CN113862816A - Preparation method of short rod-shaped aramid nanofiber, aramid nanofiber and application - Google Patents
Preparation method of short rod-shaped aramid nanofiber, aramid nanofiber and application Download PDFInfo
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- CN113862816A CN113862816A CN202111186491.XA CN202111186491A CN113862816A CN 113862816 A CN113862816 A CN 113862816A CN 202111186491 A CN202111186491 A CN 202111186491A CN 113862816 A CN113862816 A CN 113862816A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
- D01F6/605—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides from aromatic polyamides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/04—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers
- D01F11/08—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
Abstract
The invention discloses a preparation method of short rod-shaped aramid nano-fiber, the aramid nano-fiber and application, and belongs to the technical field of polymer nano-materials. The diameter of the aramid nanofiber prepared by the invention is 100-800nm short rod-shaped aramid nanofiber. The preparation method comprises the steps of placing para-aramid fibers into a PFI machine for beating, adding obtained slurry into a KOH solution, heating, stirring and dispersing uniformly, then carrying out vacuum filtration and washing on the obtained aramid fiber dispersion body to be alkalescent, and finally placing the aramid fiber dispersion body into a steam explosion feeding bin to obtain the aramid nanofibers by adjusting and controlling the pressure, time and other conditions. The aramid nano-fiber prepared by the method is in a short rod shape and can be dispersed in water or a hydrophilic solvent, so that the diversified application of the aramid nano-fiber is greatly expanded. The preparation method does not use organic solvent, is environment-friendly, and has the advantages of low cost, high treatment efficiency, simple process, mechanical method as main preparation method, and suitability for large-scale process production.
Description
Technical Field
The invention belongs to the technical field of polymer nano materials, and particularly relates to a preparation method of short rod-shaped aramid nano fibers, the aramid nano fibers and application.
Background
The one-dimensional aramid fiber, particularly the aramid nanofiber ANF, not only maintains the excellent properties of light weight, high strength, high temperature resistance, corrosion resistance, high flame retardance and insulativity of the macroscopic aramid fiber PPTA fiber, but also has the unique nano effect, large length-width ratio, high specific surface area and excellent mechanical properties of the polymer nanofiber. It can be used as one of the most promising building blocks which are comparable with carbon nano tube CNTs and cellulose nano fiber. The nano-scale ANF brings mechanical properties and optical properties which cannot be realized by aramid fibers. In addition, the abundant active groups on the surface, the large length-diameter ratio and the specific surface area of the ANF endow the ANF with excellent characteristics of the nano material.
The PPTA fiber is an excellent high-performance chemical fiber with high strength, excellent flame retardant property, good heat resistance and good chemical stability, and is an important material in the fields of national defense, aerospace, petrochemical industry and the like. The characteristics of high strength and high temperature resistance of the aramid fiber are endowed by a rigid chain structure formed by pi-pi conjugation among partial sub-chains in the aramid fiber, intermolecular hydrogen bonds, van der waals acting force and the like, but the surface active groups of the aramid fiber are also few, and the aramid fiber is difficult to be compounded with other materials, so that the application of the aramid fiber in the fields of composite materials, nano materials, biomedical materials and the like is limited. Aramid nanofibers are a polymer nanofiber material that has emerged in this year. First, in a chemical alkali dissolution method (Yang M, Cao K, Sui L, et al. Dispersions of aromatic nanofibers: a new nanoscale building block [ J ]. Acs Nano, 2011, 5 (9): 6945-54.) taught by the teaching of the American group of Nicholas A.Kotov, the dispersion of ANFs/DMSO was obtained by mixing the aramid fiber with KOH and dimethyl sulfoxide and continuously stirring at room temperature for 7-10 days. Although the aramid nano-fiber prepared by the deprotonation method has obvious advantages in the aspects of diameter and distribution, nano-fiber quality and method operability, the aramid nano-fiber is applied by extensive researchers. However, the process of preparing the aramid nanofibers by deprotonation reaction of the aramid fibers has the problems of long reaction period (7-10 days), low reaction concentration (generally 0.2% by mass concentration) and the like. And the size of the aramid nano-fiber is increased in the replacement process of the ANF from the DMSO, and even part of the ANF is reduced into macroscopic aramid fiber, so that the superiority of the nano-structure of the ANF is greatly destroyed.
