CN102691205A - Method using hydrothermal method to prepare nano-zinc-oxide assembly cotton fibers - Google Patents
Method using hydrothermal method to prepare nano-zinc-oxide assembly cotton fibers Download PDFInfo
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- CN102691205A CN102691205A CN2012101715479A CN201210171547A CN102691205A CN 102691205 A CN102691205 A CN 102691205A CN 2012101715479 A CN2012101715479 A CN 2012101715479A CN 201210171547 A CN201210171547 A CN 201210171547A CN 102691205 A CN102691205 A CN 102691205A
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Abstract
The invention discloses a method using a hydrothermal method to prepare nano-zinc-oxide assembly cotton fibers and particularly relates to a method using a hydrothermal method twice to prepare nano-zinc-oxide assembly cotton fibers with functions of fastness to washing and ultraviolet resistance. The method includes the steps: pre-treating cotton serving as main raw materials by NaOH solution to remove non-cellulosic components on the cotton fibers; then putting the pre-treated cotton fibers into initial growth medium composed of zinc nitrate and hexamethylene tetramine, transferring mixed liquor into a reaction kettle for reaction for 2h at the temperature of 60-100 DEG C after ultrasonic dispersion, and cleaning the cotton fibers with distilled water; and finally, putting the cleaned cotton fibers into newly-prepared zinc salt growth medium for reaction for 6-10h at the temperature of 60-100 DEG C so that the nano-zinc-oxide assembly cotton fibers are prepared. The method is simple in operation, and the growth medium for treating the cotton fibers can be recovered and can be returned to the cotton fiber procedures for reuse after concentration adjustment of the zinc nitrate and the hexamethylene tetramine, so that cost is reduced.
Description
Technical field
The present invention relates to the cotton fine method of a kind of nano zine oxide assembling, particularly a kind of cotton fine method of utilizing the secondary Hydrothermal Preparation to have good ultraviolet-resistent property and water-wash resistance.
Background technology
In recent years, because the fast development of industry causes the ozone layer in the atmosphere to be destroyed, cause ultraviolet radiation to increase.Have the expert to think, excessive ultraviolet radiation causes diseases such as comprising skin disease and cutaneum carcinoma.Therefore, textiles is carried out the antiultraviolet arrangement and become important topic.COTTON FABRIC is one of the most meable lining of ultraviolet ray, and COTTON FABRIC is through lining in summer commonly used, handles necessary so on pure cotton fabric, carry out uvioresistant.
It is a lot of to be used for the nano material kind that the fabric uvioresistant handles at present, but the most frequently used be nano zine oxide and nano titanium oxide.The nano zinc oxide particles anti-ultraviolet property is good, and is big to the wavelength band of ultraviolet screener, and antibiotic, the mildew-resistant and the smelly function that disappears are arranged, and cost performance is high, is desirable ultraviolet light screener.Employing oligomeric acrylic acid sodium such as Wang Hao and water-soluble titanate coupling agent carry out surface modified to nano zine oxide, obtain stability nanometer disperse system preferably; Again this dispersion liquid is made nano oxidized zinc-base COTTON FABRIC through soaking, roll, dry by the fire finishing technique; Wang Qing etc. adopt sol-gel technology preparing TiO
2-ZnO the hydrosol is put in order pure cotton fabric through operations such as padding, dry, bake; Appoint Wei to adopt sol-gel process to prepare nano-TiO
2Functional finishing agent adopts this finishing agent through soaking-roll process processing fabric, studies its uvioresistant and anti-microbial property influence to pure cotton fabric.The suitable silane coupler of selections such as Yu Aiping carries out preliminary treatment to nano-ZnO, adds a spot of thickener and dispersant then and is mixed with dressing liquid, and fabric is carried out the back arrangement, prepares the ultraviolet-resistent property COTTON FABRIC.Earlier obtain the nano silicon-based oxide dispersion liquid among the patent CN101798750A, after then COTTON FABRIC being put into above-mentioned dispersion liquid and padded, make fabric with uvioresistant performance through drying and baking with a spot of dispersant, nano silicon-based oxide and synthetic latex.Patent CN101718034A is with Ce (NO
3) 6H
2O solution, toluene, oleic acid and tert-butylamine once add in the container, make nano ultraviolet screener earlier, then with textile impregnation in the solution of above-mentioned screener, take out oven dry and can prepare high-performance uvioresistant fabric.The several method of below having reported all is stable dispersions of preparing inorganic nanometer powder earlier, and then cotton fibre handled has obtained anti-UV fabric.But because the condition of nano powder preparation is comparatively harsh, and aftertreatment technology is complicated, therefore is difficult to reach the reason of large-scale production.Secondly, because nano material is less, specific area is big, when product is dried, the secondary agglomeration of inorganic nanometer powder takes place in fabric very easily, can reduce the uvioresistant performance of nano material.The stable dispersions of the therefore this nano-powder of preparation earlier still faces big challenge in the actual production of fabric to the mode that fabric carries out post processing again.
