CN1558015A - Fiber material surface nanocrystalline processing method - Google Patents
Fiber material surface nanocrystalline processing method Download PDFInfo
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- CN1558015A CN1558015A CNA2004100121356A CN200410012135A CN1558015A CN 1558015 A CN1558015 A CN 1558015A CN A2004100121356 A CNA2004100121356 A CN A2004100121356A CN 200410012135 A CN200410012135 A CN 200410012135A CN 1558015 A CN1558015 A CN 1558015A
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Abstract
The nano fiber material surface treating process includes compounding solution as coating material precursor, soaking the fiber material to be treated inside the solution for adsorbing the precursor homogeneously, regulating pH value, setting in constant temperature water bath to form 20-100 nm thick film coating the fiber, softening treatment and stoving. The SEM analysis shows that the surface nano layer is homogeneous and has good coating effect, the treated fiber has strength, hand feeling and brightness superior to the un-treated fiber. The treated fiber has far infrared function, antibiotic function, anti-ultraviolet function, etc. depending on the coated matter.
Description
Technical field
The present invention relates to a kind of fiber-like material surface treatment method, especially a kind of method of fibrous material Surface Nanocrystalline.
Background technology
The textile industry fiber-like material is as wool, cotton and various chemical fibre.The applying nano technology makes it have functional textile product to its surface treatment, as waterproof, antifouling, saturating wet environmental protection clothes, emitting far-infrared health clothing, and have antiultraviolet, fungi-proofing, anion, suction ripple, antistatic, photocatalysis etc., existing have fiber-like material surface-treated method: surface parcel polymerization, its objective is the sorbent that makes single stable, its method is at fiber-like material surface parcel polymer; Surface modification is that performance change is carried out on the surface of fiber-like material, makes gloss, feel, the intensity of fiber surface reach some specific functions, satisfies certain purposes.But existing fiber-like material surface-treated method, employing be the mode of wrappage surface absorption, main deficiency be wrappage with fibrous material between combine insecure, wash resistant not, washing times increases, and surperficial institute decorative material easily comes off, and loses its good performance.
Summary of the invention
The technical problem to be solved in the present invention is to the fibrous material Surface Nanocrystalline, it is become have multi-functional product, and purpose is to explore this material surface nanometer processing method, thereby a kind of fibrous material Surface Nanocrystalline method is provided.
The present invention is that proportion by the wrappage precursor prepares solution to the method for fibrous material Surface Nanocrystalline, and in solution, soak desire with the fibrous material of handling, make the full and uniform fiber substance surface that is adsorbed on of precursor, regulate the pH value, putting into water bath with thermostatic control again reacts, make wrappage be grown directly upon fiber surface, dry behind formation 2~100nm film.
Its concrete grammar is undertaken by following processing step successively:
(1) proportion by wrappage precursor 1%~5%, OP emulsifying agent 5%~20%, distilled water 75%~94% prepares solution;
(2) fibrous material that desire is handled is in above-mentioned solution, soaked at normal temperatures 30~60 minutes, make the full and uniform fiber substance surface that is adsorbed on of precursor, bath raio is 1: 20~80, with pH value conditioning agent regulator solution pH value in 2~12 scope, put into water bath with thermostatic control, 30 ℃~95 ℃ of reaction temperatures in 1~5 hour reaction time, make wrappage be grown directly upon the fibrous matter surface, form one deck nanometer film, thickness is 20~100nm;
(3) fibrous material after the above-mentioned Surface Nanocrystalline is put into baking oven after soft treatment, be incubated 1.5~3 hours down, dry processing at 60 ℃~120 ℃.
Wherein: described fibrous material is wool or cotton or silk or acrylic or terylene; Described wrappage is SiO
2Or ZnO or TiO
2Or ZrO
2Or Al
2O
3Described wrappage precursor is TEOS or Zn (CH
3COO)
2Or Zr (OR)
4Or TiCl
4Or Al (OR)
3Described pH value conditioning agent is hydrochloric acid or oxalic acid or ammoniacal liquor or sodium bicarbonate;
Above ratio range is percent by volume.
