CN110725124A - Interface enhancement method for para-aramid-polytetrafluoroethylene blended fiber fabric - Google Patents
Interface enhancement method for para-aramid-polytetrafluoroethylene blended fiber fabric Download PDFInfo
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- CN110725124A CN110725124A CN201911225992.7A CN201911225992A CN110725124A CN 110725124 A CN110725124 A CN 110725124A CN 201911225992 A CN201911225992 A CN 201911225992A CN 110725124 A CN110725124 A CN 110725124A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/02—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with hydrocarbons
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic System
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- D06M13/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
- D06M13/10—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
- D06M13/144—Alcohols; Metal alcoholates
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/39—Aldehyde resins; Ketone resins; Polyacetals
- D06M15/41—Phenol-aldehyde or phenol-ketone resins
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- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/22—Polymers or copolymers of halogenated mono-olefins
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/30—Synthetic polymers consisting of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/34—Polyamides
- D06M2101/36—Aromatic polyamides
Abstract
The invention discloses an interface enhancement method of para-aramid fiber-polytetrafluoroethylene blended fiber fabric, which comprises the steps of firstly carrying out reflux washing and drying on para-aramid fiber-polytetrafluoroethylene blended fiber fabric grey cloth by using petroleum ether and ethanol respectively, then immersing the para-aramid fiber-polytetrafluoroethylene blended fiber fabric grey cloth into a dimethyl sulfoxide-potassium hydroxide etching system for etching treatment, washing the para-aramid fiber-polytetrafluoroethylene blended fiber fabric grey cloth by using distilled water, and drying the para-aramid fiber-polytetrafluoroethylene blended fiber fabric grey cloth to obtain surface-activated blended fiber fabric grey cloth; and then repeatedly dipping the fiber fabric grey cloth subjected to surface activation treatment in a dipping material consisting of phenolic resin and epoxy resin to obtain a prepreg, and drying to obtain the self-lubricating fiber fabric with the enhanced interface. The invention realizes the simultaneous modification of aramid fiber and polytetrafluoroethylene fiber through surface activation and modification treatment, so that the surface roughness, polarity and wettability of the para-aramid fiber and the polytetrafluoroethylene fiber are obviously improved, and the method has great promotion effect on the performance improvement and application field expansion of the para-aramid fiber and products thereof.
Description
Technical Field
The invention relates to an interface enhancement method of para-aramid-polytetrafluoroethylene fiber fabric, belonging to the technical field of chemical synthesis and the technical field of lubricating materials.
Background
The aramid fiber is a chemically synthesized high-performance fiber, is called aromatic polyamide fiber completely, and a macromolecular main chain consists of amido bonds and aromatic rings, wherein at least 85 percent of the amido bonds are connected with benzene rings. The aramid fiber has excellent properties such as high specific modulus, high specific strength, fatigue resistance, good temperature resistance and the like, and is widely applied. However, due to the steric effect of a benzene ring in the macromolecular structure of the aramid fiber and the conjugation between the benzene ring and an amido bond, the surface of the aramid fiber has low reactivity and few active functional groups, and the surface of the fiber is smooth, so that the interface bonding strength between the fiber and a resin matrix is weak, and the application fields of the aramid fiber and products thereof are greatly limited. Therefore, the surface of the fiber is modified by a chemical or physical method, so that the surface roughness, the active functional group content and the wettability of the fiber are increased, the interface bonding strength between the aramid fiber and the resin matrix is further improved, and the comprehensive performance of the aramid fiber product is improved.
Polytetrafluoroethylene (PTFE) has very good lubricating property and can be widely applied to self-lubricating composite materials. However, the PTFE fiber has a problem that the bond energy of the carbon-fluorine bond in the macromolecule is high, and the interface bonding property between the fiber and the resin matrix is also poor. In recent years, researches on the surface modification of aramid fibers and PTFE fibers have attracted much attention, but in the current reports related to the surface modification of aramid fibers, methods of surface grafting modification and fiber interface growth are mainly adopted, so that the uniform modification of aramid fibers and the modification of PTFE fibers are difficult to realize. Chinese patent CN109914094A discloses a preparation method of nano zinc oxide modified aramid fiber, which comprises the steps of firstly carrying out activation treatment on the aramid fiber, and then carrying out activation treatment on the aramid fiberThe zinc oxide nanowire grows through interface grafting, but the chemical bonding effect between the zinc oxide nanowire and the aramid fiber is weak. Chinese patent CN105862396A discloses a surface modified aramid fiber and a preparation method thereof, wherein aramid fiber with hydroxyl is placed in SiO2The aramid fiber with ultraviolet resistance and excellent surface activity is obtained by respectively and repeatedly soaking, washing and drying the colloidal aqueous solution and the MgAlFe layered double hydroxide suspension, but the aramid fiber is firstly required to be hydroxylated in the preparation process, and the self-assembly process is complicated. Chinese patent CN103225210 discloses a surface graft modified aramid fiber and a preparation method thereof, wherein an aminated aramid fiber is reacted with three kinds of silanes to obtain an aramid fiber with two kinds of functional groups on the surface, but the aramid fiber needs to be aminated in advance. Although there are many reports on the surface modification of aramid fibers at present, the surface of aramid fibers needs to be activated in advance, and the simultaneous modification of two types of fibers cannot be realized for a composite material consisting of aramid fibers and polytetrafluoroethylene fibers.
