CN102277733B - Ultra-hydrophobic aramid fiber and preparation method thereof - Google Patents
Ultra-hydrophobic aramid fiber and preparation method thereof Download PDFInfo
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- CN102277733B CN102277733B CN201110167213A CN201110167213A CN102277733B CN 102277733 B CN102277733 B CN 102277733B CN 201110167213 A CN201110167213 A CN 201110167213A CN 201110167213 A CN201110167213 A CN 201110167213A CN 102277733 B CN102277733 B CN 102277733B
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Abstract
The invention relates to a hydrophobic fiber and a preparation method thereof. The invention solves the problem of bad hydrophobicity of the present aramid fiber. The ultra-hydrophobic aramid fiber grows calcium oxalate or tricalcium phosphate crystal on the surface of the aramid fiber, and the preparation method of the ultra-hydrophobic aramid fiber comprises the following steps: adding excess calcium oxalate or tricalcium phosphate in dilute acid to obtain a supersaturated solution, immersing the clean aramid fiber in the supersaturated solution, adding water to the heated supersaturated solution dropwisely, standing, and then drying to obtain the ultra-hydrophobic aramid fiber. Or the ultra-hydrophobic aramid fiber grows trichloro benzene or polystyrene on the surface of the aramid fiber, and the preparation of the ultra-hydrophobic aramid fiber also can comprise the following steps: adding excess trichloro benzene or polystyrene in ethanol to obtain a supersaturated solution, then immersing the clean aramid fiber in the supersaturated solution, heating the supersaturated solution to volatilize ethanol, then drying to obtain the ultra-hydrophobic aramid fiber. The ultra-hydrophobic aramid fiber disclosed in the invention can be used in skin materials of ships and warships.
Description
Technical field
The present invention relates to hydrophobic fiber and preparation method thereof.
Background technology
The aramid fiber full name is " PPTA ", and the commodity of E.I.Du Pont Company are called Kevlar, is novel high-tech synthetic fiber; Have superhigh intensity, high-modulus and high temperature resistant, acid-fast alkali-proof, premium properties such as in light weight, its intensity is 5～6 times of steel wire, and modulus is steel wire or glass fibre 2～3 times; Toughness is 2 times of steel wire, and weight is merely about 1/5 of steel wire, under 560 ℃ temperature; Do not decompose, do not melt.It has good insulation performance property and ageing resistace, has very long life cycle, is widely used in the various aspects of national economy such as space flight and aviation, electromechanics, building, automobile, sports goods.The hydrophobicity of existing aramid fiber is poor, and the contact angle of itself and water is merely 45 °～60 °, has limited the application of aramid fiber in composite.
Summary of the invention
The present invention is the problem for the hydrophobicity difference that solves existing aramid fiber, and super-hydrophobic aramid fiber and preparation method thereof is provided.
Super-hydrophobic aramid fiber of the present invention is that the superficial growth at aramid fiber has calcium oxalate or tricalcium phosphate crystal, and the single fiber surface roughness is 120nm～800nm, and the hydrophobic angle of fibre bundle is 120 °～190 °.
The preparation method of super-hydrophobic aramid fiber of the present invention carries out according to the following steps: one, with aramid fiber with organic solvent extracting 1h～5h, wash then, dry, obtain clean aramid fiber; Two, excessive calcium oxalate or tricalcium phosphate are joined in the dilute acid soln that concentration is 0.1mol/L～2.0mol/L, obtain supersaturated solution; Three, the volume ratio of two supersaturated solutions that obtain and water is that 1: 100～1000 ratio is measured supersaturated solution and the water that step 2 obtains respectively set by step; The supersaturated solution that step 2 is obtained is heated to 90 ℃～300 ℃; The aramid fiber of the cleaning that then step 1 is obtained is immersed in the supersaturated solution; In the cooling water of measuring dropwise being added in the supersaturated solution naturally, after adding, leave standstill 1h～24h; Four, will be placed on through the aramid fiber that step 3 is handled in the baking oven, be under 100 ℃～200 ℃ the condition dry 1～2 hour in temperature, obtains super-hydrophobic aramid fiber.
