CN105063808B - A kind of preparation method of the hollow type meta-aramid nano-fiber of lamellar structure stacking - Google Patents
A kind of preparation method of the hollow type meta-aramid nano-fiber of lamellar structure stacking Download PDFInfo
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Abstract
A kind of preparation method of the hollow type meta-aramid nano-fiber of lamellar structure stacking, it comprises the following steps：1）By 0.1 2 parts of calcium chloride (CaCl2) it is added to 10 20 parts of N, N dimethylacetylamides（DMAc）In, stirred 16 hours under room temperature condition, 0.5 4 parts of PMIA are added, stirred 13 hours at 100 DEG C；2）By step 1）Middle resulting solution electrostatic spinning, fltting speed is 0.1 1.0 mls/hour, and it is 5 15 centimetres to receive distance, and voltage is 18 25 kilovolts, is dried at 50 100 DEG C after being washed respectively in water, ethanol after collection spinning film；3）By step 2）Middle products therefrom is immersed in 5 hours in the NaOH solution of PH=14, after taking-up in water washing and drying；4）1 30 parts of DMAc are added in 1 20 parts of water and are stirred, add 0.5 3.0 parts of CaCl2Stir 15 hours；Mixed solution is transferred in ptfe autoclave, step 3 is added）The film of middle gained, reacts 1 24 hours under the conditions of 50 250 DEG C, after naturally cooling to room temperature, is dried naturally after being washed respectively for several times with acetone, water, ethanol.
Description
Technical field
The present invention relates to a kind of preparation method of meta-aramid nano-fiber, especially a kind of hollow out of lamellar structure stacking
The preparation method of type meta-aramid nano-fiber.
Technical background
Aramid fiber is a kind of new high-tech synthetic fibers, with superhigh intensity, high-modulus and high temperature resistant, acid-fast alkali-proof, weight
The premium properties such as amount is light, insulation, anti-aging, life cycle are long, is widely used in composite, ballistic-resistant article, building materials, extraordinary anti-
The fields such as shield clothes, electronic equipment.The limited oxygen index (LOI) of meta-aramid is more than 28, therefore will not when it leaves flame
Burn away.Performance with excellent resistance to most of chemical substances, is resistant to the inorganic acid of most of high concentrations, alkaline-resisting under normal temperature
Performance is good.The heat resistance of p-aramid fiber is higher than meta-aramid, and continuous temperature in use scope is -196 DEG C -204 DEG C, 560
Do not decomposed under DEG C high temperature, it is non-fusible.This has significant advantage for the retrofit under the conditions of HTHP, soda acid etc. to material.
The performance of nano material is closely related with its size, structure, and to the retrofit of nano material producing multi-stage micro-nano structure
It is always the research emphasis and Research Challenges in this field to open up function.
The content of the invention
To overcome above-mentioned the deficiencies in the prior art, above-mentioned technical problem is solved, it is an object of the invention to provide a kind of piece
The preparation method of the hollow type meta-aramid nano-fiber of Rotating fields stacking, based on ion liquid dissolving system, in HTHP
Under the conditions of orientation etching in situ is carried out to meta-aramid nano-fiber, prepare size and stacked by lamellar structure with morphology controllable
Hollow out aramid nano-fiber material, can be realized to etching by controlling the factor such as ratio, temperature, time of ionic liquid and water
The control of process and product morphology.
To achieve the above object, present invention employs following technical scheme：
A kind of preparation method of the hollow type meta-aramid nano-fiber of lamellar structure stacking, it comprises the following steps：
1）By mass fraction, by 0.1-2 parts of calcium chloride (CaCl2) it is added to 10-20 parts of DMA
（DMAc）In, stirred 1-6 hours under room temperature condition, 0.5-4 parts of PMIA is added, stirred 1-3 hours at 100 DEG C；
2）By step 1）Middle resulting solution electrostatic spinning, fltting speed is 0.1-1.0 mls/hour, and it is 5- to receive distance
15 centimetres, voltage is 18-25 kilovolts, is dried at 50-100 DEG C after being washed respectively in water, ethanol after collection spinning film；
3）By step 2）Middle products therefrom is immersed in 5 hours in the NaOH solution of PH=14, is washed in water after taking-up and dried
It is dry；
4）By mass fraction, 1-30 parts of DMAc is added in 1-20 parts of water and is stirred, add 0.5-3.0 parts
CaCl2Stirring 1-5 hours；Mixed solution is transferred in ptfe autoclave, step 3 is added）The film of middle gained,
Reacted 1-24 hours under the conditions of 50-250 DEG C, it is natural after being washed respectively for several times with acetone, water, ethanol after naturally cooling to room temperature
Dry.
The beneficial effects of the invention are as follows：
1）The hollow out aramid nano-fiber of the lamella oriented stack that the present invention is prepared, its size, morphology controllable, and pattern
It is regular, structure unification.
2）Preparation method of the invention can be by reaction conditions such as etching liquid concentration, temperature, times come etching process and product
Thing form, temperature is higher, the time is more long, and lamella size is bigger, and fiber etching degree from outside to inside is deeper.Change etching liquid dense
Degree can obtain the product of different etching form.As the extension method of wet etching, to the retrofit tool of organic nano material
There is innovative significance.
3）Product preparation process of the present invention is simple, and low cost is easy to large-scale production.
Brief description of the drawings
Fig. 1 is the TEM electron microscopes of the hollow type meta-aramid nano-fiber of lamellar structure stacking of the present invention.
Specific embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention
In accompanying drawing, the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is
A part of embodiment of the present invention, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art
The every other embodiment obtained under the premise of creative work is not made, belongs to the scope of protection of the invention.
As shown in figure 1, a kind of preparation method of the hollow type meta-aramid nano-fiber of lamellar structure stacking, by difference
Aramid fiber Electrospun nano-fibers are oriented etching in situ by the ion liquid dissolving liquid of concentration under the high temperature conditions, are obtained
The engraved structure of regularly arranged lamellar structure composition.Control etching direction, speed and etching deep by controlling reaction condition
Degree, so as to obtain the hollow out form of different-shape.It is the deeper PMIA solid sections (A) of color in the middle of visible rod in figure, surrounding
It is the shallower PMIA openwork parts (B) of color.
A kind of preparation method of the hollow type meta-aramid nano-fiber of lamellar structure stacking, it comprises the following steps：
1）By mass fraction, by 0.1-2 parts of calcium chloride (CaCl2) it is added to 10-20 parts of DMA
（DMAc）In, stirred 1-6 hours under room temperature condition, 0.5-4 parts of PMIA is added, stirred 1-3 hours at 100 DEG C；
2）By step 1）Middle resulting solution electrostatic spinning, fltting speed is 0.1-1.0 mls/hour, and it is 5- to receive distance
15 centimetres, voltage is 18-25 kilovolts, is dried at 50-100 DEG C after being washed respectively in water, ethanol after collection spinning film；
3）By step 2）Middle products therefrom is immersed in 5 hours in the NaOH solution of PH=14, is washed in water after taking-up and dried
It is dry；
4）By mass fraction, 1-30 parts of DMAc is added in 1-20 parts of water and is stirred, add 0.5-3.0 parts
CaCl2Stirring 1-5 hours；Mixed solution is transferred in ptfe autoclave, step 3 is added）The film of middle gained,
Reacted 1-24 hours under the conditions of 50-250 DEG C, it is natural after being washed respectively for several times with acetone, water, ethanol after naturally cooling to room temperature
Dry.
Embodiment 1：
A kind of preparation method of the hollow type meta-aramid nano-fiber of lamellar structure stacking, it comprises the following steps：
1）By mass fraction, by 0.1 part of calcium chloride (CaCl2) it is added to 10 parts of DMAs（DMAc）In,
Stirred 1 hour under room temperature condition, add 0.5 part of PMIA, stirred 1 hour at 100 DEG C；
2）By step 1）Middle resulting solution electrostatic spinning, fltting speed is 0.1 ml/hour, and it is 5 centimetres to receive distance,
Voltage is 18 kilovolts, is dried at 50 DEG C after being washed respectively in water, ethanol after collection spinning film；
3）By step 2）Middle products therefrom is immersed in 5 hours in the NaOH solution of PH=14, is washed in water after taking-up and dried
It is dry；
4）By mass fraction, 1 part of DMAc is added in 1 part of water and is stirred, add 0.5 part of CaCl2Stir 1 small
When；Mixed solution is transferred in ptfe autoclave, step 3 is added）The film of middle gained, 1 is reacted under the conditions of 50 DEG C
Hour, after naturally cooling to room temperature, dried naturally after being washed respectively for several times with acetone, water, ethanol.
Embodiment 2：
A kind of preparation method of the hollow type meta-aramid nano-fiber of lamellar structure stacking, it comprises the following steps：
1）By mass fraction, by 1 part of calcium chloride (CaCl2) it is added to 15 parts of DMAs（DMAc）In, room
Stirred 3 hours under the conditions of temperature, add 2 parts of PMIA, stirred 2 hours at 100 DEG C；
2）By step 1）Middle resulting solution electrostatic spinning, fltting speed is 0.5 ml/hour, and it is 10 centimetres to receive distance,
Voltage is 22 kilovolts, is dried at 80 DEG C after being washed respectively in water, ethanol after collection spinning film；
3）By step 2）Middle products therefrom is immersed in 5 hours in the NaOH solution of PH=14, is washed in water after taking-up and dried
It is dry；
4）By mass fraction, 15 parts of DMAc are added in 10 parts of water and are stirred, add 1.5 parts of CaCl2Stir 3 small
When；Mixed solution is transferred in ptfe autoclave, step 3 is added）The film of middle gained, reacts under the conditions of 150 DEG C
12 hours, after naturally cooling to room temperature, dried naturally after being washed respectively for several times with acetone, water, ethanol.