Therefore, in order to address the above problem, we at first adopt the zinc solution that has configured that cotton fibre is soaked, and adopt hydrothermal reaction at low temperature at cotton fine surface and the direct synthesis of nano ZnO of internal cavities particle then.This method has solved the secondary agglomeration problem of the nano particle that exists in the conventional method, has simplified experimental technique, therefore has bright development prospect.In addition, handle cotton fine growth-promoting media and can reclaim, after the concentration of adjustment zinc nitrate and hexamethylenetetramine, return the cotton fine operation of processing and utilize again, reduced cost.
Summary of the invention
The object of the present invention is to provide a kind of simple preparation to have the cotton fine preparation method of water-wash resistance and uvioresistant performance.
The present invention includes following three steps:
(1) preliminary treatment of cotton
Earlier staple cotton is immersed in the NaOH solution of 5～30wt.%, and this solution is transferred in the agitated reactor, react 2h down at 60～150 ℃, washing dries up it to neutral then, as the reaction cotton.
The cotton fiber of (2) first assemblings of Hydrothermal Preparation ZnO
Get the Zn (NO of the 0.004mol/L of equal volume
3)
2Solution and hexamethylenetetramine solution are under stirring condition, with Zn (NO
3)
2Solution dropwise splashes in the hexamethylenetetramine solution; Form the growth-promoting media of zinc oxide, then the reaction cotton that obtains in (1) is put in the above-mentioned growth-promoting media, earlier dipping 1～3h under vacuum condition; And then sonicated; At last this cotton fibrinolytic liquid is transferred to and under 60～100 ℃, handles 2h in the agitated reactor, the cotton fibre of this ZnO assembling is clean with distilled water flushing, for use.
(3) secondary Hydrothermal Preparation ZnO assembling cotton fiber
The cotton fibre that obtains in (2) is immersed in the growth-promoting media of new preparation, contains Zn (NO in this growth-promoting media
3)
26H
2O 74～1048mg; The quality of hexamethylenetetramine is 35～525mg, is transferred to after cotton fibre is uniformly dispersed in the agitated reactor in 60～100 ℃ and handles 6～10h down, and reaction is accomplished the back with the distilled water cotton fibre that obtains of ultrasonic irrigation repeatedly; Drying obtains the cotton fine of nano-ZnO assembling; The cotton fibre of the assembling that makes is placed ultraviolet specrophotometer, carry out the ultraviolet test, light transmittance T%=I
t/ I
o* 100%, T is a light transmittance, I
tFor seeing through luminous intensity, I
oBe incident intensity.
The reaction equation that said process takes place is:
(CH
2)
6N
4+6H
2O→6HCHO+4NH
3
NH
3+H
2O→NH
4 ++OH
-
2OH
-+Zn
2+→Zn(OH)
2→ZnO+H
2O
Advance of the present invention is:
This method is simple to operate, and it is cotton fine directly to adopt zinc salt to soak, and hydrothermal treatment consists has directly generated the ZnO nano particle on cotton fine surface and internal cavities at low temperatures.And handle cotton fine growth-promoting media and can reclaim, after the concentration of adjustment zinc nitrate and hexamethylenetetramine, return the cotton fine operation of processing and utilize again, reduced cost.