The present invention is immersed in the aramid fiber of cleaning in the supersaturation acid solution of calcium oxalate or tricalcium phosphate; Through in acid solution, adding water gradually; The infinite dilution dilute acid soln, thus water-fast calcium oxalate or tricalcium phosphate are separated out gradually, and be able to growth at fiber surface.Add the amount of entry and add the amount of separating out that water speed is controlled calcium oxalate or tricalcium phosphate through control, thereby control comes the fiber surface roughness.The surface roughness of the super-hydrophobic aramid fiber that the present invention obtains is 120nm～800nm, and the hydrophobic angle of fibre bundle is 120 °～190 °.Super-hydrophobic aramid fiber of the present invention can be widely used in the skin material on boats and ships, naval vessel.Its application in boats and ships can reduce Ship Resistance, increase ship buoyance, improves the operational efficiency of boats and ships.
Super-hydrophobic aramid fiber of the present invention is that the superficial growth at aramid fiber has trichloro-benzenes or polystyrene, and the single fiber surface roughness is 200nm～2000nm, and the hydrophobic angle of fibre bundle is 150 °～190 °.
The preparation method of super-hydrophobic aramid fiber of the present invention can also carry out according to the following steps: one, with aramid fiber with organic solvent extracting 1h～5h, wash then, dry, obtain clean aramid fiber; Two, excessive trichloro-benzenes or polystyrene are joined in the ethanol, obtain supersaturated solution; Three, the aramid fiber of the cleaning that obtains of step 1 immerses in the supersaturated solution, and the heating supersaturated solution volatilizees ethanol fully; Four, will be placed on through the aramid fiber that step 3 is handled in the baking oven, be dry 0.5h～2h under 50 ℃～150 ℃ the condition in temperature, obtains super-hydrophobic aramid fiber.
The present invention is immersed in the aramid fiber of cleaning in the supersaturated solution of trichloro-benzenes or polystyrene, through the evaporation rate of control etoh solvent, thereby trichloro-benzenes or polystyrene is separated out gradually, and is able to growth at fiber surface.Through control trichloro-benzenes or the addition of polystyrene and the evaporation rate of solvent, reach the purpose of controlling fiber surface roughness.The surface roughness of the super-hydrophobic aramid fiber that the present invention obtains is 200nm～2000nm, and the hydrophobic angle of fibre bundle is 150 °～190 °.Super-hydrophobic aramid fiber of the present invention can be widely used in the skin material on boats and ships, naval vessel.Its application in boats and ships can reduce Ship Resistance, increase ship buoyance, improves the operational efficiency of boats and ships.
Description of drawings
Fig. 1 is the hydrophobic angle photo of the super-hydrophobic aramid fiber of the specific embodiment 19 preparations.
The specific embodiment
The specific embodiment one: the super-hydrophobic aramid fiber of this embodiment is that the superficial growth at aramid fiber has calcium oxalate or tricalcium phosphate crystal, and the single fiber surface roughness is 120nm～800nm, and the hydrophobic angle of fibre bundle is 120 °～190 °.
The specific embodiment two: this embodiment and the specific embodiment one are different is that the single fiber surface roughness of aramid fiber is 200nm～700nm, and the hydrophobic angle of fibre bundle is 130 °～180 °.Other is identical with the specific embodiment one.
The specific embodiment three: this embodiment and the specific embodiment one are different is that the single fiber surface roughness of aramid fiber is 400nm, and the hydrophobic angle of fibre bundle is 160 °.Other is identical with the specific embodiment one.
The specific embodiment four: the preparation method of the super-hydrophobic aramid fiber of this embodiment carries out according to the following steps: one, with aramid fiber with organic solvent extracting 1h～5h, wash then, dry, obtain clean aramid fiber; Two, excessive calcium oxalate or tricalcium phosphate are joined in the dilute acid soln that concentration is 0.1mol/L～2.0mol/L, obtain supersaturated solution; Three, the volume ratio of two supersaturated solutions that obtain and water is that 1: 100～1000 ratio is measured supersaturated solution and the water that step 2 obtains respectively set by step; The supersaturated solution that step 2 is obtained is heated to 90 ℃～300 ℃; The aramid fiber of the cleaning that then step 1 is obtained is immersed in the supersaturated solution; In the cooling water of measuring dropwise being added in the supersaturated solution naturally, after adding, leave standstill 1h～24h; Four, will be placed on through the aramid fiber that step 3 is handled in the baking oven, be under 100 ℃～200 ℃ the condition dry 1～2 hour in temperature, obtains super-hydrophobic aramid fiber.