Fibrous material Surface Nanocrystalline method of the present invention, the mode that adopts its wrappage growth in situ is in the even growth in the surface of fibrous material one deck nanometer film, compared with prior art, integument combines with fiber firmly, difficult drop-off, wash resistant, after 25 washings, 85% before the content of wrappage is not less than and washs; Can find out that through sem analysis surface nanometer layer is even, wrap up respond well.This method equipment, technical process are simple, and cost is low, and before the fiber of handling, intensity, feel, gloss all are better than handling, and according to the difference of wrappage, fiber has different functions, as: wrappage is SiO
2, TiO
2, ZrO
2And Al
2O
3The time, fiber has far-infrared functional; When wrappage was ZnO, fiber had antibacterial functions; ZnO, TiO
2The time, fiber has anti-ultraviolet function or the like.
Description of drawings
Fig. 1 is a wool SEM photo after the preliminary treatment, and its surface ratio is more coarse, and scale is outstanding.
Fig. 2 is the SEM photo that nanometer is handled the back wool, and its surface is smooth relatively.
The specific embodiment
Embodiment 1
Ratio in TEOS 0.5ml, OP emulsifying agent 2.5ml, distilled water 47ml prepares solution, with pretreated wool 0.75g in above-mentioned solution, soaked at normal temperatures 30 minutes, make the full and uniform wool surface that is adsorbed on of precursor, pH value conditioning agent hydrochloric acid, regulator solution pH value is in 2 scope; Put into water bath with thermostatic control, 30 ℃ of reaction temperatures, 5 hours reaction time, make to be reflected in the wool and carry out, make SiO
2Be grown directly upon the wool surface; To put into baking oven after the processing of the adding of the wool after above-mentioned Surface Nanocrystalline softener, be incubated 3 hours down, dry processing at 60 ℃, even one deck nanometer film of growing on the wool surface, thickness is about 20nm.
Embodiment 2
Ratio in TEOS 2.5ml, OP emulsifying agent 10ml, distilled water 37.5ml prepares solution, with pretreated wool 2.5g in above-mentioned solution, soaked at normal temperatures 60 minutes, and made the full and uniform wool surface that is adsorbed on of precursor, pH value conditioning agent oxalic acid, regulator solution pH value is in 5 scope, put into water bath with thermostatic control, 95 ℃ of reaction temperatures, 1 hour reaction time, make to be reflected at the wool surface and to carry out, make SiO
2Be grown directly upon the wool surface, the wool after the above-mentioned Surface Nanocrystalline added put into baking oven after softener is handled, be incubated 1.5 hours down at 120 ℃, dry processing, in surperficial evenly growth one deck nanometer film of wool, thickness is about 100nm.
Embodiment 3
Press TEOS 1.5ml, OP emulsifying agent 5ml, distilled water H
2The ratio of O 43.5ml prepares solution, with pretreated wool 1.5g in above-mentioned solution, soaked at normal temperatures 45 minutes, and made the full and uniform wool surface that is adsorbed on of precursor, pH value conditioning agent hydrochloric acid, regulator solution pH value is in 3.5 scope, put into water bath with thermostatic control, 65 ℃ of reaction temperatures, 2 hours reaction time, make to be reflected at the wool surface and to carry out, make SiO
2Be grown directly upon the wool surface, the wool after the above-mentioned Surface Nanocrystalline added put into baking oven after softener is handled, be incubated 2 hours down at 80 ℃, dry processing, in surperficial evenly growth one deck nanometer film of fibrous material, thickness is about 55nm.
Embodiment 4
According to the method for embodiment 1,2,3, can handle acrylic, silk, cotton and terylene surface equally.
Embodiment 5
Press zirconium-n-propylate Zr (OC
3H
7)
40.5ml, the ratio of OP emulsifying agent 2.5ml, distilled water 47ml prepares solution, pretreated wool 0.75g in above-mentioned solution, was soaked 30 minutes at normal temperatures, make the full and uniform wool surface that is adsorbed on of precursor, pH value conditioning agent hydrochloric acid, regulator solution pH value is in 2 scope; Put into water bath with thermostatic control, 30 ℃ of reaction temperatures, 5 hours reaction time, make to be reflected in the wool and carry out, make ZrO
2Be grown directly upon the wool surface; To put into baking oven after the processing of the adding of the wool after above-mentioned Surface Nanocrystalline softener, be incubated 3 hours down, dry processing at 60 ℃, even one deck nanometer film of growing on the wool surface, thickness is about 20nm.
