CN1487022A - Prepn of RE-modified composite glass fiber/PTFE material - Google Patents
Prepn of RE-modified composite glass fiber/PTFE material Download PDFInfo
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- CN1487022A CN1487022A CNA031416667A CN03141666A CN1487022A CN 1487022 A CN1487022 A CN 1487022A CN A031416667 A CNA031416667 A CN A031416667A CN 03141666 A CN03141666 A CN 03141666A CN 1487022 A CN1487022 A CN 1487022A
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Abstract
The preparation process of RE-modified composite glass fiber /PTFE material includes pre-treatment of glass fiber to eliminate its residual organic matter, surface modification of glass fiber with RE modifier, cutting modified glass fiber, mechanical mixing of the glass fiber with PTFE powder while controlling the glass fiber mass as 10-30% of the mixture, pressing the mixture in stainless steel mold to form and high temperature sintering to produce the composite material. The RE modifier consists of RE compound, ethanol, EDTA, ammonium chloride, nitric acid and urea. The composite material has excellent mechanical performance and friction performance.
Description
Technical field:
The present invention relates to a kind of preparation method of matrix material, relate in particular to a kind of rare-earth-modified glass-fiber/ptfe composite preparation method, adopt glass fibre filled polytetrafluoroethylene through the rare earth surface modification treatment, obtaining than higher interface binding power, and then the practical engineering application that improves matrix material is worth.
Background technology:
Tetrafluoroethylene is the most potential antifriction material, though it is good to have a self-lubricating property, frictional coefficient is minimum, corrosion-resistant, low temperature tolerance characteristics is excellent, but because of its bad mechanical property, linear expansivity is big, thermal conductivity is poor again, and abrasion loss is big, uses and be unsuitable for doing separately high-abrasive material.Common employing adds fillers such as glass fibre, carbon fiber, graphite it is carried out modification in tetrafluoroethylene, be prepared into ptfe composite, in the hope of when keeping its low-friction coefficient, obtain good wear resistance and high strength, high rigidity and dimensional stability.Glass fibre is the enhancing body that is most widely used in the fibre reinforced composites, and glass fibre filled polytetrafluoroethylene matrix material can reduce the wear resistance of material greatly.
But, affinity between glass fibre and the thermoplastic resin matrix is relatively poor, lacks chemical bonding and interfacial layer and has immiscible component, and interface binding intensity is low, compound tense forms space and defective easily on the interface, strengthen body and matrix resin and be difficult to be formed with effective adhesive.Composite material interface is the tie that wild phase and matrix are got in touch, and also is the bridge of wild phase performance effective capacity.For this reason, must be by to methods such as the physics of the surface modification of glass fibre and matrix, chemical modifications, improve the wetting property between fiber and the matrix, even between fiber and matrix, form Chemical bond, to improve the interface bond strength between fiber and the matrix, obtain the high matrix material of interlaminar shear strength.
At present, mainly use the interface binding power of coupling agents to improve glass fibre and polymeric matrix, to improve the over-all properties of glass fibre reinforced polymer composites.The coupling agent method has been improved the bonding force of interfacial phase to a certain extent, has improved the use value of matrix material.But handle fiberglass surfacing with conventional coupling agent method and do not reach the ideal effect, on the one hand, exist treatment effect instability, degeneration easily,, shortcomings such as fiber surface viscosity big, poor processability big, cause the interface binding power of matrix material relatively poor fibre-tendering; On the other hand, the coupling agent deficiency is so that glass fibre and resin matrix have the good interface bonding force, especially when being subjected to shock load, germinate crackle easily, cause the organic interface performance to reduce when reaching high temperature, influenced the friction and wear behavior of tetrafluoroethylene based composites, shown as mainly that to be under no oil or the boundary lubrication situation its impact wear resistance relatively poor.
Summary of the invention:
The objective of the invention is at the deficiencies in the prior art, a kind of rare-earth-modified glass-fiber/ptfe composite preparation method is provided, have that technology is simple, high efficiency, low cost, free of contamination characteristics, can improve the interface binding power of glass fibre and teflon resin matrix, thereby improve the over-all properties of matrix material.
For realizing such purpose, in the technical scheme of the present invention, earlier glass fibre is carried out pre-treatment to remove the organism of remained on surface, at room temperature adopt rare-earth modifier that glass fibre is carried out surface modification treatment again, glass chopped after will handling then, carry out mechanical blending with the tetrafluoroethylene powder, it is hot-forming then mixed powder to be put into stainless steel mould, makes matrix material.Wherein, the component of rare-earth modifier comprises rare earth compound, ethanol, ethylenediamine tetraacetic acid (EDTA), ammonium chloride, nitric acid and urea.