This embodiment is immersed in the aramid fiber of cleaning in the supersaturation acid solution of calcium oxalate or tricalcium phosphate; Through in acid solution, adding water gradually; The infinite dilution dilute acid soln, thus water-fast calcium oxalate or tricalcium phosphate are separated out gradually, and be able to growth at fiber surface.Add the amount of entry and add the amount of separating out that water speed is controlled calcium oxalate or tricalcium phosphate through control, thereby control comes the fiber surface roughness.The surface roughness of the super-hydrophobic aramid fiber that the present invention obtains is 120nm～800nm, and the hydrophobic angle of fibre bundle is 120 °～190 °, and the preparation method is simple.
The specific embodiment five: what this embodiment and the specific embodiment four were different is: the organic solvent in the step 1 is water or organic solvent, as: toluene, ethanol, acetone or oxolane.Other is identical with the specific embodiment four.
The specific embodiment six: what this embodiment was different with the specific embodiment four or five is: in the step 1 with aramid fiber with organic solvent extracting 1.5h～4.5h.Other is identical with the specific embodiment four or five.
The specific embodiment seven: what this embodiment was different with the specific embodiment four or five is: in the step 1 with aramid fiber with organic solvent extracting 3h.Other is identical with the specific embodiment four or five.
The specific embodiment eight: what this embodiment was different with one of specific embodiment four to seven is: dilute acid soln is hydrochloric acid solution or salpeter solution in the step 2.Other is identical with one of specific embodiment four to seven.
The specific embodiment nine: what this embodiment was different with one of specific embodiment four to eight is: the concentration of dilute acid soln is 0.3mol/L～1.8mol/L in the step 2.Other is identical with one of specific embodiment four to eight.
The specific embodiment ten: what this embodiment was different with one of specific embodiment four to eight is: the concentration of dilute acid soln is 1.0mol/L in the step 2.Other is identical with one of specific embodiment four to eight.
The specific embodiment 11: what this embodiment was different with one of specific embodiment four to ten is: the volume ratio of supersaturated solution and water is 1: 150～900 in the step 3.Other is identical with one of specific embodiment four to ten.
The specific embodiment 12: what this embodiment was different with one of specific embodiment four to ten is: the volume ratio of supersaturated solution and water is 1: 500 in the step 3.Other is identical with one of specific embodiment four to ten.
The specific embodiment 13: what this embodiment was different with one of specific embodiment four to 12 is: supersaturated solution is heated to 120 ℃～280 ℃ in the step 3.Other is identical with one of specific embodiment four to 12.
The specific embodiment 14: what this embodiment was different with one of specific embodiment four to 12 is: supersaturated solution is heated to 200 ℃ in the step 3.Other is identical with one of specific embodiment four to 12.
The specific embodiment 15: what this embodiment was different with one of specific embodiment four to 14 is: time of repose is 3h～20h in the step 3.Other is identical with one of specific embodiment four to 14.
The specific embodiment 16: what this embodiment was different with one of specific embodiment four to 14 is: time of repose is 10h in the step 3.Other is identical with one of specific embodiment four to 14.
The specific embodiment 17: what this embodiment was different with one of specific embodiment four to 16 is: baking temperature is that 120 ℃～180 ℃, drying time are 1.2h～1.8h in the step 4.Other is identical with one of specific embodiment four to 16.
The specific embodiment 18: what this embodiment was different with one of specific embodiment four to 16 is: baking temperature is that 150 ℃, drying time are 1.5h in the step 4.Other is identical with one of specific embodiment four to 16.