Embodiment 6
Press zirconium-n-propylate Zr (OC
3H
7)
42.5ml, the ratio of OP emulsifying agent 10ml, distilled water 37.5ml prepares solution, with pretreated wool 2.5g in above-mentioned solution, soaked at normal temperatures 60 minutes, and made the full and uniform wool surface that is adsorbed on of precursor, pH value conditioning agent oxalic acid, regulator solution pH value is in 5 scope, put into water bath with thermostatic control, 95 ℃ of reaction temperatures, 1 hour reaction time, make to be reflected at the wool surface and to carry out, make ZrO
2Be grown directly upon the wool surface, the wool after the above-mentioned Surface Nanocrystalline added put into baking oven after softener is handled, be incubated 1.5 hours down at 120 ℃, dry processing, in surperficial evenly growth one deck nanometer film of wool, thickness is about 100nm.
Embodiment 7
Press zirconium-n-propylate Zr (OC
3H
7)
41.5ml, OP emulsifying agent 5ml, distilled water H
2The ratio of O 43.5ml prepares solution, with pretreated wool 1.5g in above-mentioned solution, soaked at normal temperatures 45 minutes, and made the full and uniform wool surface that is adsorbed on of precursor, pH value conditioning agent hydrochloric acid, regulator solution pH value is in 3.5 scope, put into water bath with thermostatic control, 60 ℃ of reaction temperatures, 2 hours reaction time, make to be reflected at the wool surface and to carry out, make ZrO
2Be grown directly upon the wool surface, the wool after the above-mentioned Surface Nanocrystalline added put into baking oven after softener is handled, be incubated 2 hours down at 80 ℃, dry processing, in surperficial evenly growth one deck nanometer film of fibrous material, thickness is about 55nm.
Embodiment 8
According to the method for embodiment 5,6,7, can carry out surface treatment to acrylic, silk, cotton and terylene equally.
Embodiment 9
Press titanium tetrachloride TiCl
40.5ml, the ratio of OP emulsifying agent 2.5ml, distilled water 47ml prepares solution, pretreated wool 0.75g in above-mentioned solution, was soaked 30 minutes at normal temperatures, make the full and uniform wool surface that is adsorbed on of precursor, pH value conditioning agent hydrochloric acid, regulator solution pH value is in 2 scope; Put into water bath with thermostatic control, 30 ℃ of reaction temperatures, 5 hours reaction time, make to be reflected in the wool and carry out, make TiO
2Be grown directly upon the wool surface; To put into baking oven after the processing of the adding of the wool after above-mentioned Surface Nanocrystalline softener, be incubated 3 hours down, dry processing at 60 ℃, even one deck nanometer film of growing on the wool surface, thickness is about 20nm.
Embodiment 10
Press titanium tetrachloride TiCl
42.5ml, the ratio of OP emulsifying agent 10ml, distilled water 37.5ml prepares solution, with pretreated wool 2.5g in above-mentioned solution, soaked at normal temperatures 60 minutes, and made the full and uniform wool surface that is adsorbed on of precursor, pH value conditioning agent oxalic acid, regulator solution pH value is in 5 scope, put into water bath with thermostatic control, 95 ℃ of reaction temperatures, 1 hour reaction time, make to be reflected at the wool surface and to carry out, make TiO
2Be grown directly upon the wool surface, the wool after the above-mentioned Surface Nanocrystalline added put into baking oven after softener is handled, be incubated 1.5 hours down at 120 ℃, dry processing, in surperficial evenly growth one deck nanometer film of wool, thickness is about 100nm.
