CN113862816B - Preparation method of short-rod-shaped aramid nanofiber and application - Google Patents
Preparation method of short-rod-shaped aramid nanofiber and application Download PDFInfo
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Abstract
The invention discloses a preparation method of short rod-shaped aramid nanofibers, the aramid nanofibers and application thereof, and belongs to the technical field of polymer nanomaterials. The aramid nanofiber prepared by the invention is a short rod-shaped aramid nanofiber with the diameter of 100-800 nm. The preparation method comprises the steps of pulping para-aramid fibers in a PFI machine, adding the obtained slurry into KOH solution, heating, stirring and dispersing uniformly, then carrying out vacuum filtration on the obtained aramid fiber dispersion to be slightly alkaline, and finally placing the aramid fiber dispersion in a steam explosion feeding bin to obtain the aramid nanofibers through regulating and controlling the pressure, time and other conditions. The aramid nanofiber 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 nanofiber is greatly expanded. The preparation process does not use organic solvent, is environment-friendly, has low cost, high treatment efficiency and simple process, and is suitable for large-scale process production mainly by a mechanical method.
Description
Technical Field
The invention belongs to the technical field of polymer nano materials, and particularly relates to a preparation method of a short rod-shaped aramid nanofiber, the aramid nanofiber and application.
Background
The one-dimensional aramid fiber, in particular the aramid nanofiber ANF, not only maintains the excellent performances 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 nanometer effect, large length-width ratio, high specific surface area and excellent mechanical properties of the polymer nanofiber. It can be one of the most promising building blocks that rivals carbon nanotube CNTs and cellulose nanofibers. Nano-scale ANF is its mechanical and optical properties that are not achieved with aramid fibers. In addition, the active groups, the large length-diameter ratio and the specific surface area of the ANF surface are rich, and the excellent characteristics of the nano material are further provided.
The aramid fiber PPTA 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 rigid chain structure formed by pi-pi conjugate among molecular chains in the aramid fiber, intermolecular hydrogen bond, van der Waals acting force and the like endow the aramid fiber with high strength and high temperature resistance, but the aramid fiber has few surface active groups, is difficult to compound with other materials, and limits the application of the aramid fiber in the fields of composite materials, nano materials, biomedical materials and the like. Aramid nanofibers are a polymeric nanofiber material that has emerged in the present year. The chemical alkali method taught by Nicholas A.Kotov task group, U.S. was first used (Yang M, cao K, sui L, et al Dispersions of aramid nanofibers: a new nanoscale building block [ J ]. Acs Nano, 2011, 5 (9): 6945-54.) to obtain ANFs/DMSO dispersions by mixing aramid fibers with KOH and dimethyl sulfoxide and then stirring continuously at room temperature for 7-10 days. Although the aramid nanofibers prepared by the deprotonation method have obvious advantages in diameter and distribution, nanofiber quality and method operability, the application of the majority of researchers is obtained. However, in the process of preparing the aramid nanofibers by deprotonation of the aramid fibers, there are various problems such as long reaction period (7-10 days), low reaction concentration (generally 0.2% mass concentration), and the like. And the size of the aramid nanofiber is increased in the replacement process of the ANF from the DMSO, and even the aramid nanofiber is partially reduced into macroscopic aramid fibers, so that the superiority of the nanostructure is greatly destroyed.
The aramid nanofibers can be dispersed in the organic solvent, so that the application range of the aramid nanofibers is widened greatly, but the organic solvent has great environmental pollution, if the aramid nanofiber material is used in a large scale, the environment is endangered, and meanwhile, the aramid nanofibers cannot be well blended with the water-soluble polymer because the aramid nanofibers cannot be dispersed in the water, so that the application of the aramid nanofibers in the water-soluble polymer and the hydrophilic material is limited. The special performance of the nano material is closely related to the morphology of the nano particles, and in order to fully utilize the excellent performance of the aramid fiber and prepare the high-performance composite material, the development process is simple, the cost is low, and the novel aramid fiber nano material suitable for large-scale industrial use is an urgent market demand.