Description of drawings
The cotton fine XRD spectra (a) of ZnO assembling unassembled cotton fine (b) that accompanying drawing 1 obtains for embodiment one is (a) for to contain Zn (NO
3)
2What hydrothermal treatment consists obtained in the 520mg growth-promoting media is cotton fine, can be known through assembling on the cotton fibre after the hydrothermal treatment consists by figure and go up six side's wurtzite ZnO.
Accompanying drawing 2 is assembled the low power SEM photo in cotton fine cross section for the zinc oxide that obtains through the cotton fibre of hydrothermal treatment consists among the embodiment one; Can know the ZnO small-particle that has formed a large amount of 20～100nm through the later cotton fiber of hydrothermal treatment consists surface and fiber lumen by figure, and favorable dispersibility.
The UV absorption curve of ZnO that accompanying drawing 3 obtains for embodiment one～embodiment five hydro-thermal methods assembling cotton fiber: textile fine (a) with at the Zn of different amounts (NO
3)
2Solution (b:370mg; C:520mg; D:743mg; E:838mg; F:1048mg) soak obtain cotton fine, can be known by figure, compare with textile fibre, ultraviolet transmitance obviously reduces the cotton fibre of nano-ZnO at wavelength 210～380nm place assembling in, and along with the increase of zinc salt amount, ultraviolet permeability increases gradually.Through calculating, ultraviolet transmitance can reach 80% at 300nm, and the ultraviolet permeability at 225nm place can reach 95%.
The light transmittance of the ZnO/ cotton fiber that accompanying drawing 4 records behind the washing different time for the ZnO assembling cotton fiber that obtains among the embodiment one and the relation between the wavelength (a:0 minute; B:20 minute; C:40 minute; D:60 minute).Compare with unwashed zinc oxide assembling cotton fiber, after washing in 20 minutes, 40 minutes, 60 minutes, the assembling cotton fiber obviously reduces in 200nm～400nm wave-length coverage iuuminting rate, still can absorb short wave ultraviolet (UVC) well; Ultraviolet B radiation (UVB); Long wave ultraviolet (UVA), the effect of this explanation assembling cotton fiber anti-ultraviolet radiation can not lost with the prolongation of wash time.
Below in conjunction with embodiment the present invention is further described:
Embodiment one:
1. the invention discloses the method for the synthetic ZnO assembling of a kind of secondary hydro-thermal cotton fiber, its concrete steps are following:
(1) preliminary treatment of cotton
Earlier staple cotton is immersed in the NaOH solution of 10wt.%, and this solution is transferred in the agitated reactor of polytetrafluoroethylene (PTFE), react 2h down at 150 ℃, washing dries up it to neutral then, as the reaction cotton;
The cotton fiber of (2) first assemblings of Hydrothermal Preparation ZnO
Get the Zn (NO of the 0.004mol/L of equal volume
3)
2Solution and hexamethylenetetramine solution are under stirring condition, with Zn (NO
3)
2Solution dropwise splashes in the hexamethylenetetramine solution; Form the growth-promoting media of zinc oxide, then the reaction cotton that obtains in (1) is put in the above-mentioned growth-promoting media, earlier dipping 2h under vacuum condition; And then sonicated; At last this cotton fibrinolytic liquid is transferred to and under 80 ℃, handles 2h in the agitated reactor, the cotton fibre of this ZnO assembling is clean with distilled water flushing, for use;
(3) secondary Hydrothermal Preparation ZnO assembling cotton fiber
The cotton fibre that obtains in (2) is immersed in the growth-promoting media of new preparation, contains Zn (NO in this growth-promoting media
3)
26H
2O 520mg; The quality of hexamethylenetetramine is 232mg, is transferred to after cotton fibre is uniformly dispersed in the agitated reactor in 90 ℃ and handles 8h down, and reaction is accomplished the back with the distilled water cotton fibre that obtains of ultrasonic irrigation repeatedly; Drying obtains the cotton fine of nano-ZnO assembling; The cotton fibre of the assembling that makes is placed ultraviolet specrophotometer, carry out the ultraviolet test, light transmittance T%=I
t/ I
o* 100%, T is a light transmittance, I
tFor seeing through luminous intensity, I
oBe incident intensity.