Embodiment 11
Press titanium tetrachloride TiCl
41.5ml, OP emulsifying agent 5ml, distilled water H
2The ratio of O 43.5ml prepares solution, with pretreated wool 1.5g in above-mentioned solution, soaked at normal temperatures 45 minutes, and made the full and uniform wool surface that is adsorbed on of precursor, pH value conditioning agent hydrochloric acid, regulator solution pH value is in 3 scope, put into water bath with thermostatic control, 45 ℃ of reaction temperatures, 2 hours reaction time, make to be reflected at the wool surface and to carry out, make TiO
2Be grown directly upon the wool surface, the wool after the above-mentioned Surface Nanocrystalline added put into baking oven after softener is handled, be incubated 2 hours down at 80 ℃, dry processing, in surperficial evenly growth one deck nanometer film of fibrous material, thickness is about 55nm.
Embodiment 12
According to the method for embodiment 9,10,11, can carry out surface treatment to acrylic, silk, cotton and terylene equally.
Embodiment 13
Press aluminium isopropoxide Al (OC
3H
7)
30.5ml, the ratio of OP emulsifying agent 2.5ml, distilled water 47ml prepares solution, pretreated wool 0.75g in above-mentioned solution, was soaked 30 minutes at normal temperatures, make the full and uniform wool surface that is adsorbed on of precursor, pH value conditioning agent hydrochloric acid, regulator solution pH value is in 2 scope; Put into water bath with thermostatic control, 30 ℃ of reaction temperatures, 5 hours reaction time, make to be reflected in the wool and carry out, make Al
2O
3Be grown directly upon the wool surface; To put into baking oven after the processing of the adding of the wool after above-mentioned Surface Nanocrystalline softener, be incubated 3 hours down, dry processing at 60 ℃, even one deck nanometer film of growing on the wool surface, thickness is about 20nm.
Embodiment 14
Press aluminium isopropoxide Al (OC
3H
7)
32.5ml, the ratio of OP emulsifying agent 10ml, distilled water 37.5ml prepares solution, with pretreated wool 2.5g in above-mentioned solution, soaked at normal temperatures 60 minutes, and made the full and uniform wool surface that is adsorbed on of precursor, pH value conditioning agent oxalic acid, regulator solution pH value is in 5 scope, put into water bath with thermostatic control, 95 ℃ of reaction temperatures, 1 hour reaction time, make to be reflected at the wool surface and to carry out, make Al
2O
3Be grown directly upon the wool surface, the wool after the above-mentioned Surface Nanocrystalline added put into baking oven after softener is handled, be incubated 1.5 hours down at 120 ℃, dry processing, in surperficial evenly growth one deck nanometer film of wool, thickness is about 100nm.
Embodiment 15
Press aluminium isopropoxide Al (OC
3H
7)
31.5ml, OP emulsifying agent 5ml, distilled water H
2The ratio of O 43.5ml prepares solution, with pretreated wool 2g in above-mentioned solution, soaked at normal temperatures 45 minutes, and made the full and uniform wool surface that is adsorbed on of precursor, pH value conditioning agent oxalic acid, regulator solution pH value is in 3 scope, put into water bath with thermostatic control, 75 ℃ of reaction temperatures, 2 hours reaction time, make to be reflected at the wool surface and to carry out, make Al
2O
3Be grown directly upon the wool surface, the wool after the above-mentioned Surface Nanocrystalline added put into baking oven after softener is handled, be incubated 2 hours down at 80 ℃, dry processing, in surperficial evenly growth one deck nanometer film of fibrous material, thickness is about 55nm.
Embodiment 16
According to the method for embodiment 13,14,15, can carry out surface treatment to acrylic, silk, cotton and terylene equally.
Embodiment 17
Press zinc acetate Zn (CH
3COO)
20.5ml, the ratio of OP emulsifying agent 2.5ml, distilled water 47ml prepares solution, with pretreated wool 0.75g in above-mentioned solution, soaked at normal temperatures 30 minutes, make the full and uniform wool surface that is adsorbed on of precursor, pH value conditioning agent sodium bicarbonate, regulator solution pH value is in 12 scope; Put into water bath with thermostatic control, 30 ℃ of reaction temperatures, 5 hours reaction time, make to be reflected in the wool and carry out, make ZnO be grown directly upon the wool surface; To put into baking oven after the processing of the adding of the wool after above-mentioned Surface Nanocrystalline softener, be incubated 3 hours down, dry processing at 60 ℃, even one deck nanometer film of growing on the wool surface, thickness is about 20nm.
