CN114197075A - Preparation method of carbon nanotube aramid fibrid and carbon nanotube aramid fibrid - Google Patents
Preparation method of carbon nanotube aramid fibrid and carbon nanotube aramid fibrid Download PDFInfo
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- CN114197075A CN114197075A CN202010986479.6A CN202010986479A CN114197075A CN 114197075 A CN114197075 A CN 114197075A CN 202010986479 A CN202010986479 A CN 202010986479A CN 114197075 A CN114197075 A CN 114197075A
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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
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
- D01F6/905—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides of aromatic polyamides
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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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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Abstract
The carbon nanotube aramid fibrid formed by the invention has the advantages of long fiber brooming shape and long fiber sheet membrane shape, so that the carbon nanotube aramid fibrid has rich hairiness and strong bonding capability, and the carbon nanomaterial is accessed, so that the temperature resistance, the insulativity, the conductivity and the heat conductivity of the material are excellent. The invention also provides the carbon nano tube aramid fibrid.
Description
Technical Field
The invention belongs to the technical field of aramid fibers, and particularly relates to a preparation method of carbon nanotube aramid fibrids and the carbon nanotube aramid fibrids.
Background
Aramid fiber is a novel synthetic material with special purpose. Since the long-chain polymer molecules constituting the fibers contain amide groups and the amide groups are connected to each other by an aromatic ring or a derivative of an aromatic ring, these fibers are collectively called aromatic polyamide fibers, abbreviated as aramid fibers. Aramid fiber has remarkable heat resistance and initial modulus, and is a main class of the organic high-temperature resistant fiber at present. The two varieties with the most practical value are the meta-aramid fiber with zigzag molecular chain arrangement, namely aramid fiber 1313; one is para-aramid fiber with linear molecular chain arrangement, namely aramid 1414. The two have similar chemical structures but have great performance difference and different application fields: the meta-aramid fiber has excellent high-temperature resistance and insulativity and is mainly used for special protective clothing, high-temperature filter materials, electric insulating materials, honeycomb structure materials and the like; the para-aramid fiber has excellent metal characteristics and is mainly used as a framework material of national defense military industry, aerospace and aviation, tires and civil engineering and protective articles.
The meta-aramid fibrid has the conventional structure and performance of meta-aramid fibers, is similar to wood fibers in appearance, has excellent wet processing performance and reinforcing performance, is extremely good in dispersion in water, has an average specific surface area of 5-8m2/g, is large in length-diameter ratio and extremely high in strength, is one of important binding fibers for wet papermaking of aramid fibers, and is suitable for manufacturing high-grade insulating paper and electronic products with high dimensional stability, such as printed circuit boards, satellite communication, high-speed transmission loops and the like.
The length and shape of the ultra-short fiber produced by the method introduced in the prior document are suitable for the paper making grade and are all ultra-small fiber shapes, so the tearing strength of the ultra-short fiber of the finished paper is far from the international advanced level. How to improve the tearing strength of the aramid ultra-short fiber becomes a technical problem which needs to be solved urgently in the prior art.
Disclosure of Invention
In view of this, it is necessary to provide a method for preparing carbon nanotube aramid fibrids with high tear strength.
A preparation method of carbon nanotube aramid fibrid comprises the following steps:
obtaining a carbon nano tube aramid polymer;
obtaining a solidification solution;
mixing the carbon nanotube aramid polymer and the solidification solution at a high speed to obtain aramid ultrashort fibers;
and washing the aramid fiber ultrashort fibers to obtain the carbon nanotube aramid fiber fibrids.
In some embodiments, the step of obtaining the carbon nanotube-aramid polymer specifically includes the following steps:
placing an amide polar organic solvent in a polymerization apparatus filled with nitrogen;
adding m-phenylenediamine and a carbon nano tube into the amide polar organic solvent for dissolving to obtain a mixed solution;
performing polycondensation reaction on the isophthaloyl dichloride and the mixed solution at the temperature of 0-20 ℃ to obtain a byproduct hydrogen chloride;
and (3) carrying out a neutralization reaction on the byproduct hydrogen chloride by using alkaline earth metal oxide, hydroxide or ammonia gas at the temperature of lower than 30 ℃ to obtain the carbon nano tube aramid polymer.
In some embodiments, the carbon nanotube material accounts for 5% -40% of the absolute dry content of the aramid fiber; the diameter of the carbon nano is 60-100nm, and the length is 3-10 um.