Embodiment two:
(1) preliminary treatment of cotton
Earlier staple cotton is immersed in the NaOH solution of 10wt.%, and this solution is transferred in the agitated reactor of polytetrafluoroethylene (PTFE), react 2h down at 150 ℃, washing dries up it to neutral then, as the reaction cotton;
The cotton fiber of (2) first assemblings of Hydrothermal Preparation ZnO
Get the Zn (NO of the 0.004mol/L of equal volume
3)
2Solution and hexamethylenetetramine solution are under stirring condition, with Zn (NO
3)
2Solution dropwise splashes in the hexamethylenetetramine solution; Form the growth-promoting media of zinc oxide, then the reaction cotton that obtains in (1) is put in the above-mentioned growth-promoting media, earlier dipping 2h under vacuum condition; And then sonicated; At last this cotton fibrinolytic liquid is transferred to and under 80 ℃, handles 2h in the agitated reactor, the cotton fibre of this ZnO assembling is clean with distilled water flushing, for use;
(3) secondary Hydrothermal Preparation ZnO assembling cotton fiber
The cotton fibre that obtains in (2) is immersed in the growth-promoting media of new preparation, contains Zn (NO in this growth-promoting media
3)
26H
2O 370mg; The quality of hexamethylenetetramine is 165mg, is transferred to after cotton fibre is uniformly dispersed in the agitated reactor in 90 ℃ and handles 8h down, and reaction is accomplished the back with the distilled water cotton fibre that obtains of ultrasonic irrigation repeatedly; Drying obtains the cotton fine of nano-ZnO assembling; The cotton fibre of the assembling that makes is placed ultraviolet specrophotometer, carry out the ultraviolet test, light transmittance T%=I
t/ I
o* 100%, T is a light transmittance, I
tFor seeing through luminous intensity, I
oBe incident intensity.
Embodiment three:
(1) preliminary treatment of cotton
Earlier staple cotton is immersed in the NaOH solution of 10wt.%, and this solution is transferred in the agitated reactor of polytetrafluoroethylene (PTFE), react 2h down at 150 ℃, washing dries up it to neutral then, as the reaction cotton;
The cotton fiber of (2) first assemblings of Hydrothermal Preparation ZnO
Get the Zn (NO of the 0.004mol/L of equal volume
3)
2Solution and hexamethylenetetramine solution are under stirring condition, with Zn (NO
3)
2Solution dropwise splashes in the hexamethylenetetramine solution; Form the growth-promoting media of zinc oxide, then the reaction cotton that obtains in (1) is put in the above-mentioned growth-promoting media, earlier dipping 2h under vacuum condition; And then sonicated; At last this cotton fibrinolytic liquid is transferred to and under 80 ℃, handles 2h in the agitated reactor, the cotton fibre of this ZnO assembling is clean with distilled water flushing, for use;
(3) secondary Hydrothermal Preparation ZnO assembling cotton fiber
The cotton fibre that obtains in (2) is immersed in the growth-promoting media of new preparation, contains Zn (NO in this growth-promoting media
3)
26H
2O 743mg; The quality of hexamethylenetetramine is 332mg, is transferred to after cotton fibre is uniformly dispersed in the agitated reactor in 90 ℃ and handles 8h down, and reaction is accomplished the back with the distilled water cotton fibre that obtains of ultrasonic irrigation repeatedly; Drying obtains the cotton fine of nano-ZnO assembling; The cotton fibre of the assembling that makes is placed ultraviolet specrophotometer, carry out the ultraviolet test, light transmittance T%=I
t/ I
o* 100%, T is a light transmittance, I
tFor seeing through luminous intensity, I
oBe incident intensity.
Embodiment four:
(1) preliminary treatment of cotton
Earlier staple cotton is immersed in the NaOH solution of 10wt.%, and this solution is transferred in the agitated reactor of polytetrafluoroethylene (PTFE), react 2h down at 150 ℃, washing dries up it to neutral then, as the reaction cotton;
The cotton fiber of (2) first assemblings of Hydrothermal Preparation ZnO
Get the Zn (NO of the 0.004mol/L of equal volume
3)
2Solution and hexamethylenetetramine solution are under stirring condition, with Zn (NO
3)
2Solution dropwise splashes in the hexamethylenetetramine solution; Form the growth-promoting media of zinc oxide, then the reaction cotton that obtains in (1) is put in the above-mentioned growth-promoting media, earlier dipping 2h under vacuum condition; And then sonicated; At last this cotton fibrinolytic liquid is transferred to and under 80 ℃, handles 2h in the agitated reactor, the cotton fibre of this ZnO assembling is clean with distilled water flushing, for use;
(3) secondary Hydrothermal Preparation ZnO assembling cotton fiber
The cotton fibre that obtains in (2) is immersed in the growth-promoting media of new preparation, contains Zn (NO in this growth-promoting media
3)
26H
2O 838mg; The quality of hexamethylenetetramine is 375mg, is transferred to after cotton fibre is uniformly dispersed in the agitated reactor in 90 ℃ and handles 8h down, and reaction is accomplished the back with the distilled water cotton fibre that obtains of ultrasonic irrigation repeatedly; Drying obtains the cotton fine of nano-ZnO assembling; The cotton fibre of the assembling that makes is placed ultraviolet specrophotometer, carry out the ultraviolet test, light transmittance T%=I
t/ I
o* 100%, T is a light transmittance, I
tFor seeing through luminous intensity, I
oBe incident intensity.
Embodiment five:
(1) preliminary treatment of cotton
Earlier staple cotton is immersed in the NaOH solution of 10wt.%, and this solution is transferred in the agitated reactor of polytetrafluoroethylene (PTFE), react 2h down at 150 ℃, washing dries up it to neutral then, as the reaction cotton;
The cotton fiber of (2) first assemblings of Hydrothermal Preparation ZnO
Get the Zn (NO of the 0.004mol/L of equal volume
3)
2Solution and hexamethylenetetramine solution are under stirring condition, with Zn (NO
3)
2Solution dropwise splashes in the hexamethylenetetramine solution; Form the growth-promoting media of zinc oxide, then the reaction cotton that obtains in (1) is put in the above-mentioned growth-promoting media, earlier dipping 2h under vacuum condition; And then sonicated; At last this cotton fibrinolytic liquid is transferred to and under 80 ℃, handles 2h in the agitated reactor, the cotton fibre of this ZnO assembling is clean with distilled water flushing, for use;
(3) secondary Hydrothermal Preparation ZnO assembling cotton fiber
The cotton fibre that obtains in (2) is immersed in the growth-promoting media of new preparation, contains Zn (NO in this growth-promoting media
3)
26H
2O 1048mg; The quality of hexamethylenetetramine is 469mg, is transferred to after cotton fibre is uniformly dispersed in the agitated reactor in 90 ℃ and handles 8h down, and reaction is accomplished the back with the distilled water cotton fibre that obtains of ultrasonic irrigation repeatedly; Drying obtains the cotton fine of nano-ZnO assembling; The cotton fibre of the assembling that makes is placed ultraviolet specrophotometer, carry out the ultraviolet test, light transmittance T%=I
t/ I
o* 100%, T is a light transmittance, I
tFor seeing through luminous intensity, I
oBe incident intensity.
Claims (2)
1. the invention discloses a kind of method of utilizing secondary hydro-thermal method synthesis of nano ZnO assembling cotton fiber, its concrete steps are following:
(1) preliminary treatment of cotton
Earlier staple cotton is immersed in the NaOH solution of 5～30wt.%, and this solution is transferred in the agitated reactor, react 2h down at 60～150 ℃, washing dries up it to neutral then, as the reaction cotton;
The cotton fiber of (2) first assemblings of Hydrothermal Preparation ZnO
Get the Zn (NO of the 0.004mol/L of equal volume
3)
2Solution and hexamethylenetetramine solution are under stirring condition, with Zn (NO
3)
2Solution dropwise splashes in the hexamethylenetetramine solution; Form the growth-promoting media of zinc oxide, then the reaction cotton that obtains in (1) is put in the above-mentioned growth-promoting media, earlier dipping 1～3h under vacuum condition; And then sonicated; At last this cotton fibrinolytic liquid is transferred to and under 60～100 ℃, handles 2h in the agitated reactor, the cotton fibre of this ZnO assembling is clean with distilled water flushing, for use;
(3) secondary Hydrothermal Preparation ZnO assembling cotton fiber
The cotton fibre that obtains in (2) is immersed in the growth-promoting media of new preparation, contains Zn (NO in this growth-promoting media
3)
26H
2O 74～1048mg; The quality of hexamethylenetetramine is 35～525mg, is transferred to after cotton fibre is uniformly dispersed in the agitated reactor in 60～100 ℃ and handles 6～10h down, and reaction is accomplished the back with the distilled water cotton fibre that obtains of ultrasonic irrigation repeatedly; Drying obtains the cotton fine of nano-ZnO assembling; The cotton fibre of the assembling that makes is placed ultraviolet specrophotometer, carry out the ultraviolet test, light transmittance T%=I
t/ I
o* 100%, T is a light transmittance, I
tFor seeing through luminous intensity, I
oBe incident intensity.
2. the method for claim 1 is characterized in that: hexamethylenetetramine and Zn (NO in the growth-promoting media of new preparation
3)
2Mol ratio be 0.95: 1.
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|---|---|---|---|
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|---|---|---|---|
| CN2012101715479A CN102691205A (en) | 2012-05-30 | 2012-05-30 | Method using hydrothermal method to prepare nano-zinc-oxide assembly cotton fibers |
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|---|---|---|---|---|
| CN102943379A (en) * | 2012-11-30 | 2013-02-27 | 苏州大学 | Preparation method of anti-bacterial ultraviolet-resistant textile |
| CN103194885A (en) * | 2013-04-19 | 2013-07-10 | 中国民航大学 | Method for microwave synthesis of nano-ZnO assembled cotton fibers |
| CN103343446A (en) * | 2013-06-27 | 2013-10-09 | 上海大学 | Method for preparing hydrophobic lipophilic cotton fabric material through structuring zinc oxide fine structure |
| CN109162086A (en) * | 2018-08-22 | 2019-01-08 | 广西大学 | A kind of preparation method of nano zine oxide in-situ modification anti-bacterial fibre |
| CN113087021A (en) * | 2021-04-14 | 2021-07-09 | 南阳师范学院 | MnO composed of2Preparation method of micron line composed of nanosheets |
| CN114395913A (en) * | 2022-01-13 | 2022-04-26 | 南通恒绮纺织有限公司 | Comfortable and durable cotton fabric and manufacturing process thereof |
| CN116463849A (en) * | 2023-06-05 | 2023-07-21 | 和也健康科技有限公司 | Waterproof anti-ultraviolet magnetic health-care fabric |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102943379A (en) * | 2012-11-30 | 2013-02-27 | 苏州大学 | Preparation method of anti-bacterial ultraviolet-resistant textile |
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| CN103194885A (en) * | 2013-04-19 | 2013-07-10 | 中国民航大学 | Method for microwave synthesis of nano-ZnO assembled cotton fibers |
| CN103343446A (en) * | 2013-06-27 | 2013-10-09 | 上海大学 | Method for preparing hydrophobic lipophilic cotton fabric material through structuring zinc oxide fine structure |
| CN103343446B (en) * | 2013-06-27 | 2015-05-06 | 上海大学 | Method for preparing hydrophobic lipophilic cotton fabric material through structuring zinc oxide fine structure |
| CN109162086A (en) * | 2018-08-22 | 2019-01-08 | 广西大学 | A kind of preparation method of nano zine oxide in-situ modification anti-bacterial fibre |
| CN113087021A (en) * | 2021-04-14 | 2021-07-09 | 南阳师范学院 | MnO composed of2Preparation method of micron line composed of nanosheets |
| CN114395913A (en) * | 2022-01-13 | 2022-04-26 | 南通恒绮纺织有限公司 | Comfortable and durable cotton fabric and manufacturing process thereof |
| CN116463849A (en) * | 2023-06-05 | 2023-07-21 | 和也健康科技有限公司 | Waterproof anti-ultraviolet magnetic health-care fabric |
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