CN103159413A - Impregnating compound with carbon nano tube used for glass fiber and preparation method thereof - Google Patents
Impregnating compound with carbon nano tube used for glass fiber and preparation method thereof Download PDFInfo
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- CN103159413A CN103159413A CN201210553280XA CN201210553280A CN103159413A CN 103159413 A CN103159413 A CN 103159413A CN 201210553280X A CN201210553280X A CN 201210553280XA CN 201210553280 A CN201210553280 A CN 201210553280A CN 103159413 A CN103159413 A CN 103159413A
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Abstract
The invention relates to an impregnating compound with a carbon nano tube used for glass fiber. The impregnating compound comprises, by weight, 3%-10% of dye-fixing agent, 3%-10% of epoxy resin, 0.5%-5% of cationic surface active agent, 0.1%-5% of coupling agent, 0.1%-1% of carbon nano tube and 69%-93.3% of deionized water. A preparation method comprises a step of adding bisphenol A epoxy resin into ionized water, a step of stirring the mixture of the bisphenol A epoxy resin and the ionized water 200-500 revolutions per minute for 1-2 hours under a condition that the temperature is kept in the range of 60-80 DEG C, a step of adding dicyandiamide formaldehyde resin, the cationic surface active agent, a silane coupling agent and a modified carbon nano tube in sequence to be stirred and adding the deionized water to be stirred to obtain the impregnating compound. The impregnating compound is simple and practical in ingredient and suitable for industrial production. The prepared impregnating compound can effectively enhance the strength of the glass fiber, and can improve the strength of glass fiber composites.
Description
Technical field
The invention belongs to treating compound and preparation field thereof, particularly a kind of glass fibre is with adding carbon nanotube treating compound and preparation thereof.
Background technology
In the glass fibre actual production, in drawing process, the sharply decline of temperature can make glass fibre produce surface stress, thereby the formation crizzle descends fibre property, therefore usually sprays or dip-coating one deck treating compound at fiber surface when stretching.Treating compound mainly contains two effects: prevent on the one hand the generation of fiberglass surfacing tiny crack and diffusion, the interfibrous frictionally damage of minimizing, improve the intensity of fiber; Treating compound can improve the cohesive strength between fiber and matrix on the other hand.
CNTs has fabulous mechanical property, as tensile strength (200GPa), Young's modulus (200～500GPa) and breaking strain (10 ~ 30%), be the ideal chose as modifying interface.More and more about the research report of CNTs/ nanocomposite, add a small amount of CNTs just can obviously improve the performance of material in resin.CNTs has huge specific surface area, plays obvious interfacial effect, bridging action in the middle of resin, Anticrack, thus improved the strength of materials.Report is arranged, by electrophoretic deposition (EPD) method, CNTs is deposited to fiberglass surfacing, think that nanoparticle is similar to the mineral substance in biological bone, the suitable nano level interfacial energy that forms thus improves the cohesive strength of fiber and resin, improves the intensity of glass filament reinforced plastics.
When CNTs adds in treating compound, modified CNTs and glass fibre are combined closely, and play bridging action in cracks, improve the tensile strength of fiber; Also can improve simultaneously the interface structure between glass fibre and resin, improve cohesive strength.In a word, add CNTs in treating compound, can greatly improve the fiberglass products quality.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of glass fibre with adding carbon nanotube treating compound and preparation method thereof, and the formula that the present invention adopts is simple, practical, is applicable to suitability for industrialized production; The treating compound of preparation can effectively improve the intensity of glass fibre; And can improve the intensity of glass fiber compound material.
A kind of glass fibre of the present invention is with adding the carbon nanotube treating compound, and it is characterized in that: this treating compound is composed of the following components by weight percentage:
Described laking agent is the Dyhard RU 100 formaldehyde resin, and density is 1.198g/cm
3, viscosity is 500 ~ 560mPas.
Described epoxy resin is the bisphenol A type epoxy resin emulsion, and relative molecular mass is 350 ~ 1000, and median size is 0.2 ~ 2.0 μ m.
Described cats product is palmityl trimethyl ammonium chloride.
Described coupling agent is silane coupling agent, and model is KH-550, KH-560 or A186.
