CN113278172A - Preparation method of cellulose/aramid nano-fiber in-situ composite fiber - Google Patents
Preparation method of cellulose/aramid nano-fiber in-situ composite fiber Download PDFInfo
- Publication number
- CN113278172A CN113278172A CN202110730375.3A CN202110730375A CN113278172A CN 113278172 A CN113278172 A CN 113278172A CN 202110730375 A CN202110730375 A CN 202110730375A CN 113278172 A CN113278172 A CN 113278172A
- Authority
- CN
- China
- Prior art keywords
- fiber
- cellulose
- aramid
- aramid nano
- dispersion liquid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- 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
- C08J5/04—Reinforcing macromolecular compounds with loose or coherent fibrous material
- C08J5/046—Reinforcing macromolecular compounds with loose or coherent fibrous material with synthetic macromolecular fibrous material
-
- 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
- C08J2301/00—Characterised by the use of cellulose, modified cellulose or cellulose derivatives
- C08J2301/02—Cellulose; Modified cellulose
-
- 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
- C08J2477/00—Characterised by the use of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Derivatives of such polymers
- C08J2477/10—Polyamides derived from aromatically bound amino and carboxyl groups of amino carboxylic acids or of polyamines and polycarboxylic acids
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Artificial Filaments (AREA)
- Paper (AREA)
Abstract
The invention discloses a preparation method of cellulose/aramid nano-fiber in-situ composite fiber, which utilizes aramid nano-fiber with unique nano-scale structure, high strength and high modulus, high specific surface area, high length-diameter ratio, good temperature resistance and wet strength as a reinforcement of cellulose, and realizes fiber in-situ protonation reduction and efficient composite by blending aramid nano-fiber/dimethyl sulfoxide dispersion liquid and cellulose fiber to obtain the aramid nano-fiber coated cellulose composite fiber so as to overcome the defects of easy moisture absorption, low wet strength, poor thermal stability, weak ultraviolet shielding property, easy aging and the like of cellulose-based materials. The cellulose/aramid nano-fiber in-situ composite fiber developed by adopting a new process and a new method has the advantages of high specific surface area, high mechanical strength, excellent temperature resistance, excellent ultraviolet shielding and ageing resistance, and wide application prospect.
Description
Technical Field
The invention belongs to the field of composite nanofibers and papermaking, and particularly relates to a preparation method of cellulose/aramid nanofiber in-situ composite fibers.
Background
Plant Cellulose Fiber (CF) is a biomass polymer material which is widely distributed and rich in content in nature, is a renewable biological resource which is widely available, degradable and environment-friendly, and is widely applied to the fields of papermaking, buildings, furniture, clothing and the like which are closely related to human life. Although cellulose fibers have shown wide application prospects in the field of new materials, the new materials prepared from the cellulose fibers have the characteristics of easy moisture absorption and deformation, sensitivity to humidity, poor water resistance, poor dimensional moisture/heat stability, corrosion resistance and easy aging due to the characteristics of natural hydrophilicity, poor temperature resistance, easy combustion, weak chemical stability and the like of the cellulose. For example, paper-based functional materials prepared from cellulose fibers have certain limitations in physicochemical properties, paper structure and performance due to the above problems, and cannot meet the application requirements in high-end fields. Therefore, the high-valued application and comprehensive performance enhancement technology of the cellulose-based material still needs to be further overcome, and a high-performance cellulose-based new material with excellent mechanical strength and hydrophobicity, excellent ultraviolet shielding and ageing resistance and good temperature resistance needs to be developed urgently, so that the service capacity and the service life of the traditional cellulose-based material in severe service environments such as high temperature, high humidity and the like are improved, the product grade is improved, and the requirements of high-end field application are met.
Disclosure of Invention
The invention aims to provide a preparation method of cellulose/aramid nano-fiber in-situ composite fiber, which overcomes the defects of easy moisture absorption, low wet strength, poor thermal stability, weak ultraviolet shielding property, easy aging and the like of cellulose-based materials.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of cellulose/aramid nano-fiber in-situ composite fiber comprises the following steps:
the method comprises the following steps: preparing cellulose fiber/water dispersion and aramid fiber nanofiber/dimethyl sulfoxide dispersion;
step two: adding the aramid nano-fiber/dimethyl sulfoxide dispersion liquid into the cellulose fiber/water dispersion liquid in a high-pressure injection mode, wherein the mass ratio of the aramid nano-fiber to the cellulose fiber is (5-30): (70-95), realizing in-situ protonation reduction of the aramid nano-fiber and effectively compounding the aramid nano-fiber with cellulose fiber to prepare the cellulose/aramid nano-fiber in-situ composite fiber.