The application range of the aramid nano fiber is really widened by dispersing the aramid nano fiber in the organic solvent, but the organic solvent has large pollution to the environment, so that the environment is bound to be damaged if the aramid nano fiber material is applied in a large scale, and meanwhile, the aramid nano fiber cannot be well blended with the water-soluble polymer because the aramid nano fiber cannot be dispersed in water, so that the application of the aramid nano fiber in the water-soluble polymer and the hydrophilic material is limited. The special performance of the nano material is closely related to the appearance of the nano particles, in order to fully utilize the excellent performance of the aramid fiber and prepare the high-performance composite material, the research and development process is simple, the cost is low, and the novel aramid fiber nano material suitable for large-scale industrial use is an urgent need of the market.
Disclosure of Invention
The invention provides a preparation method of short rod-shaped aramid nano-fiber and application thereof, aiming at overcoming the defects of overlong reaction period, low yield, environmental pollution caused by organic solvent and the like in the prior art for preparing the aramid nano-fiber.
In order to achieve the technical purpose, the technical scheme adopted by the invention is as follows:
a preparation method of short rod-shaped aramid nanofibers comprises the following steps:
(1) adding water into para-aramid fibers, placing the para-aramid fibers in a PFI machine, and pulping to obtain para-aramid fibers A;
(2) adding para-aramid fiber A into a KOH aqueous solution to obtain a para-aramid fiber A and KOH aqueous solution mixed system, and heating and stirring the para-aramid fiber A and the KOH aqueous solution in a water bath to obtain para-aramid fiber dispersoid A;
(3) performing vacuum suction filtration and washing on the para-aramid fiber dispersoid A obtained in the step (2) to be alkalescent to obtain para-aramid fiber dispersoid B;
(4) and (4) putting the para-aramid fiber dispersoid B obtained in the step (3) into a steam explosion feeding bin for point explosion to obtain a short rod-shaped aramid nanofiber aqueous solution, and drying to obtain a final product.
Further, in the step (1), the para-aramid fiber is para-chopped fiber with the average length of 1-10mm, and the mass concentration of the para-aramid fiber is 1-20%.
Further, in the step (2), 2-5g of para-aramid fiber and 10-100 g of KOH are added into every 100mL of water.
Further, the temperature of the water bath in the step (2) is maintained at 50-80 ℃, the stirring speed is 200-.
Further, the pH value of the para-aramid fiber dispersion B after suction filtration in the step (3) is 8-12.
Further, 2.8-3.6L of water is introduced into the step (4), the bursting pressure is 0.5-3.5MPa, and the maintaining time is 1-20 min.
Further, the drying mode in the step (4) is spray drying or freeze drying.
A short rod-shaped aramid nanofiber prepared by the preparation method.
An application of a preparation method of short rod-shaped aramid nano-fiber in the preparation of nano-materials.
Advantageous effects
The method for efficiently preparing the aramid nano-fiber by adopting the new process and the new method solves the problems of overlong reaction time, low preparation efficiency, incapability of dispersing the aramid nano-fiber in water and the like in the prior art. The method for quickly and efficiently preparing the novel aramid nano-fiber is simple and convenient to operate, can quickly and successfully prepare the aramid nano-fiber, greatly shortens the reaction period, improves the production efficiency, realizes batch preparation of the aramid nano-fiber, is expected to promote large-scale production and diversified application of the aramid nano-fiber, and has extremely high market popularization value.
Drawings
Fig. 1 is a transmission electron microscope SEM image of the aramid nanofibers obtained in example 6 of the present invention;
fig. 2 is a TEM image of the aramid nanofibers obtained in example 6 of the present invention.
Detailed Description
The technical solution of the present invention is further described below with reference to specific embodiments, but is not limited thereto.
Example 1
A preparation method of short rod-shaped aramid nanofibers comprises the following steps:
(1) putting 20g of oven-dried para-aramid fiber with the average length of 3mm into a beaker, adding water to 200g, uniformly mixing, adding into a PFI beater, and beating at the beating speed of 5000r to obtain para-aramid fiber A;
(2) adding 50mL of water into 1g of para-aramid fiber A and 5g of KOH in a beaker, placing the beaker in a water bath kettle, and stirring with the help of a stirrer to obtain a para-aramid fiber dispersoid A; the treatment conditions are as follows: the water bath temperature is 80 ℃, the rotating speed of the stirrer is 500r, and the processing time is 3 h;
(3) carrying out vacuum filtration on the para-aramid fiber dispersoid A obtained in the step (2) until the pH value is 8, so as to obtain a para-aramid fiber dispersoid B;
(4) putting the para-aramid fiber dispersoid B obtained in the step (3) into a steam explosion feeding bin for point explosion to obtain a short rod-shaped aramid nanofiber aqueous solution, and drying to obtain a final product; the steam explosion treatment conditions are as follows: 3.6L of water is introduced, the bursting pressure is 1.5MPa, and the maintaining time is 5 min.