Embodiment 18
Press zinc acetate Zn (CH
3COO)
22.5ml, OP emulsifying agent 10ml, the ratio of distilled water 37.5ml prepares solution, with pretreated wool 2.5g in above-mentioned solution, soaked at normal temperatures 60 minutes, make the full and uniform wool surface that is adsorbed on of precursor, pH value conditioning agent ammoniacal liquor, regulator solution pH value is put into water bath with thermostatic control in 9 scope, 95 ℃ of reaction temperatures, 1 hour reaction time, make to be reflected at the wool surface and to carry out, make ZnO be grown directly upon the wool surface, will the wool after the above-mentioned Surface Nanocrystalline add and put into baking oven after softener is handled, be incubated 1.5 hours down at 120 ℃, dry processing, one deck nanometer film of evenly growing on the surface of wool, thickness is about 100nm.
Embodiment 19
Press zinc acetate Zn (CH
3COO)
22ml, OP emulsifying agent 5ml, distilled water H
2The ratio of O 43ml prepares solution, with pretreated wool 1.5g in above-mentioned solution, soaked at normal temperatures 45 minutes, make the full and uniform wool surface that is adsorbed on of precursor, pH value conditioning agent ammoniacal liquor, regulator solution pH value is put into water bath with thermostatic control in 10 scope, 60 ℃ of reaction temperatures, 2 hours reaction time, make to be reflected at the wool surface and to carry out, make ZnO be grown directly upon the wool surface, will the wool after the above-mentioned Surface Nanocrystalline add and put into baking oven after softener is handled, be incubated 2 hours down at 80 ℃, dry processing, one deck nanometer film of evenly growing on the surface of fibrous material, thickness is about 55nm.
Embodiment 20
According to the method for embodiment 17,18,19, can carry out surface treatment to acrylic, silk, cotton and terylene equally.
Claims (6)
1. fibrous material Surface Nanocrystalline method, its method is that the proportion by the wrappage precursor prepares solution, and in solution, soak desire with the fibrous material of handling, make the full and uniform fiber substance surface that is adsorbed on of precursor, regulate the pH value, put into water bath with thermostatic control again and react, make wrappage be grown directly upon fiber surface, dry behind formation 2~100nm film.
2. fibrous material Surface Nanocrystalline method according to claim 1, this method is undertaken by following processing step successively:
(1) proportion by wrappage precursor 1%~5%, OP emulsifying agent 5%~20%, distilled water 75%~94% prepares solution;
(2) fibrous material that desire is handled is in above-mentioned solution, soaked at normal temperatures 30~60 minutes, make the full and uniform fiber substance surface that is adsorbed on of precursor, bath raio is 1: 20~80, with pH value conditioning agent regulator solution pH value in 2~12 scope, put into water bath with thermostatic control, 30 ℃~95 ℃ of reaction temperatures in 1~5 hour reaction time, make wrappage be grown directly upon the fibrous matter surface, form one deck nanometer film, thickness is 2~100nm;
(3) fibrous material after the above-mentioned Surface Nanocrystalline is put into baking oven after soft treatment, be incubated 1.5~3 hours down, dry processing at 60 ℃~120 ℃.
Ratio range in the above processing step is percent by volume.
3. fibrous material Surface Nanocrystalline method according to claim 2, the fibrous material described in this method are wool or cotton or silk or acrylic or terylene;
4. fibrous material Surface Nanocrystalline method according to claim 2, the wrappage described in this method is SiO
2Or ZnO or TiO
2Or ZrO
2Or Al
2O3;
5. fibrous material Surface Nanocrystalline method according to claim 2, the wrappage precursor described in this method are TEOS or Zn (CH
3COO)
2Or Zr (OR)
4Or TiCl
4Or Al (OR)
3
6. fibrous material Surface Nanocrystalline method according to claim 2, the pH value conditioning agent described in this method can be hydrochloric acid or oxalic acid or ammoniacal liquor or sodium bicarbonate.
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