Further, the cellulose fiber in the first step is one of softwood pulp board, hardwood pulp board and cotton pulp board.
Further, the cellulose fiber/water dispersion is prepared by the following steps: mixing cellulose fibers with water, pulping, diluting and dispersing to obtain the cellulose fiber/water dispersion with the beating degree of 40-70 DEG SR.
Further, when the cellulose fiber is mixed with water for refining, the refining mass concentration is 10%.
Further, the mass concentration of the cellulose fiber/water dispersion is 0.2-1.5%.
Further, the preparation process of the aramid nanofiber/dimethyl sulfoxide dispersion liquid is as follows: the method comprises the following steps of taking the recovered para-aramid waste as a raw material, and carrying out deprotonation reaction in a potassium hydroxide/dimethyl sulfoxide/water system to obtain an aramid nanofiber/dimethyl sulfoxide dispersion liquid with the mass concentration of 0.2-1.0%.
Furthermore, the recovered para-aramid waste material adopts one or more of aramid cloth, aramid waste silk, aramid yarn and aramid gloves.
And further, in the second step, in the process of adding the aramid nano-fiber/dimethyl sulfoxide dispersion liquid into the cellulose fiber/water dispersion liquid in a high-pressure injection mode, mechanically stirring, after injection is completed, continuously mechanically stirring to obtain a composite fiber mixed dispersion liquid, and performing suction filtration on the composite fiber mixed dispersion liquid through a filter membrane to obtain the cellulose/aramid nano-fiber in-situ composite fiber.
Further, the rotation speed of the mechanical stirring is 800-3500 rpm, and after the injection is finished, the mechanical stirring is continued for 10-60 min.
Further, the cellulose/aramid nano-fiber in-situ composite fiber prepared in the second step has the length of 0.6-1.2 mm and the specific surface area of 8-45 m2/g。
Compared with the prior art, the invention has the following beneficial technical effects:
the aramid nanofiber with a unique nanoscale structure, high strength and modulus, high specific surface area, high length-diameter ratio, good temperature resistance and wet strength is used as a cellulose reinforcement, the defects of easiness in moisture absorption, low wet strength, poor thermal stability, weak ultraviolet shielding property, easiness in aging and the like of the traditional cellulose are overcome, and the aramid nanofiber-coated cellulose composite fiber (ANF @ CF) is obtained, has high specific surface area and mechanical strength, excellent temperature resistance, excellent ultraviolet shielding and aging resistance and wide application prospect.
Secondly, the aramid nano-fiber/dimethyl sulfoxide (ANF/DMSO) dispersion liquid is used as a reinforcement of the cellulose fiber and is injected into the cellulose pulp dispersion liquid in a high-pressure injection mode. Under the action of high shear force, the injected ANF/DMSO is contacted with water in the cellulose pulp to rapidly complete protonation reduction on the surface of cellulose, fine aramid nano-fiber is separated out by uniform ANF/DMSO phase, and the injected ANF/DMSO is deposited on the surface of macroscopic cellulose fiber in situ through a large amount of hydrogen bond actions, the combination of the aramid nano-fiber and the cellulose is completed while the protonation reduction of the aramid nano-fiber is realized, the interface bonding strength of the aramid nano-fiber and the cellulose fiber can be effectively improved, and the high-efficiency and high-strength combination is realized.
The method uses the recovered para-aramid waste materials (aramid cloth, aramid waste silk, aramid yarn and aramid gloves) to replace expensive original aramid fibers as raw materials to prepare the aramid nano fibers, can greatly reduce the preparation cost of the aramid nano fibers, has the molecular weight of 43.0kg/mol, not only can endow the aramid nano fibers with excellent strength performance, but also solves the problems of single expensive source, high preparation cost and the like of the aramid nano fiber raw materials, and lays a foundation for realizing large-scale production and application of the aramid nano fibers.
The novel cellulose composite fiber is prepared by blending the aramid nano-fiber/dimethyl sulfoxide dispersion liquid and the cellulose pulp dispersion liquid in an in-situ composite mode, the preparation process is simple, the flow is short, and large-scale and industrial production can be realized; the obtained novel cellulose composite fiber has excellent comprehensive performance, can solve the scientific and technical problems of the existing cellulose-based material in the high-valued application process, obviously improve the mechanical strength, the thermal stability and the aging resistance of the cellulose-based material, can meet the continuous requirements of high-end fields such as photoelectricity, composite materials, electrical insulation and the like on high-strength, transparent, flexible and aging-resistant materials, and has wide application prospect in the fields of special paper, composite material reinforcement and the like.