Owing to 4f layer structure and electronegativity that rare earth element is special are less, rare earth element itself has outstanding chemically reactive, can improve the interfacial combined function of glass fibre/ptfe composite by the chemical action that takes place with glass fibre and tetrafluoroethylene.
Specific embodiment of the present invention is as follows:
At first glass fibre is carried out pre-treatment, glass fibre is placed in 500～550 ℃ of muffle furnaces ablated 0.5～1 hour, make its surface organic matter residual quantity below 1%.
Pretreated glass fibre is at room temperature immersed in the rare-earth modifier, and immersion treatment 2～4 hours is filtered and is removed liquid, dries in baking oven then, obtains the glass fibre through the rare earth surface modification treatment.
To carry out mechanical blending with tetrafluoroethylene molding powder through the short glass fiber or the mealy glass fibre of rare earth surface modification treatment, feed glass quality of fiber per-cent is 10～30% of mixed powder, then mixed powder is packed in the stainless steel mould, compression moulding on pressing machine, pressure-controlling is at 40～50MPa, time is 30～50 minutes, pressurization and stress-relief process must slowly carry out, the blank of above-mentioned compression moulding is taken out gently, put into muffle furnace, carry out sintering: slowly be warming up to about 320 ℃ earlier, and then be warming up to about 380 ℃ with 30 ℃/hour speed, be incubated 5～6 hours, again by being machined into glass fibre/ptfe composite sample or part.
The weight percentages of components of the rare-earth modifier that the present invention adopts is:
Rare earth compound: 0.1～2%
Ethanol: 96～99.7%
Ethylenediamine tetraacetic acid (EDTA) (EDTA): 0.05～0.5%
Ammonium chloride: 0.1～1%
Nitric acid: 0.02～0.5%
Urea: 0.03～1%
Rare earth compound of the present invention can be Lanthanum trichloride, Cerium II Chloride, lanthanum trioxide or cerium oxide.
The present invention is applicable to various glass fiber reinforced polyester tetrafluoroethylene matrix materials, wherein glass fibre comprises the alkali free glass fibre of various models, tetrafluoroethylene comprises with suspension polymerization and through the teflon resin of the broken various trades mark that form of fine powder, as SM021 etc.
The present invention can solve the problem of glass fibre/ptfe composite interface binding power difference, improves the mechanical property and the tribological property of matrix material, and processing method is simple, and cost is low.Adopt the matrix material of making through rare earth surface-treated glass fibre filled polytetrafluoroethylene to compare, have better mechanical property and tribological property with common similar matrix material.
Embodiment:
Below by specific embodiment technical scheme of the present invention is further described.
Embodiment 1:
Used starting material comprise: teflon resin, the SM021-F type that ShanghaiChlorine and Alkali Chemical Co Ltd produces; Glass fibre, the alkali free glass fibre that Nanjing Glass Fibre Research and Design Institute is produced, 50 orders.
The weight percentages of components of the rare-earth modifier that adopts is as follows:
Lanthanum trichloride: 0.2%, ethanol: 98.62%, ethylenediamine tetraacetic acid (EDTA) (EDTA): 0.05%, ammonium chloride: 0.1%, nitric acid: 0.03%, urea: 1%.
Earlier glass fibre is carried out pre-treatment, in 500 ℃ of muffle furnaces, ablated 1 hour, make its surface organic matter residual quantity below 1%.Adopt above-mentioned rare-earth modifier for treatment then, glass fibre is at room temperature immersed in the properties-correcting agent, soaked 2 hours, after the filtration, oven dry.
To carry out mechanical blending with tetrafluoroethylene molding powder through the short glass fiber of rare earth surface modification treatment, feed glass quality of fiber per-cent is 10% of mixed powder, pack in the stainless steel mould, compression moulding on pressing machine, pressure-controlling is about 40MPa, time is 30 minutes, pressurization and stress-relief process slowly carry out, the blank of above-mentioned compression moulding is taken out gently, put into muffle furnace, carry out sintering: slowly be warming up to about 320 ℃ earlier, and then be warming up to about 380 ℃, be incubated 5 hours with 30 ℃/hour speed.
It is 16.82MPa that the matrix material that makes according to the method described above records its tensile strength according to ASTM D638-89 standard.
Routine in contrast, under identical fibre content and composite material preparation process condition, untreated glass reinforced TFE matrix material tensile strength is 12.61MPa, and the glass reinforced TFE matrix material tensile strength of handling through silane coupling agent is 14.71MPa.As can be seen, rare-earth modifier for treatment improves the most effective for the tensile property of matrix material.
Embodiment 2:
Used starting material comprise: teflon resin, the SM021-F type that ShanghaiChlorine and Alkali Chemical Co Ltd produces; Glass fibre, the alkali-free milled glass fiber that Nanjing Glass Fibre Research and Design Institute is produced, 150 orders.
