CN1240894C - Fiber material surface nanocrystalline processing method - Google Patents
Fiber material surface nanocrystalline processing method Download PDFInfo
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- CN1240894C CN1240894C CN 200410012135 CN200410012135A CN1240894C CN 1240894 C CN1240894 C CN 1240894C CN 200410012135 CN200410012135 CN 200410012135 CN 200410012135 A CN200410012135 A CN 200410012135A CN 1240894 C CN1240894 C CN 1240894C
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Abstract
The present invention discloses a fiber material surface nanometer crystallization treatment method which comprises: a solution is prepared according to the ratio of coating substance precursors; fiber materials to be treated are soaked in the prepared solution, which enables the precursors to be sufficiently and uniformly adsorbed on the surfaces of the fiber materials; the pH value of the solution is regulated, and then, the solution is put in thermostatic water bath for reacting, which enables the coating substances to directly grow on the surfaces of the fiber materials to form films with the thickness of 20 to 100 nm; finally, the fiber materials which are nanometer crystallized are dried through softening treatment. Shown by SEM analysis, surface nanometer layers are homogeneous, coating effects are good and treated fibre strength, hand feelings and luster are all superior to that before treatment. The surface nanometer layers also have the advantages of firm combination and washing resistance, and after being washed for 25 times, the content of the coating substances is not lower than 85% that before washing. According to different coating substances, the fibers can have far infrared functions, antibacterial functions, ultraviolet ray resistance functions, etc., which is practical to the surface treatment of fiber class materials.
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 fibers 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 fibers, 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 fibers, 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 fibers, 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 fibers, 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 fibers, silk, cotton and terylene equally.
Claims (4)
1. fibrous material Surface Nanocrystalline method, its method is by wrappage precursor TEOS or Zn (CH
3COO)
2Or Zr (OC
3H
7)
4Or TiCl
4Or Al (OC
3H
7)
31%～5%, the volume ratio scope of OP emulsifying agent 5%～20%, distilled water 75%～94% 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 SiO
2Or ZnO or TiO
2Or ZrO
2Or Al
2O
3Be grown directly upon fiber surface, dry behind formation 20～100nm film.
2. fibrous material Surface Nanocrystalline method according to claim 1, this method is undertaken by following processing step successively:
(1) presses wrappage precursor TEOS or Zn (CH
3COO)
2Or Zr (OC
3H
7)
4Or TiCl
4Or Al (OC
3H
7)
31%～5%, the volume ratio scope of 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 ℃.
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 fibers or terylene;
4. 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410012135 CN1240894C (en) | 2004-01-19 | 2004-01-19 | Fiber material surface nanocrystalline processing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200410012135 CN1240894C (en) | 2004-01-19 | 2004-01-19 | Fiber material surface nanocrystalline processing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1558015A CN1558015A (en) | 2004-12-29 |
| CN1240894C true CN1240894C (en) | 2006-02-08 |
Family
ID=34350966
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|---|---|---|---|
| CN 200410012135 Expired - Fee Related CN1240894C (en) | 2004-01-19 | 2004-01-19 | Fiber material surface nanocrystalline processing method |
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| CN (1) | CN1240894C (en) |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101845746A (en) * | 2010-06-07 | 2010-09-29 | 西安工程大学 | Method for modifying surface of polyester fabric with titanium tetrachloride |
| CN101956027B (en) * | 2010-10-13 | 2013-06-05 | 四川大学 | Sheep fur with nanometer antibacterial function and preparation method thereof |
| CN104373405B (en) * | 2014-11-29 | 2017-03-22 | 南京萨伯工业设计研究院有限公司 | Servo valve body and machining method of servo valve body |
| CN106560546B (en) * | 2015-09-30 | 2020-12-25 | 东丽纤维研究所（中国）有限公司 | Ultraviolet-proof knitted fabric |
| CN108735859A (en) * | 2018-05-30 | 2018-11-02 | 淮阴师范学院 | Photovoltaic device making Nano surface dry method making herbs into wool preparation method |
| CN109276824A (en) * | 2018-09-27 | 2019-01-29 | 国网河南省电力公司内乡县供电公司 | A kind of electric power overhaul dedicated safety belt |
| CN109046307B (en) * | 2018-10-21 | 2021-05-18 | 浙江海洋大学 | Preparation method of photocatalyst for degrading emerging pollutants |
| CN109797546B (en) * | 2019-01-22 | 2021-04-27 | 乐清市雅格狮丹服饰有限公司 | Finishing process of warm overcoat |
| CN111188189B (en) * | 2020-01-13 | 2022-05-17 | 江苏大学 | Biomass membrane material with ultraviolet resistance and heat management functions and preparation method thereof |
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