Drawings
The accompanying drawings are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
Fig. 1 is an SEM image of the cellulose/aramid nanofiber in-situ composite fiber obtained in example 5 of the present invention.
Detailed Description
The invention is described in further detail below:
a cellulose/aramid nano-fiber in-situ composite fiber is obtained by blending aramid nano-fiber/dimethyl sulfoxide dispersion liquid and cellulose fiber/water dispersion liquid to realize fiber in-situ protonation reduction and compounding; in the cellulose/aramid nano-fiber in-situ composite fiber, the mass ratio of aramid nano-fiber to cellulose fiber is (5-30): (70-95); the cellulose/aramid nano-fiber in-situ composite fiber has the length of 0.6-1.2 mm and the specific surface area of 8-45 m2/g。
A preparation method of cellulose/aramid nano-fiber in-situ composite fiber comprises the following steps:
the method comprises the following steps: preparing cellulose fiber slurry: one of softwood pulp boards, hardwood pulp boards and cotton pulp boards is used as a raw material, grinding is carried out in a grinding machine at the grinding concentration of 10%, the beating degree of the pulp is controlled to be 40-70 DEG SR, and the ground pulp is diluted and dispersed in water to obtain the cellulose fiber pulp with the mass concentration of 0.2-1.5%.
Step two: preparing an aramid nano fiber/dimethyl sulfoxide dispersion liquid: taking recovered para-aramid waste (one or more of aramid cloth, aramid waste silk, aramid yarn and aramid gloves) as a raw material, and adding potassium hydroxide/dimethyl sulfoxide/water (KOH/DMSO/H)2And O) carrying out deprotonation reaction in a system to prepare the aramid nano-fiber/dimethyl sulfoxide dispersion liquid with the mass concentration of 0.2-1.0%.
Step three: in-situ protonation reduction and recombination: placing the cellulose fiber slurry obtained in the step one into a beaker, and injecting the aramid nano-fiber/dimethyl sulfoxide dispersion liquid obtained in the step two into the cellulose fiber slurry through an injector to carry out in-situ protonation reduction and compounding; further, the mass ratio of the aramid nano fiber/dimethyl sulfoxide dispersion liquid to the aramid nano fiber and the cellulose fiber in the cellulose pulp is (5-30): (70-95); further, mechanical stirring is needed in the process of injecting the ANF/DMSO into the cellulose pulp, and the stirring speed is controlled to be 800-3500 rpm; further, after the aramid nano fiber/dimethyl sulfoxide dispersion liquid is injected, continuously mechanically stirring for 10-60 min at the rotating speed of 800-3500 rpm to obtain a composite fiber mixed dispersion liquid; and further, carrying out suction filtration on the obtained composite fiber mixed dispersion liquid through a filter membrane, and intercepting the composite fiber mixed dispersion liquid on the filter membrane to obtain the cellulose/aramid nano fiber in-situ composite fiber.
The present invention will be described in detail with reference to examples. It should be noted that the embodiments and features of the embodiments in the present application may be combined with each other without conflict.
The following detailed description is illustrative of the embodiments and is intended to provide further details of the invention. Unless otherwise defined, all technical terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. The terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention.
Example 1
A cellulose/aramid nano-fiber in-situ composite fiber is obtained by blending aramid nano-fiber/dimethyl sulfoxide dispersion liquid and cellulose fiber/water dispersion liquid to realize fiber in-situ protonation reduction and compounding; in the cellulose/aramid nano-fiber in-situ composite fiber, the mass ratio of the aramid nano-fiber to the cellulose fiber is 5: 95; the length of the cellulose/aramid nano-fiber in-situ composite fiber is 0.6mm, and the specific surface area is 8m2/g。
A preparation method of cellulose/aramid nano-fiber in-situ composite fiber comprises the following steps:
the method comprises the following steps: preparing cellulose fiber slurry: the method comprises the steps of grinding broad-leaved wood pulp boards serving as raw materials in a grinding machine at the grinding concentration of 10%, controlling the beating degree of pulp to be 40 DEG SR, and diluting and dispersing the ground pulp in water to obtain cellulose fiber pulp with the mass concentration of 0.2%.
Step two: preparing an aramid nano fiber/dimethyl sulfoxide dispersion liquid: taking the recovered para-position waste aramid fabric as a raw material, and adding the para-position waste aramid fabric into potassium hydroxide/dimethyl sulfoxide/water (KOH/DMSO/H)2O) is subjected to deprotonation reaction in a system to prepare the aramid nano-fiber/dimethyl sulfoxide dispersion liquid with the mass concentration of 0.2%.