Each weight percentages of components of rare-earth modifier is as follows:
Cerium II Chloride 1%; Ethanol 97.27%; Ethylenediamine tetraacetic acid (EDTA) (EDTA) 0.5%; Ammonium chloride 1%; Nitric acid 0.2%; Urea 0.03%.
Earlier glass fibre is carried out pre-treatment, in 550 ℃ of muffle furnaces, ablated 0.5 hour, make its surface organic matter residual quantity below 1%.Adopt above-mentioned rare-earth modifier for treatment then, glass fibre is at room temperature immersed in the properties-correcting agent, soaked 4 hours, after the filtration, oven dry.
To carry out mechanical blending with tetrafluoroethylene molding powder through the mealy glass fibre of rare earth surface modification treatment, feed glass quality of fiber per-cent is 20% of mixed powder, pack in the stainless steel mould, compression moulding on pressing machine, pressure-controlling is about 50MPa, time is 40 minutes, pressurization and stress-relief process slowly carry out, the blank of above-mentioned compression moulding is taken out gently, put into muffle furnace, carry out sintering: slowly be warming up to about 320 ℃ earlier, and then be warming up to about 380 ℃, be incubated 6 hours with 30 ℃/hour speed.
Utilize MMD-10 type end side wear testing machine (production of Jinan trier factory), matrix material is carried out the friction and wear behavior test, and compare with the glass fibre/epoxy composite material of coupling agent treatment, experimental result shows: the tribological property of glass fibre/ptfe composite of handling through rare earth is better than the glass fibre/epoxy composite material of coupling agent treatment.
Embodiment 3:
The raw material that adopts only changes the proportioning of rare-earth modifier: lanthanum trioxide 2% with embodiment 1; Ethanol 96.49%; Ethylenediamine tetraacetic acid (EDTA) (EDTA) 0.25%; Ammonium chloride 0.06%; Nitric acid 0.5%; Urea 0.7%.Earlier glass fibre is carried out pre-treatment, in 530 ℃ of muffle furnaces, ablated 1 hour, make its surface organic matter residual quantity below 1%.Adopt above-mentioned rare-earth modifier for treatment then, glass fibre is at room temperature immersed in the properties-correcting agent, soaked 3 hours, after the filtration, oven dry.
To carry out mechanical blending with tetrafluoroethylene molding powder through the short glass fiber of rare earth surface modification treatment, feed glass quality of fiber per-cent is 30% of mixed powder, pack in the stainless steel mould, compression moulding on pressing machine, pressure-controlling is about 45MPa, time is 50 minutes, pressurization and stress-relief process slowly carry out, the blank of above-mentioned compression moulding is taken out gently, put into muffle furnace, carry out sintering: slowly be warming up to about 320 ℃ earlier, and then be warming up to about 380 ℃, be incubated 6 hours with 30 ℃/hour speed.
Carry out on the MPV200 type that the is determined at friction wear testing machine of matrix material rubbing factor and abrasion loss, before each test, sample and antithesis ring surface acetone (analytical pure) cotton balls scrub.Experimental result: frictional coefficient is less than 0.2, and load is at 300 Newtonian times, and abrasion loss is 150m/mg.
Claims (3)
1, a kind of rare-earth-modified glass-fiber/ptfe composite preparation method, it is characterized in that earlier glass fibre being placed in 500～550 ℃ of muffle furnaces ablating 0.5～1 hour, make its surface organic matter residual quantity below 1%, then glass fibre is at room temperature immersed and soak 2～4 hours in the rare-earth modifier, filter the back oven dry, weak point after handling is cut or mealy glass fibre carries out mechanical blending with the tetrafluoroethylene powder, feed glass quality of fiber per-cent is 10～30% of mixed powder, then mixed powder is put into stainless steel mould, compression moulding on pressing machine, pressure-controlling is at 40～50MPa, time is 30～50 minutes, pressurization and stress-relief process slowly carry out, the blank of above-mentioned compression moulding is put into muffle furnace carry out sintering, slowly be warming up to about 320 ℃ earlier, and then be warming up to about 380 ℃ with 30 ℃/hour speed, be incubated 5～6 hours, be machined into matrix material again, the weight percentages of components of wherein said rare-earth modifier is: rare earth compound 0.1～2%, ethanol 96～99.7%, ethylenediamine tetraacetic acid (EDTA) 0.05～0.5%, ammonium chloride 0.1～1%, nitric acid 0.02～0.5%, urea 0.03～1%.
2, rare-earth-modified glass-fiber as claimed in claim 1/ptfe composite preparation method is characterized in that described rare earth compound is Lanthanum trichloride, Cerium II Chloride, lanthanum trioxide or cerium oxide.