Disclosure of Invention
The invention provides a preparation method and application of short-rod-shaped aramid nanofibers, which are used for overcoming the defects of overlong reaction period, low yield, environmental pollution caused by organic solvents and the like in the prior art for preparing the aramid nanofibers, and the method is simple and convenient to operate, can be used for preparing the aramid nanofibers quickly and successfully, greatly shortens the reaction period, and promotes the large-scale production and the multi-element application of the aramid nanofibers.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
the preparation method of the short rod-shaped aramid nanofiber comprises the following steps:
(1) Adding water into the para-aramid fiber, and pulping in a PFI machine to obtain para-aramid fiber A;
(2) Adding para-aramid fiber A into KOH aqueous solution to obtain a mixed system of para-aramid fiber A and KOH aqueous solution, and placing the mixed system in a water bath kettle for heating and stirring treatment to obtain para-aramid fiber dispersion A;
(3) The para-aramid fiber dispersion A obtained in the step (2) is filtered and washed to alkalescence by vacuum to obtain a para-aramid fiber dispersion B;
(4) And (3) putting the para-aramid fiber dispersion 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, the para-aramid fiber in the step (1) 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 100mL of water.
Further, the water bath temperature in the step (2) is maintained at 50-80 ℃, the stirring speed is 200-500r/min, and the stirring time is 2-5h.
Further, the pH of the para-aramid fiber dispersion B after the suction filtration in the step (3) is 8-12.
Further, 2.8-3.6L of water is introduced in the step (4), the bursting pressure is 0.5-3.5MPa, and the maintenance time is 1-20min.
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.
The application of a preparation method of short rod-shaped aramid nanofiber in the preparation of a nanomaterial.
Advantageous effects
The method for efficiently preparing the aramid nanofibers, which is developed by adopting the novel process and the novel method, solves the problems of long reaction time, low preparation efficiency, incapability of dispersing the aramid nanofibers in water and the like in the prior art. The method for rapidly and efficiently preparing the novel aramid nanofibers is simple and convenient to operate, can rapidly and successfully prepare the aramid nanofibers, greatly shortens the reaction period, improves the production efficiency, realizes the mass preparation of the aramid nanofibers, is expected to promote the mass production and the diversified application of the aramid nanofibers, and has extremely high market popularization value.
Drawings
FIG. 1 is a SEM image of an aramid nanofiber obtained in example 6 of the present invention;
fig. 2 is a TEM image of the aramid nanofiber obtained in example 6 of the present invention.
Detailed Description
The technical scheme of the present invention is further described below with reference to specific examples, but is not limited thereto.
Example 1
The preparation method of the short rod-shaped aramid nanofiber comprises the following steps:
(1) Placing 20g of absolute dry para-aramid fiber with the average length of 3mm into a beaker, adding water to 200g, uniformly mixing, adding into a PFI (pulse frequency reactor) beater, and obtaining para-aramid fiber A at the beating speed of 5000 r;
(2) Adding 1g of para-aramid fiber A and 5g of KOH into 50mL of water in a beaker, placing the beaker in a water bath, and stirring by a stirrer to obtain para-aramid fiber dispersion A; the treatment conditions are as follows: the water bath temperature is 80 ℃, the rotation speed of the stirrer is 500r, and the treatment time is 3h;
(3) Vacuum-filtering the para-aramid fiber dispersion A obtained in the step (2) until the pH value is 8 to obtain a para-aramid fiber dispersion B;
(4) Putting the para-aramid fiber dispersion 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 maintenance time is 5min.
Example 2
The preparation method of the short rod-shaped aramid nanofiber comprises the following steps:
(1) Placing absolute dry para-aramid fiber with the average length of 1mm and 20g into a beaker, adding water to 200g, uniformly mixing, adding into a PFI (pulse frequency reactor) beater, and obtaining para-aramid fiber A at the beating speed of 10000 r;
(2) 1g of para-aramid fiber A and 10g of KOH are added 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) into a water bath, and stirring by means of a stirrer to obtain para-aramid fiber dispersion A; the treatment conditions are as follows: the water bath temperature is 80 ℃, the rotation speed of the stirrer is 500r, and the treatment time is 3h;
(4) Vacuum-filtering the para-aramid fiber dispersion A obtained in the step (3) until the pH value is 8 to obtain a para-aramid fiber dispersion B;
(5) Putting the para-aramid fiber dispersion 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 maintenance time is 10min.
