CN108084468A - A kind of preparation method of the nanometer aramid fiber film based on vacuum aided LBL self-assembly - Google Patents
A kind of preparation method of the nanometer aramid fiber film based on vacuum aided LBL self-assembly Download PDFInfo
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- CN108084468A CN108084468A CN201711469366.3A CN201711469366A CN108084468A CN 108084468 A CN108084468 A CN 108084468A CN 201711469366 A CN201711469366 A CN 201711469366A CN 108084468 A CN108084468 A CN 108084468A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2377/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2377/06—Polyamides derived from polyamines and polycarboxylic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2439/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a single or double bond to nitrogen or by a heterocyclic ring containing nitrogen; Derivatives of such polymers
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Abstract
A kind of preparation method of nanometer aramid fiber film based on vacuum aided LBL self-assembly disclosed by the invention, including：Potassium hydroxide and p-aramid fiber chopped strand are added in dimethyl sulphoxide solution, is stirred at room temperature to obtain p-aramid fiber and is chopped nanofiber suspension；Then polydiene propyl dichloromethyl ammonium salt solution is configured, be chopped nanofiber suspension and polydiene propyl dichloromethyl ammonium salt solution interval of isometric p-aramid fiber is taken to carry out layer assembly using vacuum filtration mode, deionized water is reused after assembling and ethyl alcohol is respectively washed, is finally air-dried by squeezing, room temperature up to nanometer aramid fiber film.The present invention using vacuum aided self-service dress layer by layer method, prepare the aramid fiber nano thin-film haveing excellent performance, this method is easy to operate, and number of repetition greatly shortens, ultrahigh in efficiency, the introducing of other components can be greatly reduced simultaneously, given full play to the excellent properties of nanometer aramid fiber, widened its development and application in other materials field.
Description
Technical field
The invention belongs to technical field of material, and in particular to a kind of nanometer virtue based on vacuum aided LBL self-assembly
The preparation method of synthetic fibre film.
Background technology
Para-aramid fiber, i.e. poly(p-phenylene terephthalamide) (PPTA) fiber is a kind of the close of plan cross-linked network
High polymer has the excellent properties such as high intensity, high-modulus, high temperature resistant, anticorrosive, can be used as high intensity, light-weighted honeycomb
Structural material, heat safe insulating materials and high-performance electronic Communication Equipment material, thus it is widely used in aviation boat
My god, the various fields such as traffic power, national defense and military, very important status is occupied in modern industry.But since aramid fiber is (short
Cut) fiber surface strand oriented degree is high, crystallinity is high, and the big steric hindrance of phenyl ring so that the hydrogen on amide group is difficult
With other atomic reactions；In addition fiber surface is smooth, and specific surface area is small, lacks chemical active radical, is engaged with matrix without physics
Point etc., greatly affected its application in field of compound material.
With constantly bringing forth new ideas for nanometer technology, aramid nano-fiber also slowly becomes focus of concern.It is well known that
When material it is small to nanoscale when, due to the change of the physical and chemical properties of itself so as to showing small-size effect, surface
The tunnel-effect of effect, quantum size effect and macroscopic quantum.Nanofiber usually because the variation of size, form and structure,
The performance of unexistent uniqueness in original substance is showed on the basis of original macroscopic material is kept.
There is researcher that aramid nano-fiber (ANF) and polyethylene oxide (PEO) is compound, pass through LBL self-assembly method
(LBL) nano compound film of high ion flux and good thermal stability is obtained；Also there is researcher by aramid nano-fiber (ANF)
Compound, the film for by LBL methods being prepared for that there are very good mechanical properties with polydiene propyl dichloromethyl ammonium (PDDA).But
This LBL methods under normal circumstances will repeatedly at least 200-300 times or so, the consuming time extremely.Early-stage study finds simple
ANF is difficult film forming, also very fragile even if forming a film.
The content of the invention
It is an object of the invention to provide a kind of preparation sides of the nanometer aramid fiber film based on vacuum aided LBL self-assembly
Method solves the problems, such as that time-consuming, film forming difficulty is big for existing LBL methods preparation nanometer aramid fiber film.
The technical solution adopted in the present invention is：A kind of system of the nanometer aramid fiber film based on vacuum aided LBL self-assembly
Preparation Method, including step：
Potassium hydroxide and p-aramid fiber chopped strand are added in dimethyl sulphoxide solution, are stirred at room temperature to obtain pair
Position aramid fiber is chopped nanofiber suspension；Then polydiene propyl dichloromethyl ammonium salt solution is configured, takes isometric contraposition virtue
Be chopped nanofiber suspension and polydiene propyl dichloromethyl ammonium salt solution interval of synthetic fibre is carried out layer by layer using vacuum filtration mode
Assembling, reuses deionized water and ethyl alcohol is respectively washed after assembling, finally air-dried by squeezing, room temperature up to nanometer aramid fiber
Film.
The features of the present invention also resides in,
The mass ratio of the potassium hydroxide and p-aramid fiber chopped strand is 3：2.
The potassium hydroxide and p-aramid fiber chopped strand quality sum are added to the ratio in the dimethyl sulphoxide solution
Example is 1g/ (200-500ml).
The mixing speed turns/min for (600-800), and mixing time is 7 days or 7 days or more.
The polydiene propyl dichloromethyl ammonium salt solution mass fraction of configuration is 1%.
The p-aramid fiber is chopped nanofiber suspension and polydiene propyl dichloromethyl ammonium salt solution interval using true
Empty bottle,suction carries out layer assembly using the mode of vacuum filtration.
It is 10-15min that pressure is squeezed during the squeezing processing no more than 4MPa, squeezing time.
The beneficial effects of the invention are as follows：A kind of nanometer aramid fiber film based on vacuum aided LBL self-assembly of the present invention
Preparation method solves the problems, such as existing LBL methods preparation nanometer aramid fiber film, and time-consuming, film forming difficulty is big.One kind of the present invention
The preparation method of nanometer aramid fiber film based on vacuum aided LBL self-assembly utilizes the method for vacuum aided self-service dress layer by layer, system
It is standby go out the aramid fiber nano thin-film that has excellent performance, this method is easy to operate, and number of repetition greatly shortens, ultrahigh in efficiency, while energy
The introducing of other components is greatly reduced, the excellent properties of nanometer aramid fiber is given full play to, widens it in other materials field
Development and application.
Description of the drawings
Fig. 1 is made using a kind of preparation method of the nanometer aramid fiber film based on vacuum aided LBL self-assembly of the present invention
Nanometer aramid fiber film clarity demonstration graph；
Fig. 2 is made using a kind of preparation method of the nanometer aramid fiber film based on vacuum aided LBL self-assembly of the present invention
The static state of nanometer aramid fiber film wash rear contact angle figure.
Specific embodiment
The preparation method of a kind of nanometer aramid fiber film based on vacuum aided LBL self-assembly provided by the invention, including step
Suddenly：
According to mass ratio 3：2 weigh potassium hydroxide (KOH) and p-aramid fiber chopped strand (PPTA) respectively after be added to two
In methyl sulfoxide (DMSO) solution, the quality sum of KOH and PPTA are added to the ratio of DMSO solution as 1g/ (200-500) ml,
The sum of KOH and PPTA for being dissolved in DMSO solution i.e. per 200-500ml are 1g, then turn/min at room temperature with 600-800
Speed stir 7 days or 7 days kermesinus derived above p-aramid fiber be chopped nanofiber (aramid nano-fiber, referred to as
ANF) suspension；Then configuration quality fraction is 1% polydiene propyl dichloromethyl ammonium (PDDA) solution, then takes and waits bodies
Long-pending ANF suspension and PDDA solution interval carry out layer assembly using bottle is filtered by vacuum using the mode of vacuum filtration, assembling
After reuse deionized water and ethyl alcohol is respectively washed, finally air-dried by squeezing, room temperature up to nanometer aramid fiber film.Squeezing
It is 10-15min that pressure is squeezed during processing no more than 4MPa, squeezing time.
It is received using made from a kind of preparation method of the nanometer aramid fiber film based on vacuum aided LBL self-assembly of the present invention
Meter Fang Lun films, mechanics relevant parameter are as shown in table 1：
1 nanometer of aramid fiber thin film mechanics relevant parameter of table
It is received using made from a kind of preparation method of the nanometer aramid fiber film based on vacuum aided LBL self-assembly of the present invention
Meter Fang Lun films are in faint yellow, have good transparent performance (can pass through the film from Fig. 1 and see Chinese character and letter), compared with
Good hydrophilicity (as shown in Figure 2) and excellent mechanical property (as shown in Table 1).
With reference to specific embodiment, the present invention is described in detail.
Embodiment 1
A kind of preparation method of nanometer aramid fiber film based on vacuum aided LBL self-assembly of the present embodiment includes step：
Be added to after weighing 0.3g KOH and 0.2g PPTA respectively in 100ml dimethyl sulfoxide (DMSO)s (DMSO) solution, then at room temperature with
The speed of 600 turns/min stirs the 12 days ANF suspension for obtaining kermesinus；Then 80ml is configured, the PDDA that mass fraction is 1%
Solution then takes the ANF suspension of 20ml and the PDDA solution interval of 20ml to use vacuum filtration using bottle is filtered by vacuum every time
Mode carry out layer assembly, deionized water is reused after assembling and ethyl alcohol is respectively washed, finally by squeezing, room temperature wind
Dry nanometer aramid fiber film to obtain the final product.Squeezing pressure is 4MPa during squeezing processing, the squeezing time is 10min.
It it is, of course, also understood that can be according to the number of plies for the nanometer aramid fiber film to be prepared, to determine title every time
The ANF suspension and the volume of PDDA solution that take account for the volume fraction of respective solution.
Embodiment 2
A kind of preparation method of nanometer aramid fiber film based on vacuum aided LBL self-assembly of the present embodiment includes step：
Be added to after weighing 0.3g KOH and 0.2g PPTA respectively in 140ml dimethyl sulfoxide (DMSO)s (DMSO) solution, then at room temperature with
The speed of 650 turns/min stirs the 10 days ANF suspension for obtaining kermesinus；Then 120ml is configured, mass fraction is 1%
PDDA solution then takes the ANF suspension of 20ml and the PDDA solution interval of 20ml to use vacuum using bottle is filtered by vacuum every time
The mode of suction filtration carries out layer assembly, and deionized water is reused after assembling and ethyl alcohol is respectively washed, finally by squeezing, room
Warm air is done up to nanometer aramid fiber film.Squeezing pressure is 3.5MPa during squeezing processing, the squeezing time is 11min.
Embodiment 3
A kind of preparation method of nanometer aramid fiber film based on vacuum aided LBL self-assembly of the present embodiment includes step：
Be added to after weighing 0.3g KOH and 0.2g PPTA respectively in 180ml dimethyl sulfoxide (DMSO)s (DMSO) solution, then at room temperature with
The speed of 700 turns/min stirs the 8 days ANF suspension for obtaining kermesinus；Then 160ml is configured, the PDDA that mass fraction is 1%
Solution then takes the ANF suspension of 20ml and the PDDA solution interval of 20ml to use vacuum filtration using bottle is filtered by vacuum every time
Mode carry out layer assembly, deionized water is reused after assembling and ethyl alcohol is respectively washed, finally by squeezing, room temperature wind
Dry nanometer aramid fiber film to obtain the final product.Specifically, squeezing pressure is 3.4MPa during squeezing processing, the squeezing time is 12min.
Embodiment 4
A kind of preparation method of nanometer aramid fiber film based on vacuum aided LBL self-assembly of the present embodiment includes step：
Be added to after weighing 0.3g KOH and 0.2g PPTA respectively in 200ml dimethyl sulfoxide (DMSO)s (DMSO) solution, then at room temperature with
The speed of 750 turns/min stirs the 8 days ANF suspension for obtaining kermesinus；Then 160ml is configured, the PDDA that mass fraction is 1%
Solution then takes the ANF suspension of 40ml and the PDDA solution interval of 40ml to use vacuum filtration using bottle is filtered by vacuum every time
Mode carry out layer assembly, deionized water is reused after assembling and ethyl alcohol is respectively washed, finally by squeezing, room temperature wind
Dry nanometer aramid fiber film to obtain the final product.Squeezing pressure is 3.3MPa during squeezing processing, the squeezing time is 13min.
Embodiment 5
A kind of preparation method of nanometer aramid fiber film based on vacuum aided LBL self-assembly of the present embodiment includes step：
Be added to after weighing 0.3g KOH and 0.2g PPTA respectively in 250ml dimethyl sulfoxide (DMSO)s (DMSO) solution, then at room temperature with
The speed of 800 turns/min stirs the 7 days ANF suspension for obtaining kermesinus；Then 200ml is configured, the PDDA that mass fraction is 1%
Solution then takes the ANF suspension of 50ml and the PDDA solution interval of 50ml to use vacuum filtration using bottle is filtered by vacuum every time
Mode carry out layer assembly, deionized water is reused after assembling and ethyl alcohol is respectively washed, finally by squeezing, room temperature wind
Dry nanometer aramid fiber film to obtain the final product.Squeezing pressure is 3MPa during squeezing processing, the squeezing time is 15min.
It is received using made from a kind of preparation method of the nanometer aramid fiber film based on vacuum aided LBL self-assembly of the present invention
Meter Fang Lun films are that the obtained a kind of nanofiber of specially treated is carried out to the p-aramid fiber chopped strand of macroscopic view, though size
So Nano grade, but still maintain molecular structure and macroscopic fibres this height of macroscopic view crystallinity and high-modulus,
The excellent properties such as high intensity, therefore be usually introduced into it as reinforcing agent among some polymer.
Claims (7)
1. a kind of preparation method of the nanometer aramid fiber film based on vacuum aided LBL self-assembly, which is characterized in that including step：
Potassium hydroxide and p-aramid fiber chopped strand are added in dimethyl sulphoxide solution, are stirred at room temperature to obtain contraposition virtue
Synthetic fibre is chopped nanofiber suspension；Then polydiene propyl dichloromethyl ammonium salt solution is configured, takes isometric p-aramid fiber short
It cuts nanofiber suspension and polydiene propyl dichloromethyl ammonium salt solution interval and carries out layer assembly using vacuum filtration mode,
Deionized water is reused after assembling and ethyl alcohol is respectively washed, is finally air-dried by squeezing, room temperature up to nanometer aramid fiber film.
2. a kind of preparation method of the nanometer aramid fiber film based on vacuum aided LBL self-assembly as described in claim 1,
It is characterized in that, the mass ratio of the potassium hydroxide and p-aramid fiber chopped strand is 3：2.
3. a kind of preparation method of the nanometer aramid fiber film based on vacuum aided LBL self-assembly as claimed in claim 1 or 2,
It is characterized in that, the potassium hydroxide and p-aramid fiber chopped strand quality sum are added in the dimethyl sulphoxide solution
Ratio is 1g/ (200-500ml).
4. a kind of preparation method of the nanometer aramid fiber film based on vacuum aided LBL self-assembly as described in claim 1,
It is characterized in that, the mixing speed turns/min for (600-800), and mixing time is 7 days or 7 days or more.
5. a kind of preparation method of the nanometer aramid fiber film based on vacuum aided LBL self-assembly as described in claim 1,
It is characterized in that, the polydiene propyl dichloromethyl ammonium salt solution mass fraction of configuration is 1%.
6. a kind of preparation method of the nanometer aramid fiber film based on vacuum aided LBL self-assembly as described in claim 1,
It is characterized in that, the p-aramid fiber is chopped nanofiber suspension and polydiene propyl dichloromethyl ammonium salt solution interval using true
Empty bottle,suction carries out layer assembly using the mode of vacuum filtration.
7. a kind of preparation method of the nanometer aramid fiber film based on vacuum aided LBL self-assembly as described in claim 1,
It is characterized in that, the squeezing squeezes pressure no more than 4MPa, squeezing time when handling be 10-15min.
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Cited By (7)
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| CN109385928A (en) * | 2018-11-02 | 2019-02-26 | 陕西科技大学 | A kind of nano-cellulose/aramid nano-fiber film composite Nano paper and preparation method thereof |
| CN109468882A (en) * | 2018-10-18 | 2019-03-15 | 华南理工大学 | A kind of manufacturing method of gradient-structure nanometer aramid paper |
| CN110117416A (en) * | 2019-04-19 | 2019-08-13 | 陕西科技大学 | A kind of Ti2C3/ p-aramid fiber nanofiber electromagnetic shielding composite material and preparation method thereof |
| CN110655668A (en) * | 2019-10-25 | 2020-01-07 | 陕西科技大学 | Hydroxyapatite nanowire/ANF composite film and preparation method and application thereof |
| CN111244366A (en) * | 2020-01-20 | 2020-06-05 | 哈尔滨工业大学 | Preparation method of lithium-sulfur battery diaphragm based on multilayer aramid nanofibers |
| CN114805879A (en) * | 2022-05-31 | 2022-07-29 | 陕西科技大学 | Aramid nanofiber-based insulating composite film and preparation method and application thereof |
| CN115418885A (en) * | 2022-09-15 | 2022-12-02 | 黄河三角洲京博化工研究院有限公司 | Low-dielectric-loss aramid paper and preparation method thereof |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109468882A (en) * | 2018-10-18 | 2019-03-15 | 华南理工大学 | A kind of manufacturing method of gradient-structure nanometer aramid paper |
| CN109385928A (en) * | 2018-11-02 | 2019-02-26 | 陕西科技大学 | A kind of nano-cellulose/aramid nano-fiber film composite Nano paper and preparation method thereof |
| CN109385928B (en) * | 2018-11-02 | 2021-04-06 | 陕西科技大学 | Nano cellulose/aramid nano fiber film composite nano paper and preparation method thereof |
| CN110117416A (en) * | 2019-04-19 | 2019-08-13 | 陕西科技大学 | A kind of Ti2C3/ p-aramid fiber nanofiber electromagnetic shielding composite material and preparation method thereof |
| CN110117416B (en) * | 2019-04-19 | 2022-08-19 | 陕西科技大学 | Ti 2 C 3 Electromagnetic shielding composite material of/para-aramid nano-fiber and preparation method thereof |
| CN110655668A (en) * | 2019-10-25 | 2020-01-07 | 陕西科技大学 | Hydroxyapatite nanowire/ANF composite film and preparation method and application thereof |
| CN111244366A (en) * | 2020-01-20 | 2020-06-05 | 哈尔滨工业大学 | Preparation method of lithium-sulfur battery diaphragm based on multilayer aramid nanofibers |
| CN114805879A (en) * | 2022-05-31 | 2022-07-29 | 陕西科技大学 | Aramid nanofiber-based insulating composite film and preparation method and application thereof |
| CN114805879B (en) * | 2022-05-31 | 2023-09-19 | 陕西科技大学 | Aramid nanofiber-based insulation composite film and preparation method and application thereof |
| CN115418885A (en) * | 2022-09-15 | 2022-12-02 | 黄河三角洲京博化工研究院有限公司 | Low-dielectric-loss aramid paper and preparation method thereof |
| CN115418885B (en) * | 2022-09-15 | 2023-09-01 | 黄河三角洲京博化工研究院有限公司 | Low-dielectric-loss aramid paper and preparation method thereof |
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