Disclosure of Invention
The invention aims to provide an interface reinforcing method for a para-aramid-polytetrafluoroethylene blended fiber fabric.
Interface enhancement method for para-aramid-polytetrafluoroethylene blended fiber fabric
The interface enhancement method of the para-aramid fiber-polytetrafluoroethylene blended fiber fabric comprises the steps of firstly carrying out reflux washing and drying on a para-aramid fiber-polytetrafluoroethylene blended fiber fabric gray fabric by using petroleum ether and ethanol respectively, then immersing the para-aramid fiber-polytetrafluoroethylene blended fiber fabric gray fabric into a dimethyl sulfoxide-potassium hydroxide etching system for etching treatment, washing by using distilled water, drying to obtain a surface activation treated blended fiber fabric gray fabric, then repeatedly immersing the surface activation treated fiber fabric gray fabric into an impregnating material consisting of phenolic resin and epoxy resin until the weight of the fiber fabric is increased by 5 ~ 35wt%, stopping impregnation, obtaining a prepreg, and drying to obtain the interface enhanced self-lubricating fiber fabric.
The fiber fabric grey cloth reflux washing is carried out by adopting a Soxhlet extractor, and the petroleum ether and ethanol reflux time is 15 ~ 48h respectively.
In the dimethyl sulfoxide-potassium hydroxide etching system, the mass volume ratio of potassium hydroxide to dimethyl sulfoxide is 0.2 ~ 6g/L, and the etching treatment is carried out for 0.5 ~ 15h under the conditions that the system temperature is controlled at 18.4 ~ 189 ℃ and the stirring speed is 50 ~ 1000 rpm.
In the impregnating compound, the mass ratio of the phenolic resin to the epoxy resin is 4:1 ~ 7:1, and the drying is carried out in an oven at 60 ~ 80 ℃ for 10 ~ 12 h.
Evaluation of interfacial properties of para-aramid-polytetrafluoroethylene blended fiber fabric-phenolic resin
1. Bonding property of para-aramid-polytetrafluoroethylene blended fiber fabric
Cutting the self-lubricating fiber fabric obtained by the treatment into prepreg (2 multiplied by 12 cm) with a certain size, adhering the prepreg to the surface of the AISI-1045 stainless steel base material, and curing at 180 ℃ for 2h to obtain a test piece for testing the bonding strength. A universal material testing machine is adopted to carry out bonding performance test, and the peeling test speed is 50 mm/min.
FIG. 1 is a graph showing the effect of the surface treatment of the fibers of the present invention on the bonding strength of a gasket. The test results in fig. 1 show that the bonding strength of the self-lubricating fiber fabric composite material (b) after the modification treatment is improved by 84% compared with that of the untreated self-lubricating fiber fabric (a) (i.e., the composite material obtained by directly and repeatedly impregnating the grey fabric of the fiber fabric in the impregnating material consisting of the phenolic resin and the epoxy resin and then curing).
2. Tensile property of para-aramid-polytetrafluoroethylene blended fiber fabric
The self-lubricating fiber fabric obtained by the treatment is cut into a prepreg (2 multiplied by 12 cm) with a certain size, and is cured for 2 hours at 180 ℃ to obtain a test piece for tensile strength test. A universal material testing machine is adopted to carry out bonding performance test, and the tensile test speed is 50 mm/min.
FIG. 2 is a graph showing the effect of the surface treatment of the fibers of the present invention on the tensile strength of a liner. The test results in fig. 2 show that the tensile strength of the self-lubricating fiber fabric (b) modified by the treatment of the invention is improved by 32% compared with the untreated self-lubricating fiber fabric (a).
3. Surface appearance before and after para-aramid fiber modification
FIG. 3 shows the surface morphology of para-aramid fibers before and after treatment by the method of the present invention. In fig. 3a, the untreated para-aramid fiber has a smooth surface, and only a small amount of particulate matter adheres to the surface, which is not favorable for forming an excellent fiber-resin interface. After the modification treatment (fig. 3 b), the fiber surface roughness is obviously increased, and a large amount of nano fibers are distributed on the fiber surface, which is beneficial to improving the bonding effect at the fiber-resin interface and improving the comprehensive performance of the composite material.