Example 3
The preparation method of the short rod-shaped aramid nanofiber comprises the following steps:
(1) Placing absolute dry para-aramid fiber with the average length of 1mm and 20g into a beaker, adding water to 200g, uniformly mixing, adding into a PFI (pulse frequency reactor) beater, and obtaining para-aramid fiber A with the beating speed of 20000 r;
(2) 1g of para-aramid fiber A and 20g of KOH are added 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) into a water bath, and stirring by means of a stirrer to obtain para-aramid fiber dispersion A; the treatment conditions are as follows: the water bath temperature is 80 ℃, the rotation speed of the stirrer is 500r, and the treatment time is 3h;
(4) Vacuum-filtering the para-aramid fiber dispersion A obtained in the step (3) until the pH value is 8 to obtain a para-aramid fiber dispersion B;
(5) Putting the para-aramid fiber dispersion 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 maintenance time is 10min.
Example 4
The preparation method of the short rod-shaped aramid nanofiber comprises the following steps:
(1) Placing absolute dry para-aramid fiber with the average length of 1mm and 20g into a beaker, adding water to 200g, uniformly mixing, adding into a PFI (pulse frequency reactor) beater, and obtaining para-aramid fiber A at the beating speed of 50000 r;
(2) 1g of para-aramid fiber A and 50g of KOH are taken and added into a beaker with 50mL of water;
(3) Placing the beaker containing the para-aramid fiber and KOH solution system obtained in the step (2) into a water bath, and stirring by means of a stirrer to obtain para-aramid fiber dispersion A; the treatment conditions are as follows: the water bath temperature is 80 ℃, the rotation speed of the stirrer is 500r, and the treatment time is 3h;
(4) Vacuum-filtering the para-aramid fiber dispersion A obtained in the step (3) until the pH value is 8 to obtain a para-aramid fiber dispersion B;
(5) Putting the para-aramid fiber dispersion 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 maintenance time is 10min.
Example 5
The preparation method of the short rod-shaped aramid nanofiber comprises the following steps:
(1) Placing absolute dry para-aramid fiber with the average length of 1mm and 20g into a beaker, adding water to 200g, uniformly mixing, adding into a PFI (pulse frequency reactor) beater, and obtaining para-aramid fiber A at the beating speed of 50000 r;
(2) 1g of para-aramid fiber A and 30g of KOH are added 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) into a water bath, and stirring by means of a stirrer to obtain para-aramid fiber dispersion A; the treatment conditions are as follows: the water bath temperature is 80 ℃, the rotation speed of the stirrer is 500r, and the treatment time is 3h;
(4) Vacuum-filtering the para-aramid fiber dispersion A obtained in the step (3) until the pH value is 8 to obtain a para-aramid fiber dispersion B;
(5) Putting the para-aramid fiber dispersion 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 maintenance time is 10min.
Example 6
The preparation method of the short rod-shaped aramid nanofiber comprises the following steps:
(1) Placing absolute dry para-aramid fiber with the average length of 1mm and 20g into a beaker, adding water to 200g, uniformly mixing, adding into a PFI (pulse frequency reactor) beater, and obtaining para-aramid fiber A at the beating speed of 50000 r;
(2) 1g of para-aramid fiber A and 50g of KOH are taken and added into a beaker with 50mL of water;
(3) Placing the beaker containing the para-aramid fiber and KOH solution system obtained in the step (2) into a water bath, and stirring by means of a stirrer to obtain para-aramid fiber dispersion A; the treatment conditions are as follows: the water bath temperature is 80 ℃, the rotation speed of the stirrer is 500r, and the treatment time is 3h;
(4) Vacuum-filtering the para-aramid fiber dispersion A obtained in the step (3) until the pH value is 12 to obtain a para-aramid fiber dispersion B;
(5) Putting the para-aramid fiber dispersion 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 maintenance time is 20min.
The product obtained in the embodiment 6 is subjected to scanning electron microscopy and transmission electron microscopy to analyze the morphological characteristics, as shown in fig. 1-2, as can be seen from fig. 1-2, the obtained nanofiber has uniform size, clear boundary and obvious short bar-shaped morphology, is uniformly dispersed without agglomeration and without caking, can effectively solve the problems existing in the prior art, can fully prove the superiority of the preparation method of the invention, completely meets the requirements of large-scale popularization and application in marketization, and has wide prospect.