Step three: in-situ protonation reduction and recombination: placing the cellulose fiber slurry obtained in the step one into a beaker, and injecting the aramid nano-fiber/dimethyl sulfoxide dispersion liquid obtained in the step two into the cellulose fiber slurry through an injector to carry out in-situ protonation reduction and compounding; further, the mass ratio of the aramid nano fiber/dimethyl sulfoxide dispersion liquid to the aramid nano fiber to the cellulose fiber in the cellulose pulp is 5: 95; further, mechanical stirring is needed in the process of injecting the ANF/DMSO into the cellulose pulp, and the stirring speed is controlled at 800 rpm; further, after the injection of the aramid nano-fiber/dimethyl sulfoxide dispersion liquid is completed, continuously mechanically stirring for 60min at the rotating speed of 800rpm to obtain a composite fiber mixed dispersion liquid; and further, carrying out suction filtration on the obtained composite fiber mixed dispersion liquid through a filter membrane, and intercepting the composite fiber mixed dispersion liquid on the filter membrane to obtain the cellulose/aramid nano fiber in-situ composite fiber.
Example 2
A cellulose/aramid nano-fiber in-situ composite fiber is obtained by blending aramid nano-fiber/dimethyl sulfoxide dispersion liquid and cellulose fiber/water dispersion liquid to realize fiber in-situ protonation reduction and compounding; in the cellulose/aramid nano-fiber in-situ composite fiber, the mass ratio of the aramid nano-fiber to the cellulose fiber is 10: 90, respectively; the length of the cellulose/aramid nano-fiber in-situ composite fiber is 0.7mm, and the specific surface area is 13m2/g。
A preparation method of cellulose/aramid nano-fiber in-situ composite fiber comprises the following steps:
the method comprises the following steps: preparing cellulose fiber slurry: the softwood pulp board is used as a raw material, the pulp is ground in a grinding machine at the grinding concentration of 10%, the beating degree of the pulp is controlled to be 48 DEG SR, and the ground pulp is diluted and dispersed in water to obtain the cellulose fiber pulp with the mass concentration of 0.4%.
Step two: preparing an aramid nano fiber/dimethyl sulfoxide dispersion liquid: taking recovered para-aramid fabric and aramid waste silk as raw materials, and adding the raw materials into potassium hydroxide/dimethyl sulfoxide/water (KOH/DMSO/H)2O) is subjected to deprotonation reaction in a system to prepare the aramid nano-fiber/dimethyl sulfoxide dispersion liquid with the mass concentration of 0.3%.
Step three: in-situ protonation reduction and recombination: placing the cellulose fiber slurry obtained in the step one into a beaker, and injecting the aramid nano-fiber/dimethyl sulfoxide dispersion liquid obtained in the step two into the cellulose fiber slurry through an injector to carry out in-situ protonation reduction and compounding; further, the mass ratio of the aramid nano fiber/dimethyl sulfoxide dispersion liquid to the aramid nano fiber to the cellulose fiber in the cellulose pulp is 10: 90, respectively; further, mechanical stirring is required in the process of injecting the ANF/DMSO into the cellulose pulp, and the stirring speed is controlled at 1200 rpm; further, after the injection of the aramid nano-fiber/dimethyl sulfoxide dispersion liquid is completed, continuously mechanically stirring for 50min at the rotating speed of 1200rpm to obtain a composite fiber mixed dispersion liquid; and further, carrying out suction filtration on the obtained composite fiber mixed dispersion liquid through a filter membrane, and intercepting the composite fiber mixed dispersion liquid on the filter membrane to obtain the cellulose/aramid nano fiber in-situ composite fiber.
Example 3
A cellulose/aramid nano-fiber in-situ composite fiber is obtained by blending aramid nano-fiber/dimethyl sulfoxide dispersion liquid and cellulose fiber/water dispersion liquid to realize fiber in-situ protonation reduction and compounding; in the cellulose/aramid nano-fiber in-situ composite fiber, the mass ratio of the aramid nano-fiber to the cellulose fiber is 15: 85 parts by weight; the length of the cellulose/aramid nano-fiber in-situ composite fiber is 0.8mm, and the specific surface area is 17m2/g。
A preparation method of cellulose/aramid nano-fiber in-situ composite fiber comprises the following steps:
the method comprises the following steps: preparing cellulose fiber slurry: the softwood pulp board is used as a raw material, the pulp is ground in a grinding machine at the grinding concentration of 10%, the beating degree of the pulp is controlled to be 55 DEG SR, and the ground pulp is diluted and dispersed in water to obtain the cellulose fiber pulp with the mass concentration of 0.5%.