Embodiment 3：
A kind of preparation method of the hollow type meta-aramid nano-fiber of lamellar structure stacking, it comprises the following steps：
1）By mass fraction, by 2 parts of calcium chloride (CaCl2) it is added to 20 parts of DMAs（DMAc）In, room
Stirred 6 hours under the conditions of temperature, add 4 parts of PMIA, stirred 3 hours at 100 DEG C；
2）By step 1）Middle resulting solution electrostatic spinning, fltting speed is 1.0 mls/hour, and it is 15 centimetres to receive distance,
Voltage is 25 kilovolts, is dried at 100 DEG C after being washed respectively in water, ethanol after collection spinning film；
3）By step 2）Middle products therefrom is immersed in 5 hours in the NaOH solution of PH=14, is washed in water after taking-up and dried
It is dry；
4）By mass fraction, 30 parts of DMAc are added in 20 parts of water and are stirred, add 3.0 parts of CaCl2Stirring 1-5
Hour；Mixed solution is transferred in ptfe autoclave, step 3 is added）The film of middle gained, it is anti-under the conditions of 250 DEG C
Answer 24 hours, after naturally cooling to room temperature, dried naturally after being washed respectively for several times with acetone, water, ethanol.
Claims (1)
1. the preparation method of the hollow type meta-aramid nano-fiber of a kind of lamellar structure stacking, it is characterised in that it includes as follows
Step：
1) by mass fraction, by 0.1-2 parts of calcium chloride (CaCl2) be added in 10-20 parts of DMA (DMAc),
Stirred 1-6 hours under room temperature condition, add 0.5-4 parts of PMIA, stirred 1-3 hours at 100 DEG C；
2) by step 1) in resulting solution electrostatic spinning, spinning fltting speed be 0.1-1.0 mls/hour, receive distance be 5-
15 centimetres, voltage is 18-25 kilovolts；Dried at 50-100 DEG C after being washed respectively in water, ethanol after collection spinning film；
3) by step 2) in products therefrom be immersed in 5 hours in the NaOH solution of pH=14, after taking-up in water washing and drying；
4) by mass fraction, 1-30 parts of DMA (DMAc) is added in 1-20 parts of water and is stirred, then added
Enter 0.5-3.0 parts of calcium chloride (CaCl2) stir 1-5 hours；Mixed solution is transferred in ptfe autoclave, step is added
The film of rapid 3) middle gained, reacts 1-24 hours under the conditions of 50-250 DEG C, after naturally cooling to room temperature, with acetone, water, ethanol point
Dried naturally after not washing for several times.
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| CN101838888A (en) * | 2010-05-10 | 2010-09-22 | 张家港耐尔纳米科技有限公司 | Method for preparing electrospun meta-aramid nano-fiber |
| CN102704028A (en) * | 2012-05-26 | 2012-10-03 | 东华大学 | Preparation method of meta-aramid nano-nets fiber membrane |
| CN103046427A (en) * | 2012-12-20 | 2013-04-17 | 华南理工大学 | Method for preparing aromatic polyamide fiber paper base material by electrospinning technology |
| CN103088627A (en) * | 2013-02-07 | 2013-05-08 | 贵州大学 | Treatment method for surface of aramid fiber |
| CN103726233A (en) * | 2013-12-09 | 2014-04-16 | 同济大学 | Preparation method and application of polyisophthaloyl metaphenylene diamine-polyacrylonitrile composite nanofiber film |
| CN103806221A (en) * | 2014-02-24 | 2014-05-21 | 东华大学 | Preparation method for multi-component net-shaped nanofiber membrane |
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2015
- 2015-07-29 CN CN201510449901.3A patent/CN105063808B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101838888A (en) * | 2010-05-10 | 2010-09-22 | 张家港耐尔纳米科技有限公司 | Method for preparing electrospun meta-aramid nano-fiber |
| CN102704028A (en) * | 2012-05-26 | 2012-10-03 | 东华大学 | Preparation method of meta-aramid nano-nets fiber membrane |
| CN103046427A (en) * | 2012-12-20 | 2013-04-17 | 华南理工大学 | Method for preparing aromatic polyamide fiber paper base material by electrospinning technology |
| CN103088627A (en) * | 2013-02-07 | 2013-05-08 | 贵州大学 | Treatment method for surface of aramid fiber |
| CN103726233A (en) * | 2013-12-09 | 2014-04-16 | 同济大学 | Preparation method and application of polyisophthaloyl metaphenylene diamine-polyacrylonitrile composite nanofiber film |
| CN103806221A (en) * | 2014-02-24 | 2014-05-21 | 东华大学 | Preparation method for multi-component net-shaped nanofiber membrane |
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Effective date of registration: 20191009 Address after: 313300 Northwest Industrial Park, Anji Economic Development Zone, Anji County, Huzhou City, Zhejiang Province Patentee after: Zhejiang Xuyi New Material Technology Co., Ltd. Address before: 310018 No. 2, Xiasha Higher Education Zone, Hangzhou, Zhejiang Patentee before: Zhejiang University of Technology |
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Address after: 313300 No. 28, Jingtu Road, Dipu street, Anji County, Huzhou City, Zhejiang Province Patentee after: Zhejiang Xuyi New Material Technology Co.,Ltd. Address before: 313300 Northwest Industrial Park, Anji Economic Development Zone, Anji County, Huzhou City, Zhejiang Province Patentee before: Zhejiang Xuyi New Material Technology Co.,Ltd. |
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