid. Silane coupler will be hydrolyzed under certain pH conditions, and the consumption of acid is according to coupling agent kind used and useAmount determines. The size preparing will store and be suitable under certain pH conditions, the sour environment that general pH value is 3～7,Be preferably 3.5～5.5.
Above-mentioned high-performance glass fiber is wound around the preparation method of roving sizing agent, comprises the steps:
(1) in premixed container, add the deionized water that accounts for size total amount 40～60%, add while stirring organic acid,PH value is adjusted to 3～4, then slowly adds while stirring silane coupler, continue stirring until liquid surface clarification, obtainSilane coupler solution;
(2) epoxy resin latex is added and become owner of in mixer, add deionized water that epoxy resin latex is diluted;
(3) by lubricant with in the epoxy resin latex joining after deionized water dilution after step (2) dilution, stir allEven, obtain mixed liquor;
(4) silane coupler solution of step (1) is joined in the mixed liquor of step (3), stir, lastAdd remaining deionized water, regulate solid content, obtain size of the present invention.
Adopt high-performance glass fiber of the present invention to be wound around the glass fibre that roving sizing agent makes, its glass fiber precursor is in processBefore the processing of rear road, to pass through oven for drying, increase the convergence of precursor, can improve wear resistance. The bake out temperature of precursor is120℃，6～12h。
Compared with prior art, size recipe ingredient of the present invention is simpler, simplifies configuration preparation technology, shouldFormula is given the processing characteristics that fiber is good, with the thermosetting resin compatibility such as epoxy resin, mylar and vinyliteGood, the mechanical property of raising fibrous composite.
Detailed description of the invention
Below in conjunction with specific embodiment, further set forth the present invention. Should be understood that these embodiment are only for illustrating the present inventionBe not used in and limit the scope of the invention.
The formula of embodiment 1-5 sees the following form:
| Size component | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 |
| Epoxy resin latex | 66.29 | 66.29 | 62.29 | 61.15 | 63.84 |
| A-1100 | - | 10.19 | 0.7 | 8.34 | 8.53 |
| A-187 | 10.19 | - | 9.49 | - | - |
| A-174 | - | - | - | 3.33 | - |
| PEG-400 monoleate | 19.27 | 19.27 | 23.27 | 22.84 | 23.85 |
| Pentaerythrite | 1.19 | 1.19 | 1.19 | 1.17 | 1.22 |
| Glacial acetic acid | 3.06 | 3.06 | 3.06 | 3.17 | 2.56 |
| Size adds up to containing thing admittedly | 100 | 100 | 100 | 100 | 100 |
Note: epoxy resin latex: the epoxide equivalent of epoxy resin is 210～240g/eq, emulsifying agent in epoxy resin latexTotal consumption is weight resin 11%.
Preparation method:
(1) to the water that adds size total amount 40% in premixed container, add glacial acetic acid pH value to be adjusted to 3～4, limitStir limit and slowly add silane coupler, continue stirring until hold the clarification of liquid surface without oil bloom,, obtain silane coupler solution;
(2) in main mixer, add epoxy emulsion, then add the deionized water of 4 times of epoxy emulsion weight, stirring willEpoxy emulsion dilution;
(3) by lubricant with joining the epoxy resin latex after step (2) dilution after the dilution of its deionized water of 10 timesIn, stir, obtain mixed liquor;
(4) silane coupler solution of step (1) is joined in the mixed liquor of step (3), stir, lastAdd remaining deionized water, regulate solid content 5.0～7.0%, to obtain final product.
Performance test:
The size that embodiment 1-5 is made is applied to high-performance glass fiber and is wound around yarn, and its glass fiber precursor is after warpBefore road processing, will pass through oven for drying, the stoving process of precursor is 120 DEG C (7h), and with the high-performance glass of prior artThe size (JA that Zhongcai Sci. & Tech. Co., Ltd produces) that is wound around yarn product compares.
Test result sees the following form:
Note: the method for testing of above-mentioned test index: 1. LOI:GB/T9914.2 strengthens development test method part 2:The mensuration of glass fibre combustible content; 2. yarn breakage intensity: GB/T7690.3 reinforcing material yarn testing method3 parts: the mensuration of glass fibre ultimate strength and extension at break; 3. filoplume: statistics rove group end face lousiness quantity; 4. soakGlue yarn intensity: according to the making of ASTMD2343 woven glass roving fabric impregnation yarn sample and the mensuration of hot strength;5. NOL interlaminar shear strength: with reference to GB/T1458-2008, comparison ASTMD2344 polymeric matrix composite material andThe short beam shear test method of laminate.