Step two: preparing an aramid nano fiber/dimethyl sulfoxide dispersion liquid: the recovered para-aramid waste silk is used as a raw material to be added into potassium hydroxide/dimethyl sulfoxide/water (KOH/DMSO/H)2O) is subjected to deprotonation reaction in a system to prepare the aramid nano-fiber/dimethyl sulfoxide dispersion liquid with the mass concentration of 0.5%.
Step three: in-situ protonation reduction and recombination: placing the cellulose fiber slurry obtained in the step one into a beaker, and injecting the aramid nano-fiber/dimethyl sulfoxide dispersion liquid obtained in the step two into the cellulose fiber slurry through an injector to carry out in-situ protonation reduction and compounding; further, the mass ratio of the aramid nano fiber/dimethyl sulfoxide dispersion liquid to the aramid nano fiber to the cellulose fiber in the cellulose pulp is 15: 85 parts by weight; further, mechanical stirring is required in the process of injecting the ANF/DMSO into the cellulose pulp, and the stirring speed is controlled at 2000 rpm; further, after the injection of the aramid nano-fiber/dimethyl sulfoxide dispersion liquid is completed, continuously mechanically stirring for 30min at the rotating speed of 2000rpm to obtain a composite fiber mixed dispersion liquid; and further, carrying out suction filtration on the obtained composite fiber mixed dispersion liquid through a filter membrane, and intercepting the composite fiber mixed dispersion liquid on the filter membrane to obtain the cellulose/aramid nano fiber in-situ composite fiber.
Example 4
A cellulose/aramid nano-fiber in-situ composite fiber is obtained by blending aramid nano-fiber/dimethyl sulfoxide dispersion liquid and cellulose fiber/water dispersion liquid to realize fiber in-situ protonation reduction and compounding; in the cellulose/aramid nano-fiber in-situ composite fiber, the mass ratio of the aramid nano-fiber to the cellulose fiber is 20: 80; the length of the cellulose/aramid nano-fiber in-situ composite fiber is 0.9mm, and the specific surface area is 20m2/g。
A preparation method of cellulose/aramid nano-fiber in-situ composite fiber comprises the following steps:
the method comprises the following steps: preparing cellulose fiber slurry: the softwood pulp board is used as a raw material, the refining concentration of 10% is performed in a refiner, the beating degree of the pulp is controlled to be 58 DEG SR, and the refined pulp is diluted and dispersed in water to obtain cellulose fiber pulp with the mass concentration of 0.6%.
Step two: preparing an aramid nano fiber/dimethyl sulfoxide dispersion liquid: taking recovered para-aramid yarn as raw material in potassium hydroxide/dimethyl sulfoxide/water (KOH/DMSO/H)2O) is subjected to deprotonation reaction in a system to prepare the aramid nano-fiber/dimethyl sulfoxide dispersion liquid with the mass concentration of 0.7%.
Step three: in-situ protonation reduction and recombination: placing the cellulose fiber slurry obtained in the step one into a beaker, and injecting the aramid nano-fiber/dimethyl sulfoxide dispersion liquid obtained in the step two into the cellulose fiber slurry through an injector to carry out in-situ protonation reduction and compounding; further, the mass ratio of the aramid nano fiber/dimethyl sulfoxide dispersion liquid to the aramid nano fiber to the cellulose fiber in the cellulose pulp is 20: 80; further, mechanical stirring is required in the process of injecting the ANF/DMSO into the cellulose pulp, and the stirring speed is controlled at 2500 rpm; further, after the injection of the aramid nano fiber/dimethyl sulfoxide dispersion liquid is completed, continuously mechanically stirring for 25min at the rotating speed of 2500rpm to obtain a composite fiber mixed dispersion liquid; and further, carrying out suction filtration on the obtained composite fiber mixed dispersion liquid through a filter membrane, and intercepting the composite fiber mixed dispersion liquid on the filter membrane to obtain the cellulose/aramid nano fiber in-situ composite fiber.
Example 5
A cellulose/aramid nano-fiber in-situ composite fiber is obtained by blending aramid nano-fiber/dimethyl sulfoxide dispersion liquid and cellulose fiber/water dispersion liquid to realize fiber in-situ protonation reduction and compounding; in the cellulose/aramid nano-fiber in-situ composite fiber, the mass ratio of the aramid nano-fiber to the cellulose fiber is 25: 75; the length of the cellulose/aramid nano-fiber in-situ composite fiber is 1.0mm, and the specific surface area is 38m2/g。
A preparation method of cellulose/aramid nano-fiber in-situ composite fiber comprises the following steps:
the method comprises the following steps: preparing cellulose fiber slurry: the method comprises the steps of taking a cotton pulp board as a raw material, pulping in a pulping machine at a pulping concentration of 10%, controlling the pulping degree of the pulp to be 62 DEG SR, and diluting and dispersing the pulp after pulping in water to obtain cellulose fiber pulp with a mass concentration of 1.0%.