FIG. 4 shows the surface morphology of the polytetrafluoroethylene fibers before and after treatment by the method of the invention. Wherein, FIG. 4a shows the untreated polytetrafluoroethylene fiber, the surface is very smooth, the inertia of the polytetrafluoroethylene fiber surface is strong, and the fiber-resin interface bonding effect is weak. After modification treatment, the surface roughness of the fiber is obviously increased, and a large amount of granular substances are coated on the surface of the fiber, so that the improvement of the bonding effect on a fiber-resin interface is facilitated, and the comprehensive performance of the composite material is improved.
In conclusion, the invention realizes the simultaneous modification of the para-aramid fiber and the polytetrafluoroethylene fiber by the surface activation modification treatment, so that the surface roughness, the polarity and the wettability of the para-aramid fiber and the polytetrafluoroethylene fiber are obviously improved. The mechanical property evaluation result shows that the interface performance of the para-aramid fiber-polytetrafluoroethylene fiber-phenolic resin is greatly improved, and the method has a great promotion effect on the improvement of the performance of the para-aramid fiber and products thereof and the expansion of the application field.
Drawings
FIG. 1 is a graph showing the effect of the surface treatment of the fibers of the present invention on the bonding strength of a gasket.
FIG. 2 is a graph showing the effect of the surface treatment of the fibers of the present invention on the tensile strength of a liner.
FIG. 3 is a photograph of the surface morphology of para-aramid fibers before and after treatment by the method of the present invention.
FIG. 4 is a photograph of the surface topography of the polytetrafluoroethylene fibers before and after treatment by the method of the invention.
Detailed Description
The method and effect of the invention for enhancing the interface of the para-aramid-polytetrafluoroethylene mixed fiber fabric are further explained by the following specific examples.
Example 1
Placing the para-aramid fiber-polytetrafluoroethylene blended fiber fabric grey cloth in a Soxhlet extractor, and respectively adopting petroleum ether and ethanol for reflux washing for 36 hours; then taking out the self-lubricating fabric and putting the self-lubricating fabric in an oven at 80 ℃ overnight; cutting washed aramid fiber-Polytetrafluoroethylene (PTFE) fiber fabric grey cloth (6 multiplied by 12 cm) with a certain size, immersing the grey cloth in a mixed system consisting of dimethyl sulfoxide (500 ml) and potassium hydroxide (0.5 g), and continuously stirring for 6 hours at the temperature of 40 ℃ and the speed of 200 rpm; then taking out the fiber fabric grey cloth, and washing the fiber fabric grey cloth by using dimethyl sulfoxide and deionized water respectively to obtain the fiber fabric grey cloth subjected to surface treatment; and finally, repeatedly impregnating the fiber fabric gray fabric subjected to surface treatment in an impregnating material consisting of phenolic resin and epoxy resin (the mass ratio of the phenolic resin to the epoxy resin in the impregnating material is 4: 1), and stopping impregnation after the weight of the fiber fabric is increased by 25% to obtain the prepreg. The fabric blank was tested for adhesion of 4.4N/mm and tensile strength of 240 MPa according to the method described above.
Example 2
Placing the para-aramid fiber-polytetrafluoroethylene blended fiber fabric grey cloth in a Soxhlet extractor, and respectively adopting petroleum ether and ethanol for reflux washing for 36 hours; then taking out the self-lubricating fabric and putting the self-lubricating fabric in an oven at 80 ℃ overnight; cutting washed aramid fiber-Polytetrafluoroethylene (PTFE) fiber fabric grey cloth (6 multiplied by 12 cm) with a certain size, immersing the grey cloth in a mixed system consisting of dimethyl sulfoxide (500 ml) and potassium hydroxide (1 g), and continuously stirring for 3 hours at room temperature and 400 rpm; then taking out the fiber fabric grey cloth, and washing the fiber fabric grey cloth by using dimethyl sulfoxide and deionized water respectively to obtain the fiber fabric grey cloth subjected to surface treatment; and finally, repeatedly impregnating the fiber fabric gray fabric subjected to surface treatment in an impregnating material consisting of phenolic resin and epoxy resin (the mass ratio of the phenolic resin to the epoxy resin in the impregnating material is 7: 1), and stopping impregnation after the weight of the fiber fabric is increased by 25wt% to obtain the prepreg. The fabric blank was tested for its adhesive strength of 5.12N/mm and tensile strength of 276 MPa according to the method described above.