From table 3, each embodiment performance data is known, and embodiment all can meet application requirements and be better than comparative example, wherein implementsExample 4 best results, are secondly embodiment 3, and embodiment 4 is with 3 compared with comparative example, and mechanical strength and interface performance enter oneStep improves.
Claims (10)
1. high-performance glass fiber is wound around a roving sizing agent, it is characterized in that, the thing that admittedly contains of described size accounts for the total matter of size5～7% of amount, all the other are deionized water, the thing that admittedly contains of described size comprises following component: the gross mass that admittedly contains thing with sizeBe 100%, contain 55～80% epoxy resin latex, 10～27% non-ionic lubricant, the silane coupler of 5-18%,0.5～2.5% wetting agent, 1～5.5% organic acid.
2. high-performance glass fiber as claimed in claim 1 is wound around roving sizing agent, it is characterized in that, consolidating of described size containsThing comprises following component: the gross mass that admittedly contains thing taking size, as 100%, contains 60～72% epoxy resin latex, 15～25%Non-ionic lubricant, 8～14% silane coupler, 1～1.5% wetting agent, 2～5% organic acids.
3. high-performance glass fiber as claimed in claim 1 is wound around roving sizing agent, it is characterized in that described epoxy resin latexBe that the emulsification of low-molecular-weight liquid bisphenol A epoxy resin process surfactant is prepared from, epoxy resin epoxide equivalent is180～250g/eq, dosage of surfactant is 8～20% of epoxy resin quality.
4. high-performance glass fiber as claimed in claim 1 is wound around roving sizing agent, it is characterized in that described non-ionic lubricantBe selected from PEG400 monoleate, PEG600 monoleate, PEG200 monolaurate, PEG600 monostearate orThe mixture of one or more arbitrary proportions in PEG600 laurate.
5. high-performance glass fiber as claimed in claim 4 is wound around roving sizing agent, it is characterized in that described non-ionic lubricantFor PEG400 monoleate.
6. high-performance glass fiber as claimed in claim 1 is wound around roving sizing agent, it is characterized in that, described silane coupler choosingFrom gamma-aminopropyl-triethoxy-silane, N-β (aminoethyl-γ-aminopropyltrimethoxysilane, γ-glycidyl ether propane threeIn methoxy silane, γ-(methacryloxypropyl) propyl trimethoxy silicane or vinyl-tri-(2-methoxy ethoxy) silaneAny one.
7. high-performance glass fiber as claimed in claim 1 is wound around roving sizing agent, it is characterized in that, described wetting agent is season pentaTetrol.
High-performance glass fiber as described in claim 1 to 7 any one be wound around roving sizing agent, it is characterized in that, described in haveMachine acid is selected from any one in acetic acid, formic acid, butanedioic acid, boric acid or citric acid.
9. high-performance glass fiber as claimed in claim 8 is wound around roving sizing agent, it is characterized in that, described organic acid is acetic acidOr citric acid.
10. the preparation method of high-performance glass fiber winding roving sizing agent described in claim 1 to 9 any one, is characterized in that,Comprise the steps:
(1) in premixed container, add the deionized water that accounts for size total amount 40～60%, add while stirring organic acid, willPH value is adjusted to 3～4, then slowly adds while stirring silane coupler, continues stirring until liquid surface clarification, obtains silane evenConnection agent solution;
(2) epoxy resin latex is added and become owner of in mixer, add deionized water that epoxy resin latex is diluted;
(3) by lubricant with in the epoxy resin latex joining after deionized water dilution after step (2) dilution, stir,Obtain mixed liquor;
(4) silane coupler solution of step (1) is joined in the mixed liquor of step (3), stir, finally addRemaining deionized water, regulates solid content, obtains size of the present invention.