Step two: preparing an aramid nano fiber/dimethyl sulfoxide dispersion liquid: taking recovered para-aramid yarn and aramid gloves as raw materials in potassium hydroxide/dimethyl sulfoxide/water (KOH/DMSO/H)2O) is subjected to deprotonation reaction in a system to prepare the aramid nano-fiber/dimethyl sulfoxide dispersion liquid with the mass concentration of 0.8%.
Step three: in-situ protonation reduction and recombination: placing the cellulose fiber slurry obtained in the step one into a beaker, and injecting the aramid nano-fiber/dimethyl sulfoxide dispersion liquid obtained in the step two into the cellulose fiber slurry through an injector to carry out in-situ protonation reduction and compounding; further, the mass ratio of the aramid nano fiber/dimethyl sulfoxide dispersion liquid to the aramid nano fiber to the cellulose fiber in the cellulose pulp is 25: 75; further, mechanical stirring is needed in the process of injecting the ANF/DMSO into the cellulose pulp, and the stirring speed is controlled at 3000 rpm; further, after the injection of the aramid nano-fiber/dimethyl sulfoxide dispersion liquid is completed, continuously mechanically stirring for 10min at the rotating speed of 3000rpm to obtain a composite fiber mixed dispersion liquid; and further, carrying out suction filtration on the obtained composite fiber mixed dispersion liquid through a filter membrane, and intercepting the composite fiber mixed dispersion liquid on the filter membrane to obtain the cellulose/aramid nano fiber in-situ composite fiber.
Example 6
A cellulose/aramid nano-fiber in-situ composite fiber is obtained by blending aramid nano-fiber/dimethyl sulfoxide dispersion liquid and cellulose fiber/water dispersion liquid to realize fiber in-situ protonation reduction and compounding; in the cellulose/aramid nano-fiber in-situ composite fiber, the mass ratio of the aramid nano-fiber to the cellulose fiber is 30: 70; the length of the cellulose/aramid nano-fiber in-situ composite fiber is 1.2mm, and the specific surface area is 45m2/g。
A preparation method of cellulose/aramid nano-fiber in-situ composite fiber comprises the following steps:
the method comprises the following steps: preparing cellulose fiber slurry: one of softwood pulp board, hardwood pulp board and cotton pulp board is used as a raw material, grinding is carried out in a grinding machine at the grinding concentration of 10%, the beating degree of the pulp is controlled to be 70 DEG SR, and the ground pulp is diluted and dispersed in water to obtain the cellulose fiber pulp with the mass concentration of 1.5%.
Step two: preparing an aramid nano fiber/dimethyl sulfoxide dispersion liquid: taking recovered para-aramid gloves as raw materials in potassium hydroxide/dimethyl sulfoxide/water (KOH/DMSO/H)2O) is subjected to deprotonation reaction in a system to prepare the aramid nano-fiber/dimethyl sulfoxide dispersion liquid with the mass concentration of 1.0%.
Step three: in-situ protonation reduction and recombination: placing the cellulose fiber slurry obtained in the step one into a beaker, and injecting the aramid nano-fiber/dimethyl sulfoxide dispersion liquid obtained in the step two into the cellulose fiber slurry through an injector to carry out in-situ protonation reduction and compounding; further, the mass ratio of the aramid nano fiber/dimethyl sulfoxide dispersion liquid to the aramid nano fiber to the cellulose fiber in the cellulose pulp is 30: 70; further, mechanical stirring is needed in the process of injecting the ANF/DMSO into the cellulose pulp, and the stirring speed is controlled at 3500 rpm; further, after the injection of the aramid nano fiber/dimethyl sulfoxide dispersion liquid is completed, continuously mechanically stirring for 30min at the rotating speed of 3500rpm to obtain a composite fiber mixed dispersion liquid; and further, carrying out suction filtration on the obtained composite fiber mixed dispersion liquid through a filter membrane, and intercepting the composite fiber mixed dispersion liquid on the filter membrane to obtain the cellulose/aramid nano fiber in-situ composite fiber.
The cellulose/aramid nano-fiber in-situ composite fiber prepared in the embodiment 5 of the invention and paper made by the same are detected and characterized, and part of indexes are as follows: 1. average length of composite fiber: 1.2 mm; 2. specific surface area of composite fiber: 38m2(ii)/g; 3. paper made with conjugate fibers: quantification: 94g/m2Thickness: 0.16mm, tensile strength: 84N/cm, tear Strength: 1843mN, folding endurance: 3210 times.