Described carbon nanotube is modified carbon nano-tube, and method of modifying is: (1) carbon nanotube adds acid with strong oxidizing property, and 20 ~ 30h is stirred in then heating, and then centrifugal or natural subsidence is cleaned, and obtains the black mixed solution of carbon nanotube and water; (2) add second diene triamine, polypropylene pyrrolidone in the black mixed solution that makes, stir 5 ~ 10h under 70 ℃ ~ 110 ℃ conditions, namely obtain the CNT (carbon nano-tube) of modification, wherein the mass ratio of carbon nanotube and acid with strong oxidizing property is 1:50 ~ 1:300, and the mass ratio of polypropylene pyrrolidone and carbon nanotube is 1:20 ~ 1:10; The mass ratio of second diene triamine and carbon nanotube is 1:15 ~ 1:10.
Described acid with strong oxidizing property is concentrated nitric acid.
A kind of glass fibre treating compound preparation method who adds carbon nanotube of the present invention, comprise: add by weight percentage bisphenol A type epoxy resin 3%-10%, add in ionized water, temperature keeps 60 ~ 80 ℃, stir 1 ~ 2h under 200 ~ 500r/min, then the carbon nanotube 0.1%-1% that adds successively Dyhard RU 100 formaldehyde resin 3%-10%, cats product 0.5%-5%, silane coupling agent 0.1%-5%, modification, stir, add at last deionized water, stir, namely get treating compound, wherein the total weight percent of deionized water is 69%-93.3%.
The present invention is by the intensity of multifilament strength tester tested glass fiber, and precursor powerful (N/TEX) represents the intensity of glass fibre, gets 10 groups of samples and records fibre strength, and getting its mean value is glass fiber strength.
The present invention has improved the intensity of glass fibre by the organic assembling of several raw materials.The Dyhard RU 100 formaldehyde resin is the polymkeric substance of the strong positive charge of a kind of lower molecular weight ,-CONH
2Hydrophilic radical coordinates distinctive dual quaternary amine type cation activity group, and making between itself and fiber has very strong bonding force.Membrane-forming agent epoxy resin and laking agent form the higher resin film of one deck intensity at fiber surface, and have added the carbon nanotube of modification, can realize the effect of effective reinforcing glass fiber.This formula is simple, practical, not only can improve the intensity of glass fibre, and the Fiber In Composite Material of making and the cohesive strength of resin are higher, can improve to a great extent the quality of glass fiber product.
Beneficial effect
(1) formula of the present invention's employing is simple, practical, is applicable to suitability for industrialized production;
(2) treating compound of the present invention's preparation can effectively improve the intensity of glass fibre;
(3) treating compound of the present invention's preparation can improve the intensity of glass fiber compound material.
Description of drawings
Fig. 1 is the field emission scanning electron microscope photo that has applied the glass fibre that adds 0.3% carbon nanotube treating compound.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used for explanation the present invention and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
The 5g carbon nanotube is put into there-necked flask, adds the 250ml concentrated nitric acid, then stir 20h under heating condition, then with dehydrated alcohol, deionized water is centrifugal or natural subsidence is cleaned repeatedly, obtains at last the black mixed solution of carbon nanotube and water.Add 0.5g second diene triamine, 1.0g polypropylene pyrrolidone to stir 10h under 70 ℃ of conditions in the black mixed solution that makes, obtain the CNT (carbon nano-tube) of modification.
Per distribution ratio takes 5% bisphenol A type epoxy resin by weight, adds that to add weight percent be in the container of 50% deionized water to, and temperature keeps 60 ℃, stirs 1h under 500r/min.Then add successively by weight percentage Dyhard RU 100 formaldehyde resin 5%, cats product 1%, silane resin acceptor kh-550 0.3%, modified carbon nano-tube 0.1%, each stirs 0.5h, wherein cats product dilutes with deionized water in advance, adding at last weight percent is 38.6% deionized water, stir 2.5h, namely get treating compound, intensity N/TEX is 0.52.
Embodiment 2
The 5g carbon nanotube is put into there-necked flask, adds the 300ml concentrated nitric acid, then stir 30h under heating condition, then with dehydrated alcohol, deionized water is centrifugal or natural subsidence is cleaned repeatedly, obtains at last the black mixed solution of carbon nanotube and water.Add 0.7g second diene triamine, 0.9g polypropylene pyrrolidone to stir 5h under 110 ℃ of conditions in the black mixed solution that makes, obtain the CNT (carbon nano-tube) of modification.