In some embodiments, the concentration of the carbon nanotube-aramid polymer is 8-20%, the viscosity is 1.2-2.2, and the temperature is 0-60 degrees.
In some embodiments, in the step of obtaining the coagulation solution, specifically:
the coagulating solution is a mixture of at least one inorganic salt, an alcohol substance and water, wherein the mass ratio of the inorganic salt to the alcohol substance is (10-70%): (1-10%) and the balance of water.
In some of these embodiments, the temperature of the coagulating solution is 0-90 degrees.
In some embodiments, the inorganic salt includes one or more of calcium chloride, lithium chloride, magnesium chloride or sodium chloride, and the alcohol includes one or more of glycerol, ethylene glycol, butylene glycol, and the like.
In some embodiments, in the step of mixing the carbon nanotube-aramid polymer and the coagulation solution at a high speed to obtain the ultra-short aramid fibers, the steps are specifically:
mixing a carbon nanotube aramid polymer and a solidification solution according to a mass ratio of 1: (5-30) in a sealed high-speed stirring device, and mixing at a high speed of 1000-3000rpm to obtain the aramid ultrashort fibers.
In some embodiments, the step of washing the ultra-short aramid fiber to obtain the carbon nanotube-aramid fibrid specifically includes:
and washing the aramid ultra-short fibers by adopting paper pulp washing equipment to obtain the carbon nanotube aramid fibrids, wherein the paper pulp washing equipment comprises a belt type pulp washer or a rotary drum pulp washer.
In addition, the invention also provides a carbon nanotube aramid fibrid which is prepared by the preparation method of the carbon nanotube aramid fibrid.
Compared with the prior art, the preparation method of the carbon nanotube aramid fibrid provided by the application obtains the carbon nanotube aramid polymer, obtains the solidification solution, mixes the carbon nanotube aramid polymer and the solidification solution at a high speed to obtain the ultra-short aramid fiber, and washes the ultra-short aramid fiber to obtain the carbon nanotube aramid fibrid.
The carbon nano aramid fibrid provided by the application can be used for manufacturing paper sheets, friction materials, rubber reinforcement and the like, the tear strength of the carbon nano aramid paper prepared from the fibrid can reach 1000-1500N, and the paper has good electric and thermal conductivity and can be widely applied to various occasions of high temperature resistance, electric conduction and thermal conduction.
Drawings
The accompanying drawings, which are included to provide a further understanding of the application and are incorporated in and constitute a part of this application, illustrate embodiment(s) of the application and together with the description serve to explain the application and not to limit the application. In the drawings:
fig. 1 is a flow chart of steps of a method for preparing carbon nanotube aramid fibrids provided by an embodiment of the present invention.
Fig. 2 is a flowchart of steps of a method for preparing a carbon nanotube-aramid polymer according to an embodiment of the present invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present application more apparent, the technical solutions of the present application will be described in detail and completely with reference to the following specific embodiments of the present application and the accompanying drawings. It should be apparent that the described embodiments are only some of the embodiments of the present application, and not all of the embodiments.
Referring to fig. 1, the preparation method of the carbon nanotube aramid fibrid provided by the present application includes the following steps:
step S110: and obtaining the carbon nano tube aramid polymer.
Referring to fig. 2, a flow chart of steps for obtaining a carbon nanotube-aramid polymer specifically includes the following steps:
step S111: the amide-based polar organic solvent was placed in a polymerization apparatus filled with nitrogen.
Specifically, the amide polar organic solvent is dimethylacetamide.
Step S112: adding m-phenylenediamine and a carbon nano tube into the amide polar organic solvent for dissolving to obtain a mixed solution.
Specifically, the carbon nanotube material accounts for 5-40% of the absolute dry content of the aramid fiber, the diameter of the carbon nanotube is 60-100nm, and the length of the carbon nanotube is 3-10 um.
Step S113: performing polycondensation reaction on the isophthaloyl dichloride and the mixed solution at the temperature of 0-20 ℃ to obtain a byproduct hydrogen chloride;
specifically, the molar amounts of m-phenylenediamine and isophthaloyl chloride are the same.
Step S114: and (3) carrying out a neutralization reaction on the byproduct hydrogen chloride by using alkaline earth metal oxide, hydroxide or ammonia gas at the temperature of lower than 30 ℃ to obtain the carbon nano tube aramid polymer.
In some embodiments, the concentration of the carbon nanotube-aramid polymer is 8-20%, the viscosity is 1.2-2.2, and the temperature is 0-60 degrees.