Example 2
A preparation method of short rod-shaped aramid nanofibers comprises the following steps:
(1) putting 20g of oven-dried para-aramid fiber with the average length of 1mm into a beaker, adding water to 200g, uniformly mixing, adding into a PFI beater, and beating at 10000r to obtain para-aramid fiber A;
(2) taking 1g of para-aramid fiber A, adding 10g of KOH into 50mL of water in a beaker;
(3) placing the beaker containing the para-aramid fiber and KOH solution system obtained in the step (2) in a water bath kettle, and stirring with the help of a stirrer to obtain a para-aramid fiber dispersoid A; the treatment conditions are as follows: the water bath temperature is 80 ℃, the rotating speed of the stirrer is 500r, and the processing time is 3 h;
(4) carrying out vacuum filtration on the para-aramid fiber dispersoid A obtained in the step (3) until the pH value is 8, so as to obtain a para-aramid fiber dispersoid B;
(5) putting the para-aramid fiber dispersoid B obtained in the step (4) into a steam explosion feeding bin for point explosion to obtain a short rod-shaped aramid nanofiber aqueous solution, and drying to obtain a final product; the steam explosion treatment conditions are as follows: 3.6L of water is introduced, the bursting pressure is 2.0MPa, and the maintaining time is 10 min.
Example 3
A preparation method of short rod-shaped aramid nanofibers comprises the following steps:
(1) putting 20g of oven-dried para-aramid fiber with the average length of 1mm into a beaker, adding water to 200g, uniformly mixing, adding into a PFI beater, and beating at the speed of 20000r to obtain para-aramid fiber A;
(2) taking 1g of para-aramid fiber A, adding 20g of KOH into 50mL of water in a beaker;
(3) placing the beaker containing the para-aramid fiber and KOH solution system obtained in the step (2) in a water bath kettle, and stirring with the help of a stirrer to obtain a para-aramid fiber dispersoid A; the treatment conditions are as follows: the water bath temperature is 80 ℃, the rotating speed of the stirrer is 500r, and the processing time is 3 h;
(4) carrying out vacuum filtration on the para-aramid fiber dispersoid A obtained in the step (3) until the pH value is 8, so as to obtain a para-aramid fiber dispersoid B;
(5) putting the para-aramid fiber dispersoid B obtained in the step (4) into a steam explosion feeding bin for point explosion to obtain a short rod-shaped aramid nanofiber aqueous solution, and drying to obtain a final product; the steam explosion treatment conditions are as follows: 3.6L of water is introduced, the bursting pressure is 2.0MPa, and the maintaining time is 10 min.
Example 4
A preparation method of short rod-shaped aramid nanofibers comprises the following steps:
(1) putting 20g of oven-dried para-aramid fiber with the average length of 1mm into a beaker, adding water to 200g, uniformly mixing, adding into a PFI beater, and beating at the rotating speed of 50000r to obtain para-aramid fiber A;
(2) taking 1g of para-aramid fiber A, adding 50mL of water into 50g of KOH, and putting the mixture into a beaker;
(3) placing the beaker containing the para-aramid fiber and KOH solution system obtained in the step (2) in a water bath kettle, and stirring with the help of a stirrer to obtain a para-aramid fiber dispersoid A; the treatment conditions are as follows: the water bath temperature is 80 ℃, the rotating speed of the stirrer is 500r, and the processing time is 3 h;
(4) carrying out vacuum filtration on the para-aramid fiber dispersoid A obtained in the step (3) until the pH value is 8, so as to obtain a para-aramid fiber dispersoid B;
(5) putting the para-aramid fiber dispersoid B obtained in the step (4) into a steam explosion feeding bin for point explosion to obtain a short rod-shaped aramid nanofiber aqueous solution, and drying to obtain a final product; the steam explosion treatment conditions are as follows: 3.6L of water is introduced, the bursting pressure is 2.0MPa, and the maintaining time is 10 min.