Per distribution ratio takes 5% bisphenol A type epoxy resin by weight, adds that to add weight percent be in the container of 50% deionized water to, and temperature keeps 80 ℃, stirs 2h under 200r/min.Then add successively by weight percentage Dyhard RU 100 formaldehyde resin 5%, cats product 1%, silane coupling agent KH-5600.3%, modified carbon nano-tube 0.3%, each stirs 0.5h, wherein cats product dilutes with deionized water in advance, adding at last weight percent is 38.4% deionized water, stir 2.5h, namely get treating compound, intensity N/TEX is 0.57.
Embodiment 3
The 5g carbon nanotube is put into there-necked flask, adds the 350ml concentrated nitric acid, then stir 30h under heating condition, then with dehydrated alcohol, deionized water is centrifugal or natural subsidence is cleaned repeatedly, obtains at last the black mixed solution of carbon nanotube and water.Add 0.9g second diene triamine, 0.8g polypropylene pyrrolidone to stir 5h under 110 ℃ of conditions in the black mixed solution that makes, obtain the CNT (carbon nano-tube) of modification.
Per distribution ratio takes 5% bisphenol A type epoxy resin by weight, adds that to add weight percent be in the container of 50% deionized water to, and temperature keeps 60 ℃, stirs 1h under 250r/min.Then add successively by weight percentage Dyhard RU 100 formaldehyde resin 5%, cats product 1%, silane resin acceptor kh-550 0.3%, modified carbon nano-tube 0.5%, each stirs 0.5h, wherein cats product dilutes with deionized water in advance, adding at last weight percent is 38.2% deionized water, stir 2.5h, namely get treating compound, intensity N/TEX is 0.61.
Embodiment 4
The 5g carbon nanotube is put into there-necked flask, adds the 400ml concentrated nitric acid, then stir 30h under heating condition, then with dehydrated alcohol, deionized water is centrifugal or natural subsidence is cleaned repeatedly, obtains at last the black mixed solution of carbon nanotube and water.Add that 1.0g enters second diene triamine, 0.7g polypropylene pyrrolidone stirs 5h under 110 ℃ of conditions in the black mixed solution that makes, obtain the CNT (carbon nano-tube) of modification.
Per distribution ratio takes 5% bisphenol A type epoxy resin by weight, adds that to add weight percent be in the container of 50% deionized water to, and temperature keeps 60 ℃, stirs 1h under 250r/min.Then add successively by weight percentage Dyhard RU 100 formaldehyde resin 5%, cats product 1%, silane resin acceptor kh-550 0.3%, modified carbon nano-tube 0.9%, each stirs 0.5h, wherein cats product dilutes with deionized water in advance, adding at last weight percent is 37.8% deionized water, stir 2.5h, namely get treating compound, intensity N/TEX is 0.60.
The comparative example 1
Take by weight percentage 3.5% bisphenol A type epoxy resin, add that to add weight percent be in the container of 50% deionized water to, temperature keeps 60 ℃, stirs 1h under 250r/min.Then add by weight percentage successively Dyhard RU 100 formaldehyde resin 3.5%, cats product 1%, silane resin acceptor kh-550 0.3%,, each stirs 0.5h.Cats product adds 41.7% deionized water at last by weight percentage in advance with the deionized water dilution, stirs 2.5h, namely gets treating compound, and intensity N/TEX is 0.42.
The comparative example 2
Per distribution ratio takes 5% bisphenol A type epoxy resin by weight, adds that to add weight percent be in the container of 50% deionized water to, and temperature keeps 60 ℃, stirs 1h under 250r/min.Then add successively by weight percentage Dyhard RU 100 formaldehyde resin 5%, cats product 1%, silane resin acceptor kh-550 0.3%, respectively stir 0.5h, wherein cats product dilutes with deionized water in advance, last 38.7% the deionized water of adding by weight percentage, stir 2.5h, namely get treating compound, intensity N/TEX is 0.45.
Claims (8)
1. a glass fibre is with the treating compound that adds carbon nanotube, and this treating compound is composed of the following components by weight percentage: laking agent 3%-10%, epoxy resin 3%-10%, cats product 0.5%-5%, coupling agent 0.1%-5%, carbon nanotube 0.1%-1%, deionized water 69%-93.3%.
2. a kind of glass fibre use according to claim 1 is added the treating compound of carbon nanotube, and it is characterized in that: described laking agent is the Dyhard RU 100 formaldehyde resin, and density is 1.198g/cm
3, viscosity is 500 ~ 560mPas.
3. a kind of glass fibre use according to claim 1 is added the treating compound of carbon nanotube, and it is characterized in that: described epoxy resin is the bisphenol A type epoxy resin emulsion, and relative molecular mass is 350 ~ 1000, and median size is 0.2 ~ 2.0 μ m.