The cellulose/aramid nanofiber in-situ composite fiber is developed and produced by adopting a new process and a new method, has the advantages of high specific surface area, high mechanical strength, excellent temperature resistance and excellent ultraviolet shielding and ageing resistance, overcomes the defects of easy moisture absorption, low wet strength, poor thermal stability, weak ultraviolet shielding, easy ageing and the like of the traditional cellulose, and has wide application prospect.
The embodiments described above are merely preferred embodiments of the present invention, and should not be considered as limitations of the present invention, and features in the embodiments and examples in the present application may be arbitrarily combined with each other without conflict. The protection scope of the present invention is defined by the claims, and includes equivalents of technical features of the claims. I.e., equivalent alterations and modifications within the scope hereof, are also intended to be within the scope of the invention.
Claims (10)
1. The preparation method of the cellulose/aramid nano-fiber in-situ composite fiber is characterized by comprising the following steps of:
the method comprises the following steps: preparing cellulose fiber/water dispersion and aramid fiber nanofiber/dimethyl sulfoxide dispersion;
step two: adding the aramid nano-fiber/dimethyl sulfoxide dispersion liquid into the cellulose fiber/water dispersion liquid in a high-pressure injection mode, wherein the mass ratio of the aramid nano-fiber to the cellulose fiber is (5-30): (70-95), realizing in-situ protonation reduction of the aramid nano-fiber and effectively compounding the aramid nano-fiber with cellulose fiber to prepare the cellulose/aramid nano-fiber in-situ composite fiber.
2. The method for preparing the cellulose/aramid nano-fiber in-situ composite fiber according to claim 1, wherein the cellulose fiber in the first step is one of softwood pulp board, hardwood pulp board and cotton pulp board.
3. The preparation method of the cellulose/aramid nano-fiber in-situ composite fiber according to claim 1, wherein the preparation process of the cellulose fiber/water dispersion is as follows: mixing cellulose fibers with water, pulping, diluting and dispersing to obtain the cellulose fiber/water dispersion with the beating degree of 40-70 DEG SR.
4. The preparation method of the cellulose/aramid nano-fiber in-situ composite fiber according to claim 3, wherein the mass concentration of the pulp is 10% when the cellulose fiber is mixed with water and refined.
5. The preparation method of the cellulose/aramid nano-fiber in-situ composite fiber according to claim 3, wherein the mass concentration of the cellulose fiber/water dispersion is 0.2-1.5%.
6. The preparation method of the cellulose/aramid nano fiber in-situ composite fiber according to claim 1, wherein the preparation process of the aramid nano fiber/dimethyl sulfoxide dispersion liquid is as follows: the method comprises the following steps of taking the recovered para-aramid waste as a raw material, and carrying out deprotonation reaction in a potassium hydroxide/dimethyl sulfoxide/water system to obtain an aramid nanofiber/dimethyl sulfoxide dispersion liquid with the mass concentration of 0.2-1.0%.
7. The method for preparing the cellulose/aramid nano fiber in-situ composite fiber according to claim 6, wherein the recycled para-aramid waste material is one or more of aramid cloth, aramid waste silk, aramid yarn and aramid gloves.
8. The preparation method of the cellulose/aramid nano-fiber in-situ composite fiber according to claim 1, wherein in the second step, the aramid nano-fiber/dimethyl sulfoxide dispersion liquid is mechanically stirred in the process of being added into the cellulose fiber/water dispersion liquid in a high-pressure injection mode, after the injection is completed, the mechanical stirring is continued to obtain a composite fiber mixed dispersion liquid, and the composite fiber mixed dispersion liquid is subjected to suction filtration through a filter membrane to obtain the cellulose/aramid nano-fiber in-situ composite fiber.
9. The preparation method of the cellulose/aramid nanofiber in-situ composite fiber according to claim 8, wherein the rotation speed of the mechanical stirring is 800-3500 rpm, and the mechanical stirring is continued for 10-60 min after the injection is completed.