Example 5
A preparation method of short rod-shaped aramid nanofibers comprises the following steps:
(1) putting 20g of oven-dried para-aramid fiber with the average length of 1mm into a beaker, adding water to 200g, uniformly mixing, adding into a PFI beater, and beating at the rotating speed of 50000r to obtain para-aramid fiber A;
(2) taking 1g of para-aramid fiber A, adding 50mL of water into 30g of KOH, and putting the mixture into a beaker;
(3) placing the beaker containing the para-aramid fiber and KOH solution system obtained in the step (2) in a water bath kettle, and stirring with the help of a stirrer to obtain a para-aramid fiber dispersoid A; the treatment conditions are as follows: the water bath temperature is 80 ℃, the rotating speed of the stirrer is 500r, and the processing time is 3 h;
(4) carrying out vacuum filtration on the para-aramid fiber dispersoid A obtained in the step (3) until the pH value is 8, so as to obtain a para-aramid fiber dispersoid B;
(5) putting the para-aramid fiber dispersoid B obtained in the step (4) into a steam explosion feeding bin for point explosion to obtain a short rod-shaped aramid nanofiber aqueous solution, and drying to obtain a final product; the steam explosion treatment conditions are as follows: 3.6L of water is introduced, the bursting pressure is 2.0MPa, and the maintaining time is 10 min.
Example 6
A preparation method of short rod-shaped aramid nanofibers comprises the following steps:
(1) putting 20g of oven-dried para-aramid fiber with the average length of 1mm into a beaker, adding water to 200g, uniformly mixing, adding into a PFI beater, and beating at the rotating speed of 50000r to obtain para-aramid fiber A;
(2) taking 1g of para-aramid fiber A, adding 50mL of water into 50g of KOH, and putting the mixture into a beaker;
(3) placing the beaker containing the para-aramid fiber and KOH solution system obtained in the step (2) in a water bath kettle, and stirring with the help of a stirrer to obtain a para-aramid fiber dispersoid A; the treatment conditions are as follows: the water bath temperature is 80 ℃, the rotating speed of the stirrer is 500r, and the processing time is 3 h;
(4) carrying out vacuum filtration on the para-aramid fiber dispersoid A obtained in the step (3) until the pH value is 12, so as to obtain a para-aramid fiber dispersoid B;
(5) putting the para-aramid fiber dispersoid B obtained in the step (4) into a steam explosion feeding bin for point explosion to obtain a short rod-shaped aramid nanofiber aqueous solution, and drying to obtain a final product; the steam explosion treatment conditions are as follows: 3.6L of water is introduced, the bursting pressure is 2.5MPa, and the maintaining time is 20 min.
The product obtained in the example 6 is subjected to scanning electron microscope and transmission electron microscope analysis for morphological characteristics, as shown in fig. 1-2, and as can be seen from fig. 1-2, the obtained nanofiber has uniform size and clear boundary, presents an obvious short rod-like shape, is uniformly dispersed without agglomeration and agglomeration, can effectively solve the problems in the prior art, and can fully prove the superiority of the preparation method, the method for preparing the aramid nanofiber completely meets the requirements of large-scale popularization and application in market, and has wide prospect.
Example 7
A preparation method of short rod-shaped aramid nanofibers comprises the following steps:
(1) putting 20g of oven-dried para-aramid fiber with the average length of 1mm into a beaker, adding water to 200g, uniformly mixing, adding into a PFI beater, and beating at the rotating speed of 50000r to obtain para-aramid fiber A;
(2) taking 1g of para-aramid fiber A, adding 50mL of water into 50g of KOH, and putting the mixture into a beaker;
(3) placing the beaker containing the para-aramid fiber and KOH solution system obtained in the step (2) in a water bath kettle, and stirring with the help of a stirrer to obtain a para-aramid fiber dispersoid A; the treatment conditions are as follows: the water bath temperature is 80 ℃, the rotating speed of the stirrer is 500r, and the processing time is 3 h;
(4) carrying out vacuum filtration on the para-aramid fiber dispersoid A obtained in the step (3) until the pH value is 8, so as to obtain a para-aramid fiber dispersoid B;
(5) putting the para-aramid fiber dispersoid B obtained in the step (4) into a steam explosion feeding bin for point explosion to obtain a short rod-shaped aramid nanofiber aqueous solution, and drying to obtain a final product; the steam explosion treatment conditions are as follows: 3.6L of water is introduced, the bursting pressure is 2.5MPa, and the maintaining time is 5 min.