The specific embodiment 19: the preparation method of the super-hydrophobic aramid fiber of this embodiment carries out according to the following steps: one, with aramid fiber with toluene extracting 2h, wash then, dry, obtain clean aramid fiber; Two, excessive calcium oxalate or tricalcium phosphate are joined in the dilute nitric acid solution that concentration is 1.5mol/L, obtain supersaturated solution; Three, the volume ratio of two supersaturated solutions that obtain and water is that 1: 700 ratio is measured supersaturated solution and the water that step 2 obtains respectively set by step; The supersaturated solution that step 2 is obtained is heated to 90 ℃; The aramid fiber of the cleaning that then step 1 is obtained is immersed in the supersaturated solution; In the cooling water of measuring dropwise being added in the supersaturated solution naturally, after adding, leave standstill 12h; Four, will be placed on through the aramid fiber that step 3 is handled in the baking oven, be under 150 ℃ the condition dry 2 hours in temperature, obtains super-hydrophobic aramid fiber.
The hydrophobic angle photo of the super-hydrophobic aramid fiber that this embodiment obtains is as shown in Figure 1, and the hydrophobic angle that can obtain super-hydrophobic aramid fiber from Fig. 1 is 155 °, has excellent hydrophobic property.The preparation method is simple.
The specific embodiment 20: the super-hydrophobic aramid fiber of this embodiment is that the superficial growth at aramid fiber has trichloro-benzenes or polystyrene, and the single fiber surface roughness is 200nm～2000nm, and the hydrophobic angle of fibre bundle is 150 °～190 °.
The specific embodiment 21: what this embodiment and the specific embodiment 20 were different is that aramid fiber single fiber surface roughness is 220nm～1800nm, and the hydrophobic angle of fibre bundle is 160 °～180 °.Other is identical with the specific embodiment 20.
The specific embodiment 22: what this embodiment and the specific embodiment 20 were different is that aramid fiber single fiber surface roughness is 1000nm, and the hydrophobic angle of fibre bundle is 170 °.Other is identical with the specific embodiment 20.
The specific embodiment 23: the preparation method of the super-hydrophobic aramid fiber of this embodiment can also carry out according to the following steps: one, with aramid fiber with organic solvent extracting 1h～5h, wash then, dry, obtain clean aramid fiber; Two, excessive trichloro-benzenes or polystyrene are joined in the ethanol, obtain supersaturated solution; Three, the aramid fiber of the cleaning that obtains of step 1 immerses in the supersaturated solution, and the heating supersaturated solution volatilizees ethanol fully; Four, will be placed on through the aramid fiber that step 3 is handled in the baking oven, be dry 0.5h～2h under 50 ℃～150 ℃ the condition in temperature, obtains super-hydrophobic aramid fiber.
This embodiment is immersed in the aramid fiber of cleaning in the supersaturated solution of trichloro-benzenes or polystyrene, through the evaporation rate of control etoh solvent, thereby trichloro-benzenes or polystyrene is separated out gradually, and is able to growth at fiber surface.Through control trichloro-benzenes or the addition of polystyrene and the evaporation rate of solvent, reach the purpose of controlling fiber surface roughness.The surface roughness of the super-hydrophobic aramid fiber that this embodiment obtains is 200nm～2000nm, and the hydrophobic angle of fibre bundle is 150 °～190 °.The preparation method is simple.
The specific embodiment 24: what this embodiment and the specific embodiment 23 were different is: the organic solvent in the step 1 is toluene, ethanol, acetone or oxolane.Other is identical with the specific embodiment 23.
The specific embodiment 25: what this embodiment was different with the specific embodiment 23 or 24 is: aramid fiber is with organic solvent extracting 1.5h～4.5h in the step 1.Other is identical with the specific embodiment 23 or 24.
The specific embodiment 26: what this embodiment was different with the specific embodiment 23 or 24 is: aramid fiber is with organic solvent extracting 3h in the step 1.Other is identical with the specific embodiment 23 or 24.
The specific embodiment 27: what this embodiment was different with the specific embodiment 23 or 26 is: baking temperature is that 60 ℃～140 ℃, drying time are 0.8h～1.8h in the step 4.Other and the specific embodiment 23 or 20 six phases with.
The specific embodiment 28: what this embodiment was different with the specific embodiment 23 or 26 is: baking temperature is that 100 ℃, drying time are 1.0h in the step 4.Other and the specific embodiment 23 or 20 six phases with.