3, rare-earth-modified glass-fiber as claimed in claim 1/ptfe composite preparation method is characterized in that described glass fibre is an alkali free glass fibre, and tetrafluoroethylene is for the employing suspension polymerization and through the broken tetrafluoroethylene powder that forms of fine powder.
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| CNA031416667A CN1487022A (en) | 2003-07-17 | 2003-07-17 | Prepn of RE-modified composite glass fiber/PTFE material |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100439086C (en) * | 2005-12-16 | 2008-12-03 | 广东工业大学 | Preparation method for polytetrafluoroethylene/fiber composite material added with metal oxide |
| CN101781444A (en) * | 2010-03-31 | 2010-07-21 | 上海交通大学 | Method for preparing rare-earth-modified glass-fiber epoxy-resin composite materials |
| CN101768811B (en) * | 2010-02-05 | 2011-08-31 | 东华大学 | Method for preparing polytetrafluoroethylene-based three-dimensional orthogonal composite material |
| CN105314928A (en) * | 2015-12-07 | 2016-02-10 | 苏州市神龙门窗有限公司 | High-temperature-resistant oxidation-resistant roller shutter door and preparation process thereof |
| CN106531932A (en) * | 2016-12-10 | 2017-03-22 | 芜湖航达网业有限公司 | Polymer composite separator for lead acid storage battery and preparation method thereof |
| CN106894292A (en) * | 2017-02-28 | 2017-06-27 | 贺雨晴 | A kind of alkali-free glass fibre filter paper and preparation method thereof |
| CN108285641A (en) * | 2018-02-05 | 2018-07-17 | 公牛集团股份有限公司 | A kind of modified glass-fiber, the nylon composite materials and its preparation method and application containing the modified glass-fiber |
| CN108559208A (en) * | 2018-04-18 | 2018-09-21 | 安徽斯瑞尔阀门有限公司 | A kind of ceramic modified ptfe composite of valve seal nano microcrystalline |
| CN108659410A (en) * | 2017-03-31 | 2018-10-16 | 南京工业大学 | Rare earth modified superfine glass fiber/fluorine-containing polymer composite material and preparation method thereof |
| CN111467877A (en) * | 2020-04-17 | 2020-07-31 | 安徽世倾环保科技有限公司 | Preparation method of filter material of glass fiber composite filter bag with strong cohesive force |
-
2003
- 2003-07-17 CN CNA031416667A patent/CN1487022A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100439086C (en) * | 2005-12-16 | 2008-12-03 | 广东工业大学 | Preparation method for polytetrafluoroethylene/fiber composite material added with metal oxide |
| CN101768811B (en) * | 2010-02-05 | 2011-08-31 | 东华大学 | Method for preparing polytetrafluoroethylene-based three-dimensional orthogonal composite material |
| CN101781444A (en) * | 2010-03-31 | 2010-07-21 | 上海交通大学 | Method for preparing rare-earth-modified glass-fiber epoxy-resin composite materials |
| CN105314928A (en) * | 2015-12-07 | 2016-02-10 | 苏州市神龙门窗有限公司 | High-temperature-resistant oxidation-resistant roller shutter door and preparation process thereof |
| CN106531932A (en) * | 2016-12-10 | 2017-03-22 | 芜湖航达网业有限公司 | Polymer composite separator for lead acid storage battery and preparation method thereof |
| CN106531932B (en) * | 2016-12-10 | 2019-11-12 | 芜湖航达网业有限公司 | A kind of lead-acid accumulator macromolecule composite diaphragm and preparation method thereof |
| CN106894292A (en) * | 2017-02-28 | 2017-06-27 | 贺雨晴 | A kind of alkali-free glass fibre filter paper and preparation method thereof |
| CN106894292B (en) * | 2017-02-28 | 2018-04-24 | 贺雨晴 | A kind of alkali-free glass fibre filter paper and preparation method thereof |
| CN108659410A (en) * | 2017-03-31 | 2018-10-16 | 南京工业大学 | Rare earth modified superfine glass fiber/fluorine-containing polymer composite material and preparation method thereof |
| CN108285641A (en) * | 2018-02-05 | 2018-07-17 | 公牛集团股份有限公司 | A kind of modified glass-fiber, the nylon composite materials and its preparation method and application containing the modified glass-fiber |
| CN108559208A (en) * | 2018-04-18 | 2018-09-21 | 安徽斯瑞尔阀门有限公司 | A kind of ceramic modified ptfe composite of valve seal nano microcrystalline |
| CN111467877A (en) * | 2020-04-17 | 2020-07-31 | 安徽世倾环保科技有限公司 | Preparation method of filter material of glass fiber composite filter bag with strong cohesive force |
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