Example 7
The preparation method of the short rod-shaped aramid nanofiber comprises the following steps:
(1) Placing absolute dry para-aramid fiber with the average length of 1mm and 20g into a beaker, adding water to 200g, uniformly mixing, adding into a PFI (pulse frequency reactor) beater, and obtaining para-aramid fiber A at the beating speed of 50000 r;
(2) 1g of para-aramid fiber A and 50g of KOH are taken and added into a beaker with 50mL of water;
(3) Placing the beaker containing the para-aramid fiber and KOH solution system obtained in the step (2) into a water bath, and stirring by means of a stirrer to obtain para-aramid fiber dispersion A; the treatment conditions are as follows: the water bath temperature is 80 ℃, the rotation speed of the stirrer is 500r, and the treatment time is 3h;
(4) Vacuum-filtering the para-aramid fiber dispersion A obtained in the step (3) until the pH value is 8 to obtain a para-aramid fiber dispersion B;
(5) Putting the para-aramid fiber dispersion 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 maintenance time is 5min.
Example 8
The preparation method of the short rod-shaped aramid nanofiber comprises the following steps:
(1) Placing 20g of absolute dry para-aramid fiber with the average length of 3mm into a beaker, adding water to 200g, uniformly mixing, adding into a PFI (pulse frequency reactor) beater, and obtaining para-aramid fiber A at the beating speed of 50000 r;
(2) 1g of para-aramid fiber A and 50g of KOH are taken and added into a beaker with 50mL of water;
(3) Placing the beaker containing the para-aramid fiber and KOH solution system obtained in the step (2) into a water bath, and stirring by means of a stirrer to obtain para-aramid fiber dispersion A; the treatment conditions are as follows: the water bath temperature is 80 ℃, the rotation speed of the stirrer is 500r, and the treatment time is 3h;
(4) Vacuum-filtering the para-aramid fiber dispersion A obtained in the step (3) until the pH value is 8 to obtain a para-aramid fiber dispersion B;
(5) Putting the para-aramid fiber dispersion 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 maintenance time is 10min.
It should be noted that the above-mentioned embodiments are merely some, but not all embodiments of the preferred mode of carrying out the invention. It is evident that all other embodiments obtained by a person skilled in the art without making any inventive effort, based on the above-described embodiments of the invention, shall fall within the scope of protection of the invention.
Claims (8)
1. The preparation method of the short rod-shaped aramid nanofiber comprises the following steps:
(1) Adding water into the para-aramid fiber, and pulping in a PFI machine to obtain para-aramid fiber A;
(2) Adding para-aramid fiber A into KOH aqueous solution to obtain a mixed system of para-aramid fiber A and KOH aqueous solution, and placing the mixed system in a water bath kettle for heating and stirring treatment to obtain para-aramid fiber dispersion A;
(3) The para-aramid fiber dispersion A obtained in the step (2) is filtered and washed to alkalescence by vacuum to obtain a para-aramid fiber dispersion B;
(4) Putting the para-aramid fiber dispersion 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;
2.8-3.6L of water is introduced in the step (4), the bursting pressure is 0.5-3.5MPa, and the maintenance time is 1-20min.
2. The method for preparing the short-rod-shaped aramid nanofiber according to 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 2-5g para-aramid fibers and 10-100 g KOH are added per 100mL of water in step (2).
4. The method for preparing short rod-shaped aramid nanofibers according to claim 1, wherein the water bath temperature in the step (2) is maintained at 50-80 ℃, the stirring speed is 200-500r/min, and the stirring time is 2-5h.
5. The method for producing a short rod-shaped aramid nanofiber according to claim 1, wherein the pH of the para-aramid fiber dispersion B after the suction filtration in the step (3) is 8 to 12.
6. The method for preparing short rod-shaped aramid nanofibers according to claim 1, wherein the drying mode in the step (4) is spray drying or freeze drying.
7. A short rod-shaped aramid nanofiber obtained by the method for preparing a short rod-shaped aramid nanofiber according to any one of claims 1 to 6.
8. Use of the method for preparing short rod-shaped aramid nanofibers according to any one of claims 1 to 6 in the preparation of nanomaterials.
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