4. a kind of glass fibre use according to claim 1 is added the treating compound of carbon nanotube, and it is characterized in that: described cats product is palmityl trimethyl ammonium chloride.
5. a kind of glass fibre use according to claim 1 is added the treating compound of carbon nanotube, and it is characterized in that: described coupling agent is silane coupling agent, and model is KH-550, KH-560 or A186.
6. a kind of glass fibre use according to claim 1 is added the treating compound of carbon nanotube, it is characterized in that: described carbon nanotube is modified carbon nano-tube, method of modifying is: (1) carbon nanotube adds acid with strong oxidizing property, then heating, stir 20 ~ 30h, then centrifugal or natural subsidence is cleaned, and obtains the black mixed solution of carbon nanotube and water; (2) add second diene triamine, polypropylene pyrrolidone in the black mixed solution that makes, stir 5 ~ 10h under 70 ℃ ~ 110 ℃ conditions, namely obtain the CNT (carbon nano-tube) of modification, wherein the mass ratio of carbon nanotube and acid with strong oxidizing property is 1:50 ~ 1:300, and the mass ratio of polypropylene pyrrolidone and carbon nanotube is 1:20 ~ 1:10; The mass ratio of second diene triamine and carbon nanotube is 1:15 ~ 1:10.
7. a kind of glass fibre use according to claim 6 is added the treating compound of carbon nanotube, and it is characterized in that: described acid with strong oxidizing property is concentrated nitric acid.
8. a glass fibre with the treating compound preparation method who adds carbon nanotube, comprising:
Add by weight percentage bisphenol A type epoxy resin 3%-10%, add in ionized water, temperature keeps 60 ~ 80 ℃, stir 1 ~ 2h under 200 ~ 500r/min, then add successively the carbon nanotube 0.1%-1% of Dyhard RU 100 formaldehyde resin 3%-10%, cats product 0.5%-5%, silane coupling agent 0.1%-5%, modification, stir, add at last deionized water, stir, namely get treating compound, wherein the total weight percent of deionized water is 69%-93.3%.
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| CN103553366A (en) * | 2013-10-29 | 2014-02-05 | 东华大学 | Glass fiber soakage agent for dyeing and preparation method of glass fiber soakage agent |
| CN104086094A (en) * | 2014-07-16 | 2014-10-08 | 哈尔滨工业大学 | Carbon-nanotube-containing glass fiber wetting agent, and preparation method and application thereof |
| CN107141977A (en) * | 2017-05-08 | 2017-09-08 | 河海大学 | A kind of carbon nano-tube modification coating and preparation method and application |
| CN108658480A (en) * | 2018-05-30 | 2018-10-16 | 陈毅忠 | A kind of preparation method of high combination basalt cladded type size |
| CN111620571A (en) * | 2020-06-04 | 2020-09-04 | 苏州北美国际高级中学 | Anti-ultraviolet magnetic glass fiber and manufacturing method thereof |
| CN115011041A (en) * | 2022-07-15 | 2022-09-06 | 中广核俊尔(浙江)新材料有限公司 | Environment-friendly high-gloss low-floating-fiber continuous reinforced long glass fiber polypropylene composite material |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103553366A (en) * | 2013-10-29 | 2014-02-05 | 东华大学 | Glass fiber soakage agent for dyeing and preparation method of glass fiber soakage agent |
| CN103553366B (en) * | 2013-10-29 | 2015-12-30 | 东华大学 | A kind of dyeing glass fiber infiltration agent and preparation method thereof |
| CN104086094A (en) * | 2014-07-16 | 2014-10-08 | 哈尔滨工业大学 | Carbon-nanotube-containing glass fiber wetting agent, and preparation method and application thereof |
| CN107141977A (en) * | 2017-05-08 | 2017-09-08 | 河海大学 | A kind of carbon nano-tube modification coating and preparation method and application |
| CN108658480A (en) * | 2018-05-30 | 2018-10-16 | 陈毅忠 | A kind of preparation method of high combination basalt cladded type size |
| CN111620571A (en) * | 2020-06-04 | 2020-09-04 | 苏州北美国际高级中学 | Anti-ultraviolet magnetic glass fiber and manufacturing method thereof |
| CN115011041A (en) * | 2022-07-15 | 2022-09-06 | 中广核俊尔(浙江)新材料有限公司 | Environment-friendly high-gloss low-floating-fiber continuous reinforced long glass fiber polypropylene composite material |
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