The specific embodiment 29: the preparation method of the super-hydrophobic aramid fiber of this embodiment also carries out according to the following steps: one, with aramid fiber with toluene extracting 4h, wash then, dry, obtain clean aramid fiber; Two, excessive trichloro-benzenes is joined in the ethanol, obtain supersaturated solution; Three, the aramid fiber of the cleaning that obtains of step 1 immerses in the supersaturated solution that step 2 obtains, and the heating supersaturated solution volatilizees ethanol fully; Four, will be placed on through the aramid fiber that step 3 is handled in the baking oven, be under 110 ℃ the condition dry 2 hours in temperature, obtains super-hydrophobic aramid fiber.
It is 1250nm that the super-hydrophobic aramid fiber surface growth that this embodiment obtains has trichloro-benzenes, single fiber surface roughness, and the hydrophobic angle of fibre bundle is 170 °.The preparation method is simple.
Claims (6)
1. super-hydrophobic aramid fiber is characterized in that super-hydrophobic aramid fiber is that superficial growth at aramid fiber has calcium oxalate or tricalcium phosphate crystal, and the single fiber surface roughness is 120nm～800nm, and the hydrophobic angle of fibre bundle is 120 °～190 °.
2. super-hydrophobic aramid fiber according to claim 1, the single fiber surface roughness that it is characterized in that aramid fiber is 200nm～700nm, the hydrophobic angle of fibre bundle is 130 °～180 °.
3. the preparation method of super-hydrophobic aramid fiber as claimed in claim 1; The preparation method who it is characterized in that super-hydrophobic aramid fiber carries out according to the following steps: one, with aramid fiber with organic solvent extracting 1h～5h; Wash then, dry, obtain clean aramid fiber; Two, excessive calcium oxalate or tricalcium phosphate are joined in the dilute acid soln that concentration is 0.1mol/L～2.0mol/L, obtain supersaturated solution; Three, the volume ratio of two supersaturated solutions that obtain and water is that 1: 100～1000 ratio is measured supersaturated solution and the water that step 2 obtains respectively set by step; The supersaturated solution that step 2 is obtained is heated to 90 ℃～300 ℃; The aramid fiber of the cleaning that then step 1 is obtained is immersed in the supersaturated solution; In the cooling water of measuring dropwise being added in the supersaturated solution naturally, after adding, leave standstill 1h～24h; Four, will be placed on through the aramid fiber that step 3 is handled in the baking oven, be under 100 ℃～200 ℃ the condition dry 1～2 hour in temperature, obtains super-hydrophobic aramid fiber; Dilute acid soln is hydrochloric acid solution or salpeter solution in the step 2.
4. the preparation method of super-hydrophobic aramid fiber according to claim 3 is characterized in that the organic solvent in the step 1 is toluene, ethanol, acetone or oxolane.
5. according to the preparation method of claim 3 or 4 described super-hydrophobic aramid fibers, it is characterized in that in the tool step 1 with aramid fiber with organic solvent extracting 1.5h～4.5h.
6. according to the preparation method of claim 3 or 4 described super-hydrophobic aramid fibers, the concentration that it is characterized in that dilute acid soln in the step 2 is 0.3mol/L～1.8mol/L.
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| CN105297402A (en) * | 2015-10-16 | 2016-02-03 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method for growing hydroxyapatite on surface of hydrophobic fiber |
| CN108930074A (en) * | 2018-07-16 | 2018-12-04 | 苏州联畅特种纤维有限公司 | A kind of preparation process of superhydrophobic fibers |
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| CN102039984A (en) * | 2010-11-23 | 2011-05-04 | 哈尔滨工业大学 | Super-buoyancy superhydrophobic aramid fiber bundle ship and manufacturing method thereof |
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| JP2003105195A (en) * | 2001-09-27 | 2003-04-09 | Toyobo Co Ltd | Aromatic polyamide coated with calcium phosphate compound and method for producing the same |
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| CN101157766A (en) * | 2007-11-23 | 2008-04-09 | 中南林业科技大学 | Super-hydrophobic polystyrene film and preparation method thereof |
| CN101575798A (en) * | 2008-12-19 | 2009-11-11 | 东华大学 | Method for modifying Kevlar fiber by treating nano sol through plasma |
| CN102039984A (en) * | 2010-11-23 | 2011-05-04 | 哈尔滨工业大学 | Super-buoyancy superhydrophobic aramid fiber bundle ship and manufacturing method thereof |
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