Example 8
A preparation method of short rod-shaped aramid nanofibers comprises the following steps:
(1) putting 20g of oven-dried para-aramid fiber with the average length of 3mm into a beaker, adding water to 200g, uniformly mixing, adding into a PFI beater, and beating at the rotating speed of 50000r to obtain para-aramid fiber A;
(2) taking 1g of para-aramid fiber A, adding 50mL of water into 50g of KOH, and putting the mixture into a beaker;
(3) placing the beaker containing the para-aramid fiber and KOH solution system obtained in the step (2) in a water bath kettle, and stirring with the help of a stirrer to obtain a para-aramid fiber dispersoid A; the treatment conditions are as follows: the water bath temperature is 80 ℃, the rotating speed of the stirrer is 500r, and the processing time is 3 h;
(4) carrying out vacuum filtration on the para-aramid fiber dispersoid A obtained in the step (3) until the pH value is 8, so as to obtain a para-aramid fiber dispersoid B;
(5) putting the para-aramid fiber dispersoid B obtained in the step (4) into a steam explosion feeding bin for point explosion to obtain a short rod-shaped aramid nanofiber aqueous solution, and drying to obtain a final product; the steam explosion treatment conditions are as follows: 3.6L of water is introduced, the bursting pressure is 2.5MPa, and the maintaining time is 10 min.
It should be noted that the above-mentioned embodiments are only some of the preferred modes for implementing the invention, and not all of them. Obviously, all other embodiments obtained by persons of ordinary skill in the art based on the above-mentioned embodiments of the present invention without any creative effort shall fall within the protection scope of the present invention.
Claims (9)
1. A preparation method of short rod-shaped aramid nanofibers comprises the following steps:
(1) adding water into para-aramid fibers, placing the para-aramid fibers in a PFI machine, and pulping to obtain para-aramid fibers A;
(2) adding para-aramid fiber A into a KOH aqueous solution to obtain a para-aramid fiber A and KOH aqueous solution mixed system, and heating and stirring the para-aramid fiber A and the KOH aqueous solution in a water bath to obtain para-aramid fiber dispersoid A;
(3) performing vacuum suction filtration and washing on the para-aramid fiber dispersoid A obtained in the step (2) to be alkalescent to obtain para-aramid fiber dispersoid B;
(4) and (4) putting the para-aramid fiber dispersoid B obtained in the step (3) into a steam explosion feeding bin for point explosion to obtain a short rod-shaped aramid nanofiber aqueous solution, and drying to obtain a final product.
2. The preparation method of the short rod-shaped aramid nanofiber as claimed in claim 1, wherein the para-aramid fiber in the step (1) is a para-chopped fiber with an average length of 1-10mm, and the mass concentration of the para-aramid fiber is 1% -20%.
3. The method for preparing short rod-shaped aramid nanofibers according to claim 1, wherein 2 to 5g of para-aramid fibers and 10 to 100 g of KOH are added per 100mL of water in step (2).
4. The preparation method of the short rod-shaped aramid nanofiber as claimed in claim 1, wherein the temperature of the water bath in the step (2) is maintained at 50-80 ℃, the stirring speed is 200-500r/min, and the stirring time is 2-5 h.
5. The preparation method of the short rod-shaped aramid nanofibers according to claim 1, wherein the pH of the p-aramid fiber dispersion B after suction filtration in step (3) is 8-12.
6. The preparation method of the short rod-shaped aramid nanofiber as claimed in claim 1, wherein 2.8-3.6L of water is introduced in the step (4), the bursting pressure is 0.5-3.5MPa, and the maintaining time is 1-20 min.
7. The method for preparing short rod-shaped aramid nanofibers according to claim 1, wherein the drying in step (4) is spray drying or freeze drying.
8. A short rodlike aramid nanofiber obtained by the method for preparing a short rodlike aramid nanofiber as claimed in any one of claims 1 to 7.
9. Use of the short rod-shaped aramid nanofibers according to any one of claims 1-7 in the preparation of nanomaterials.
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| CN115029920A (en) * | 2022-06-14 | 2022-09-09 | 天津科技大学 | Preparation method of aramid nanofiber |
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