Example 3
Placing the para-aramid fiber-polytetrafluoroethylene blended fiber fabric grey cloth in a Soxhlet extractor, and respectively adopting petroleum ether and ethanol for reflux washing for 36 hours; then taking out the self-lubricating fabric and putting the self-lubricating fabric in an oven at 80 ℃ overnight; the washed aramid fiber-Polytetrafluoroethylene (PTFE) fiber fabric grey cloth (6 x 12 cm) with a certain size is cut, immersed in a mixed system consisting of dimethyl sulfoxide (500 ml) and potassium hydroxide (1.5 g), and continuously stirred for 3h at the room temperature and 800 rpm. Then taking out the fiber fabric grey cloth, and washing the fiber fabric grey cloth by using dimethyl sulfoxide and deionized water respectively to obtain the fiber fabric grey cloth subjected to surface treatment; and finally, repeatedly impregnating the fiber fabric gray fabric subjected to surface treatment in an impregnating material consisting of phenolic resin and epoxy resin (the mass ratio of the phenolic resin to the epoxy resin in the impregnating material is 5: 1), and stopping impregnation after the weight of the fiber fabric is increased by 25wt% to obtain the prepreg. The fabric greige goods were tested for adhesion 4.98N/mm and tensile strength 308MPa according to the method described above.
Example 4
Placing the para-aramid fiber-polytetrafluoroethylene blended fiber fabric grey cloth in a Soxhlet extractor, and respectively adopting petroleum ether and ethanol for reflux washing for 36 hours; then taking out the self-lubricating fabric and putting the self-lubricating fabric in an oven at 80 ℃ overnight; the washed aramid fiber-Polytetrafluoroethylene (PTFE) fiber fabric grey cloth (6 x 12 cm) with a certain size is cut, immersed in a mixed system consisting of dimethyl sulfoxide (500 ml) and potassium hydroxide (1.5 g), and continuously stirred for 3 hours at the temperature of 60 ℃ and the speed of 200 rpm. Then taking out the fiber fabric grey cloth, and washing the fiber fabric grey cloth by using dimethyl sulfoxide and deionized water respectively to obtain the fiber fabric grey cloth subjected to surface treatment; and finally, repeatedly impregnating the fiber fabric gray fabric subjected to surface treatment in an impregnating material consisting of phenolic resin and epoxy resin (the mass ratio of the phenolic resin to the epoxy resin in the impregnating material is 6: 1), and stopping impregnation after the weight of the fiber fabric is increased by 25wt% to obtain the prepreg. The fabric greige goods were tested for adhesion properties of 7.01N/mm and tensile strength of 225 MPa according to the method described above.
Claims (7)
1. An interface enhancement method of a para-aramid fiber-polytetrafluoroethylene blended fiber fabric comprises the steps of firstly, respectively carrying out reflux washing and drying on a para-aramid fiber-polytetrafluoroethylene blended fiber fabric gray fabric by using petroleum ether and ethanol, then, immersing the para-aramid fiber-polytetrafluoroethylene blended fiber fabric gray fabric into a dimethyl sulfoxide-potassium hydroxide etching system for etching treatment, washing by using distilled water, and drying to obtain a surface activation treated blended fiber fabric gray fabric; and then repeatedly dipping the fiber fabric grey cloth subjected to surface activation treatment in a dipping material consisting of phenolic resin and epoxy resin to obtain a prepreg, and drying to obtain the self-lubricating fiber fabric with the enhanced interface.
2. The interface enhancement method for the para-aramid-polytetrafluoroethylene blended fiber fabric according to claim 1, wherein the fiber fabric grey fabric is washed by a Soxhlet extractor, and the petroleum ether and ethanol reflux time is 15 ~ 48h respectively.
3. The interface enhancement method for the para-aramid-polytetrafluoroethylene blended fiber fabric according to claim 1, wherein in the dimethyl sulfoxide-potassium hydroxide etching system, the mass volume ratio of potassium hydroxide to dimethyl sulfoxide is 0.2 ~ 6 g/L.
4. The interface enhancement method of the para-aramid-polytetrafluoroethylene blended fiber fabric is characterized in that the etching treatment is carried out for 0.5 ~ 15h at the temperature of 18.4 ~ 189 ℃ and the stirring speed of 50 ~ 1000rpm under the control of the system temperature.
5. The method for enhancing the interface of the para-aramid-polytetrafluoroethylene blended fiber fabric according to claim 1, wherein the mass ratio of the phenolic resin to the epoxy resin in the impregnating material is 4:1 ~ 7: 1.
6. The method for interfacial reinforcement of para-aramid-polytetrafluoroethylene blended fiber fabric according to claim 1, wherein the fiber fabric grey fabric is repeatedly impregnated in an impregnating material until the weight of the fiber fabric is increased by 5 ~ 35wt%, and then the impregnation is stopped.
7. The method for enhancing the interface of the para-aramid-polytetrafluoroethylene blended fiber fabric is characterized in that the drying is carried out in an oven at the temperature of 60 ~ 80 ℃ for 10 ~ 12 hours.
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| CN117024843A (en) * | 2023-07-23 | 2023-11-10 | 深圳赛兰仕科创有限公司 | Preparation method of ultralow-dielectric low-loss epoxy composite material |
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