10. The preparation method of the cellulose/aramid nano-fiber in-situ composite fiber according to claim 1, wherein the cellulose/aramid nano-fiber in-situ composite fiber prepared in the second step has a length of 0.6-1.2 mm and a specific surface area of 8-45 m2/g。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110730375.3A CN113278172B (en) | 2021-06-29 | 2021-06-29 | Preparation method of cellulose/aramid nano-fiber in-situ composite fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110730375.3A CN113278172B (en) | 2021-06-29 | 2021-06-29 | Preparation method of cellulose/aramid nano-fiber in-situ composite fiber |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN113278172A true CN113278172A (en) | 2021-08-20 |
| CN113278172B CN113278172B (en) | 2022-10-21 |
Family
ID=77286132
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110730375.3A Active CN113278172B (en) | 2021-06-29 | 2021-06-29 | Preparation method of cellulose/aramid nano-fiber in-situ composite fiber |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN113278172B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114507910A (en) * | 2022-02-22 | 2022-05-17 | 西安工程大学 | Nano-aramid fiber reinforced regenerated cellulose fiber material, preparation method and application |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108102147A (en) * | 2018-01-10 | 2018-06-01 | 哈尔滨工业大学 | A kind of preparation method of aramid nano-fiber/bacteria cellulose composite membrane |
| 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 |
| CN112795035A (en) * | 2020-12-31 | 2021-05-14 | 齐鲁工业大学 | Cellulose/aramid nano-fiber composite membrane and preparation method and application thereof |
-
2021
- 2021-06-29 CN CN202110730375.3A patent/CN113278172B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108102147A (en) * | 2018-01-10 | 2018-06-01 | 哈尔滨工业大学 | A kind of preparation method of aramid nano-fiber/bacteria cellulose composite membrane |
| 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 |
| CN112795035A (en) * | 2020-12-31 | 2021-05-14 | 齐鲁工业大学 | Cellulose/aramid nano-fiber composite membrane and preparation method and application thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114507910A (en) * | 2022-02-22 | 2022-05-17 | 西安工程大学 | Nano-aramid fiber reinforced regenerated cellulose fiber material, preparation method and application |
Also Published As
| Publication number | Publication date |
|---|---|
| CN113278172B (en) | 2022-10-21 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Vallejos et al. | Nanofibrillated cellulose (CNF) from eucalyptus sawdust as a dry strength agent of unrefined eucalyptus handsheets | |
| Li et al. | Dissolution of cellulose from different sources in an NaOH/urea aqueous system at low temperature | |
| Petroudy et al. | Effects of bagasse microfibrillated cellulose and cationic polyacrylamide on key properties of bagasse paper | |
| Sehaqui et al. | BIOREFINERY: Nanofibrillated cellulose for enhancement of strength in high-density paper structures | |
| Gardner et al. | Adhesion and surface issues in cellulose and nanocellulose | |
| Peng et al. | Laccase and alkali treatments of cellulose fibre: Surface lignin and its influences on fibre surface properties and interfacial behaviour of sisal fibre/phenolic resin composites | |
| Chen et al. | Properties and applications of bamboo fiber-A current-state-of-the art | |
| CN111467875A (en) | Nano-cellulose glass fiber composite filter material and preparation method and application thereof | |
| CN113389080B (en) | Aramid fiber modification method | |
| CN108316056A (en) | A kind of aramid nano-fiber Film laminated aramid paper and preparation method thereof | |
| CN108265566A (en) | It is a kind of to utilize p-aramid paper of aramid nano-fiber self-reinforcing and preparation method thereof | |
| CN110130136A (en) | A kind of preparation method of lignocellulosic nanofiber | |
| CA2811380C (en) | Method for improving the removal of water | |
| CN110067158B (en) | Paper and preparation method and application thereof | |
| Wang et al. | Mechanical property enhancement of self-bonded natural fiber material via controlling cell wall plasticity and structure | |
| Yoo et al. | Enzyme-assisted preparation of fibrillated cellulose fibers and its effect on physical and mechanical properties of paper sheet composites | |
| US20210246609A1 (en) | Materials containing cellulose nanofibers | |
| Li et al. | Interfacial stabilization of fiber-laden foams with carboxymethylated lignin toward strong nonwoven networks | |
| CN113278172B (en) | Preparation method of cellulose/aramid nano-fiber in-situ composite fiber | |
| CN108172738B (en) | Preparation method of cellulose-based lithium battery diaphragm base paper | |
| CN112585310B (en) | Water-dispersible composite structure and method for producing same | |
| Su et al. | Integrated production of cellulose nanofibers and sodium carboxymethylcellulose through controllable eco-carboxymethylation under mild conditions | |
| Barrios et al. | Innovation in lignocellulosics dewatering and drying for energy sustainability and enhanced utilization of forestry, agriculture, and marine resources-A review | |
| CN1948615A (en) | Synthetic fiber paper containing basalt fiber and chemical fiber and its preparation method | |
| JP7492457B2 (en) | Fiber reinforced resin sheet and method for producing same |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |