CN101949084A - Preparation method of ZnO-doped PET ultrafine non-woven fabric - Google Patents
Preparation method of ZnO-doped PET ultrafine non-woven fabric Download PDFInfo
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- CN101949084A CN101949084A CN2010102166291A CN201010216629A CN101949084A CN 101949084 A CN101949084 A CN 101949084A CN 2010102166291 A CN2010102166291 A CN 2010102166291A CN 201010216629 A CN201010216629 A CN 201010216629A CN 101949084 A CN101949084 A CN 101949084A
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Abstract
The invention relates to a preparation method of ZnO-doped PET ultrafine non-woven fabric, which comprises the following steps: (1) mixing zinc salt and surfactant according to the molar ratio of 1:2, dissolving the mixture into an organic solvent, and heating and refluxing for 30min at 80 DEG C; (2) adding deionized water and alkaline agent according to the volume ratio of 1:1, magnetically stirring for 1h at the room temperature, centrifuging, and then, drying in vacuum at the room temperature to obtain nano-ZnO powder; and (3) preparing a hexafluoroisopropanol solution of PET and a toluene solution of nano-ZnO, preparing the two solutions into a ZnO/PET spinning solution according to the volume ratio of 9:1, putting the ZnO/PET spinning solution into an electrostatic spinning device for spinning, and drying the obtained product in vacuum for 24h at the normal temperature. The invention has the advantages of simple processes, easy acquisition and low cost of raw materials, low equipment requirements, low energy consumption and convenient popularization; and the obtained non-woven fabric has excellent anti-ultraviolet performance and does not have obvious defects on the surface.
Description
Technical field
The invention belongs to the preparation field of the ultra-fine nonwoven fabric of PET, the preparation method of the ultra-fine nonwoven fabric of particularly a kind of ZnO doping PET.
Background technology
Because the special nature of ZnO, and ZnO makes that in the broad prospect of application of numerous areas the technology of preparing of ZnO is a research focus all the time.The progressively maturation of simultaneous superfine fibre technology of preparing, nano-ZnO and superfine fibre is compound, thus the research that obtains functional composite material also more and more causes people's extensive concern.At present, using the ZnO nano-powder to give the functional basic skills of organic fiber macromolecular material has: the surface modification that 1. is prepared into nano-powder by the water of nano-ZnO, thereby improve nano-ZnO in the organic facies dispersiveness, then nano-powder is added and spin functional fibre in the polymer dope.But such procedure complexity, cost height and nano ZnO powder difficulties in dispersion; 2. will be coated in the high-molecular organic material surface after nano ZnO powder and the adhesive blend, give its special function.But such method faces the scattering problem of superfine powder too, and the use of adhesive simultaneously is difficult to avoid to the performance impact of high-molecular organic material itself.3. by electrostatic force or chemical bond combination,, make it that point that can mutually combine be arranged promptly by modification is carried out on high-molecular organic material surface or nano ZnO powder surface.Such process obviously is complicated, and is not easy-operating, and electrostatic force is in conjunction with unstable often.
Summary of the invention
Technical problem to be solved by this invention provides the preparation method of the ultra-fine nonwoven fabric of a kind of ZnO doping PET, and technology of the present invention is simple, and raw material is easy to get and is cheap, and equipment requires low, and energy consumption is low, is convenient to promote; The nonwoven fabric that is obtained has good uvioresistant performance, and the surface does not have obvious defects; Many difficulties and shortcoming that this method has been run into when successfully having overcome the interpolation of inorganic oxide zinc nano-powder in organic polymer be the application of zinc oxide, and the preparation of functional high molecule material are had laid a good foundation.
The preparation method of the ultra-fine nonwoven fabric of a kind of ZnO doping PET of the present invention comprises:
(1) zinc salt and surfactant were mixed in 1: 2 in molar ratio, be dissolved in the organic solvent, at 80 ℃ of following reflux 30min, after cooling, discard clear liquid, wherein, surfactant is 1: 25 with the volume of organic solvent ratio;
(2) the adding volume ratio is 1: 1 deionized water and an alkaline agent, and the room temperature lower magnetic force stirs 1h, obtains nano ZnO powder after the room temperature vacuumize of centrifugal back, and wherein, the mol ratio of zinc salt and alkaline agent is 1: 5;
(3) the hexafluoroisopropanol solution of preparation 200g/LPET and the toluene solution of 60g/L nano-ZnO; Above-mentioned two kinds of solution were mixed with the ZnO/PET spinning solution in 9: 1 by volume; Place the electrostatic spinning apparatus spinning, the product that obtains is in normal temperature vacuumize 24h.
Zn salt in the described step (1) is ZnSO
4, surfactant is CH
3(CH
2)
7CH=CH (CH
2)
7COONa, organic solvent are C
6H
14
Alkaline agent in the described step (2) is that concentration is the NaOH solution of 0.1M～0.4M.
The present invention adopts the oil-water interfaces legal system to be equipped with nano zine oxide, and this method can obtain the nano zine oxide of favorable dispersibility in organic facies, and technology is simple, raw material is easy to get and is cheap, and equipment requires low, and energy consumption is low, being convenient to promote, is a kind of excellent process for preparing superfine nano-crystalline.Simultaneously, add among the PET by the nano zine oxide of method of electrostatic spinning the synthetic preparation of oil-water interfaces method, obtain the ZnO/PET superfine fibre, realize the interpolation of nano ZnO powder in the organic fiber macromolecular material by simple method, give the PET fiber certain functional, and finally obtain the ZnO/PET superfine fibre nonwoven cloth, to satisfy the requirement of specific use nonwoven fabric.
Beneficial effect
(1) this method technology is simple, and raw material is easy to get and is cheap, and equipment requires low, and energy consumption is low, is convenient to promote;
(2) nonwoven fabric that the present invention obtained has good uvioresistant performance, and the surface does not have obvious defects;
The many difficulties and the shortcoming that have been run into when (3) this method has successfully overcome the interpolation of inorganic oxide zinc nano-powder in organic polymer be the application of zinc oxide, and the preparation of functional high molecule material are had laid a good foundation.
Description of drawings
Fig. 1 is the transmission electron microscope picture of the zinc oxide of embodiment 1 gained;
Fig. 2 is the X-ray diffractogram of the zinc oxide of embodiment 1 gained;
Fig. 3 is the device for spinning figure among the embodiment 2;
Fig. 4 is the ESEM picture of product among the embodiment 2.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
(1) 2.5ml 0.4M ZnSO
4Solution and 5ml 0.4M CH
3(CH
2)
7CH=CH (CH
2)
7COONa is placed on earlier and fills 50ml C
6H
14Three-neck flask in, with 80 ℃ stir down 30min, after cooling, move into conical flask, discard down clear liquid;
(2) add the 12.5ml deionized water in conical flask, 12.5ml 0.4MNaOH solution dropwise adds, and under the room temperature, magnetic agitation 1h obtains nanometer Zinc oxide powder after the room temperature vacuumize of centrifugal back;
The transmission electron microscope picture of the ZnO nano particle that scheme 1 makes is seen Fig. 1, and the average grain diameter that is estimated particle by figure is about 8nm, and dispersive property is better.The X ray diffracting spectrum of sample is seen Fig. 2, and diffraction peak is consistent with the standard peak position of zinc oxide, calculates the particle size and the TEM picture gained sizableness of gained by the Scherrer formula.
(1) 2.5ml 0.1M ZnSO
4Solution and 5ml 0.1M CH
3(CH
2)
7CH=CH (CH
2)
7COONa is placed on earlier and fills 50ml C
6H
14Three-neck flask in, with 80 ℃ stir down 30min, after cooling, move into conical flask, discard down clear liquid;
(2) add the 12.5ml deionized water in conical flask, 12.5ml 0.1MNaOH solution dropwise adds, and under the room temperature, magnetic agitation 1h obtains nanometer Zinc oxide powder after the room temperature vacuumize of centrifugal back;
(3) C of preparation 200g/LPET
3H
2F
6O solution; The C of the nano-ZnO of preparation 60g/L
7H
8Solution, fully magnetic agitation; PETC
3H
2F
6O solution and ZnO toluene solution were mixed with the ZnO/PET spinning solution in 9: 1 by volume, placed the electrostatic spinning apparatus spinning, product normal temperature vacuumize 24h.Device for spinning as shown in Figure 3, concrete spinning technology parameter is as follows:
Operating voltage: 14kV
Needle gauge: No. 7 tack medical needles, 3mL
Syringe needle is apart from receiver distance: 13cm
Feed flow speed: 1.0mL/h
The spinning time: 4h
Vacuumize temperature and time: air drying 24h
Product specification: 10 * 8cm (long * wide)
The ESEM picture of the product that makes is seen Fig. 4, and ZnO/PET superfine fibre smooth surface does not have obvious pearl.
The uvioresistant performance that obtains product is as shown in table 1, and simple as can be seen from the table PET superfine fibre nonwoven cloth has possessed very good uvioresistant performance, and this is that structure is tight, so ultraviolet ray transmissivity is very low because the superfine fibre nonwoven cloth fibre gap is little; After adding ZnO, because its quantum size effect can absorb ultraviolet ray preferably, make the UPF value significantly improve, ultraviolet ray transmissivity is extremely low, makes this material to provide enough protections for operation under the high uitraviolet intensity condition.
Embodiment 3
(1) 2.5ml 0.1M ZnSO
4Solution and 5ml 0.1M CH
3(CH
2)
7CH=CH (CH
2)
7COONa is placed on earlier and fills 50ml C
6H
14Three-neck flask in, with 80 ℃ stir down 30min, after cooling, move into conical flask, discard down clear liquid;
(2) add the 12.5ml deionized water in conical flask, 12.5ml 0.2MNaOH solution dropwise adds, and under the room temperature, magnetic agitation 1h obtains nanometer Zinc oxide powder after the room temperature vacuumize of centrifugal back;
(3) C of preparation 200g/LPET
3H
2F
6O solution; The C of the nano-ZnO of preparation 60g/L
7H8 solution, fully magnetic agitation; PETC
3H
2F
6O solution and ZnO toluene solution were mixed with the ZnO/PET spinning solution in 9: 1 by volume, placed the electrostatic spinning apparatus spinning, product normal temperature vacuumize 24h.
Embodiment 4
(1) 2.5ml 0.1M ZnSO
4Solution and 5ml 0.1M CH
3(CH
2)
7CH=CH (CH
2)
7COONa is placed on earlier and fills 50ml C
6H
14Three-neck flask in, with 80 ℃ stir down 30min, after cooling, move into conical flask, discard down clear liquid;
(2) add the 12.5ml deionized water in conical flask, 12.5ml 0.3MNaOH solution dropwise adds, and under the room temperature, magnetic agitation 1h obtains nanometer Zinc oxide powder after the room temperature vacuumize of centrifugal back;
(3) C of preparation 200g/LPET
3H
2F
6O solution; The C of the nano-ZnO of preparation 60g/L
7H
8Solution, fully magnetic agitation; PETC
3H
2F
6O solution and ZnO toluene solution were mixed with the ZnO/PET spinning solution in 9: 1 by volume, placed the electrostatic spinning apparatus spinning, product normal temperature vacuumize 24h.
Table 1
Claims (3)
1. the preparation method of the ultra-fine nonwoven fabric of ZnO doping PET comprises:
(1) zinc salt and surfactant were mixed in 1: 2 in molar ratio, be dissolved in the organic solvent, at 80 ℃ of following reflux 30min, after cooling, discard clear liquid, wherein, surfactant is 1: 25 with the volume of organic solvent ratio;
(2) the adding volume ratio is 1: 1 deionized water and an alkaline agent, and the room temperature lower magnetic force stirs 1h, obtains nano ZnO powder after the room temperature vacuumize of centrifugal back, and wherein, the mol ratio of zinc salt and alkaline agent is 1: 5;
(3) the hexafluoroisopropanol solution of preparation 200g/LPET and the toluene solution of 60g/L nano-ZnO; Above-mentioned two kinds of solution were mixed with the ZnO/PET spinning solution in 9: 1 by volume; Place the electrostatic spinning apparatus spinning, the product that obtains is in normal temperature vacuumize 24h.
2. the preparation method of the ultra-fine nonwoven fabric of a kind of ZnO doping PET according to claim 1, it is characterized in that: the Zn salt in the described step (1) is ZnSO
4, surfactant is CH
3(CH
2)
7CH=CH (CH
2)
7COONa, organic solvent are C
6H
14
3. the preparation method of the ultra-fine nonwoven fabric of a kind of ZnO doping PET according to claim 1 is characterized in that: the alkaline agent in the described step (2) is that concentration is the NaOH solution of 0.1M～0.4M.
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| CN2010102166291A CN101949084A (en) | 2010-07-01 | 2010-07-01 | Preparation method of ZnO-doped PET ultrafine non-woven fabric |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114887497A (en) * | 2022-05-20 | 2022-08-12 | 镇江市高等专科学校 | Preparation method of electrostatic spinning oil-water separation membrane material based on waste plastics |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1776035A (en) * | 2005-11-29 | 2006-05-24 | 天津工业大学 | PVA fiber and its non-woven fabric preparing method |
| CN1800454A (en) * | 2006-01-09 | 2006-07-12 | 东华大学 | Antibacterial PET fiber and process for making same |
| CN1974906A (en) * | 2006-12-12 | 2007-06-06 | 天津泰达洁净材料有限公司 | Double component molten and jetted non-woven fabric and its making process |
| CN101144225A (en) * | 2007-10-25 | 2008-03-19 | 吉安市三江超纤无纺有限公司 | Technique for preparing dual-component spunbonded water-jet bonding non-woven fabrics |
-
2010
- 2010-07-01 CN CN2010102166291A patent/CN101949084A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1776035A (en) * | 2005-11-29 | 2006-05-24 | 天津工业大学 | PVA fiber and its non-woven fabric preparing method |
| CN1800454A (en) * | 2006-01-09 | 2006-07-12 | 东华大学 | Antibacterial PET fiber and process for making same |
| CN1974906A (en) * | 2006-12-12 | 2007-06-06 | 天津泰达洁净材料有限公司 | Double component molten and jetted non-woven fabric and its making process |
| CN101144225A (en) * | 2007-10-25 | 2008-03-19 | 吉安市三江超纤无纺有限公司 | Technique for preparing dual-component spunbonded water-jet bonding non-woven fabrics |
Non-Patent Citations (1)
| Title |
|---|
| 《纺织科技进展》 20100630 赵旭等 ZnO掺杂PET超细无纺布的制备与性能研究 16-18 1-3 , 2 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114887497A (en) * | 2022-05-20 | 2022-08-12 | 镇江市高等专科学校 | Preparation method of electrostatic spinning oil-water separation membrane material based on waste plastics |
| CN114887497B (en) * | 2022-05-20 | 2023-07-25 | 镇江市高等专科学校 | Preparation method of electrostatic spinning oil-water separation membrane material based on waste plastics |
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Open date: 20110119 |