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106277845A (en) * | 2016-07-15 | 2017-01-04 | 巨石集团有限公司 | Reinforced epoxy prepreg moves back treating compound for twistless roving with outer |
| CN106977115A (en) * | 2017-03-16 | 2017-07-25 | 江苏九鼎新材料股份有限公司 | One kind enhancing Weave type glass fiber infiltration agent and preparation method thereof |
| CN108751747A (en) * | 2018-07-13 | 2018-11-06 | 合肥连森裕腾新材料科技开发有限公司 | A kind of size of high performance fibre material and preparation method thereof |
| CN110240421A (en) * | 2019-07-04 | 2019-09-17 | 江苏九鼎新材料股份有限公司 | A kind of production technology of epoxy type glass fibre continuous felt |
| CN110981222A (en) * | 2019-12-12 | 2020-04-10 | 南京玻璃纤维研究设计院有限公司 | Glass fiber impregnating compound and preparation method and application thereof |
| CN112279525A (en) * | 2020-10-30 | 2021-01-29 | 重庆三磊玻纤股份有限公司 | Glass fiber impregnating compound for reinforcing polyurethane, preparation method and application thereof |
| CN112390541A (en) * | 2020-12-14 | 2021-02-23 | 南通天和树脂有限公司 | High-equivalent-weight epoxy impregnating compound and preparation method thereof |
| WO2021075109A1 (en) * | 2019-10-17 | 2021-04-22 | 日本電気硝子株式会社 | Glass direct roving production method and glass direct roving |
| CN113666647A (en) * | 2021-07-09 | 2021-11-19 | 山东玻纤集团股份有限公司 | Preparation method of high-performance direct twistless roving |
| CN114685063A (en) * | 2020-12-30 | 2022-07-01 | 宜兴市伟业玻纤材料有限公司 | Glass fiber yarn impregnating compound and preparation method and application thereof |
| CN115259880A (en) * | 2022-07-18 | 2022-11-01 | 浙江星辉新材料科技有限公司 | Preparation method of high-performance carbon fiber heat-insulating cylinder |
| CN116639890A (en) * | 2023-05-17 | 2023-08-25 | 湖北汇尔杰玄武岩纤维有限公司 | Basalt fiber post-treatment process |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106277845B (en) * | 2016-07-15 | 2019-04-19 | 巨石集团有限公司 | Reinforced epoxy prepreg moves back treating compound for twistless roving with directly outer |
| CN106277845A (en) * | 2016-07-15 | 2017-01-04 | 巨石集团有限公司 | Reinforced epoxy prepreg moves back treating compound for twistless roving with outer |
| CN106977115A (en) * | 2017-03-16 | 2017-07-25 | 江苏九鼎新材料股份有限公司 | One kind enhancing Weave type glass fiber infiltration agent and preparation method thereof |
| CN108751747A (en) * | 2018-07-13 | 2018-11-06 | 合肥连森裕腾新材料科技开发有限公司 | A kind of size of high performance fibre material and preparation method thereof |
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| WO2021075109A1 (en) * | 2019-10-17 | 2021-04-22 | 日本電気硝子株式会社 | Glass direct roving production method and glass direct roving |
| CN110981222A (en) * | 2019-12-12 | 2020-04-10 | 南京玻璃纤维研究设计院有限公司 | Glass fiber impregnating compound and preparation method and application thereof |
| CN112279525A (en) * | 2020-10-30 | 2021-01-29 | 重庆三磊玻纤股份有限公司 | Glass fiber impregnating compound for reinforcing polyurethane, preparation method and application thereof |
| CN112390541A (en) * | 2020-12-14 | 2021-02-23 | 南通天和树脂有限公司 | High-equivalent-weight epoxy impregnating compound and preparation method thereof |
| CN114685063A (en) * | 2020-12-30 | 2022-07-01 | 宜兴市伟业玻纤材料有限公司 | Glass fiber yarn impregnating compound and preparation method and application thereof |
| CN113666647A (en) * | 2021-07-09 | 2021-11-19 | 山东玻纤集团股份有限公司 | Preparation method of high-performance direct twistless roving |
| CN113666647B (en) * | 2021-07-09 | 2022-11-15 | 山东玻纤集团股份有限公司 | Preparation method of high-performance direct twistless roving |
| CN115259880A (en) * | 2022-07-18 | 2022-11-01 | 浙江星辉新材料科技有限公司 | Preparation method of high-performance carbon fiber heat-insulating cylinder |
| CN115259880B (en) * | 2022-07-18 | 2023-02-28 | 浙江星辉新材料科技有限公司 | Preparation method of high-performance carbon fiber heat-insulating cylinder |
| CN116639890A (en) * | 2023-05-17 | 2023-08-25 | 湖北汇尔杰玄武岩纤维有限公司 | Basalt fiber post-treatment process |
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