In the embodiment, dimethyl acetamide is added into a low-temperature polymerization device, m-phenylenediamine is added and stirred to be dissolved, then a carbon nanotube material accounting for 5% -40% of absolute dry content of aramid fiber is added, m-phthaloyl chloride with the same molar quantity as the m-phenylenediamine is slowly added, after the reaction is finished, a reaction byproduct HCL is removed by using a certain amount of alkaline earth metal, and then the polymer suitable for spinning is obtained through filtering and vacuum defoaming by a plate-and-frame filter press.
Step S120: a coagulation solution is obtained.
Specifically, the coagulating solution is a mixture of at least one inorganic salt, an alcohol substance and water, wherein the mass ratio of the inorganic salt to the alcohol substance is (10-70%): (1-10%) and the balance of water.
Further, the temperature of the coagulation solution is 0 to 90 degrees.
Further, the inorganic salts comprise one or more of calcium chloride, lithium chloride, magnesium chloride or sodium chloride, and the alcohols comprise one or more of glycerol, ethylene glycol, butanediol and the like.
Step S130: and mixing the carbon nanotube aramid polymer and the solidification solution at a high speed to obtain the aramid ultrashort fiber.
Specifically, the carbon nanotube aramid polymer and the solidification solution are mixed according to the mass ratio of 1: (5-30) in a sealed high-speed stirring device, and mixing at a high speed of 1000-3000rpm to obtain the aramid ultrashort fibers.
Step S140: and washing the aramid fiber ultrashort fibers to obtain the carbon nanotube aramid fiber fibrids.
Specifically, the aramid ultrashort fibers are washed by a paper pulp washing device to obtain the carbon nanotube aramid fibrids, wherein the paper pulp washing device comprises a belt type pulp washer or a drum pulp washer.
The carbon nano-tube aramid fibrid prepared by the embodiment of the invention forms the carbon nano-tube aramid fibrid with rich hairiness and short fiber length of 1mm-10mm, and has strong binding capacity.
The carbon nanotube aramid fibrid formed by the invention has the advantages of long fiber brooming shape and long fiber sheet membrane shape, so that the carbon nanotube aramid fibrid has rich hairiness and strong bonding capability, and the carbon nanomaterial is accessed, so that the temperature resistance, the insulativity, the conductivity and the heat conductivity of the material are excellent.
The carbon nano aramid fibrid provided by the application can be used for manufacturing paper sheets, friction materials, rubber reinforcement and the like, the tear strength of the carbon nano aramid paper prepared from the fibrid can reach 1000-1500N, and the paper has good electric and thermal conductivity and can be widely applied to various occasions of high temperature resistance, electric conduction and thermal conduction.
The technical solution of the present invention will be described in detail with reference to the following detailed examples.
Example 1
In a reaction kettle equipped with intensive stirring and jacket freezing, 1 part of phenylenediamine is added into 7.5 parts of dried dimethylacetamide, and after 30min of dissolution, 0.1 part of carbon nano tube with the diameter of 60nm and the length of 10um is added and stirred for 30 min; controlling the temperature at 0-10 ℃, continuously and slowly adding 1.88 parts of isophthaloyl dichloride to carry out polycondensation reaction, continuously neutralizing a byproduct hydrogen chloride by using 0.70 part of calcium hydroxide dimethylacetamide (the ratio of calcium hydroxide to dimethylacetamide is 1: 1.5-2.5) mixed solution, controlling the temperature to be lower than 30 ℃, and generating a poly (m-phthaloyl chloride-m-phenylenediamine) colloidal polymer with the polymer concentration of 16 wt%, the [ eta ] of 1.63 and the pH value of 6.8; the polymer is bright black and has good quality.
The components of the prepared coagulating solution are as follows: 25% of sodium chloride, and 25% of butanediol: 6 percent and the balance of water.
The polymer is simultaneously injected into a high-speed mixing device through a metering pump and a solidification solution conveyed by the metering pump at the rotating speed of 2500rpm to obtain the aramid ultra-short fiber.
The method comprises the steps of washing the aramid ultrashort fibers, and washing and cleaning the aramid ultrashort fibers in common pulping to obtain the carbon nanotube aramid fibrids, wherein the fibrids formed by the method are bright black, the mechanical beating degree of the product is 39SR, the fiber form is long when the product is observed under a fiberscope, the forming is good, the wet product can be used for manufacturing paper sheets, and the tearing strength can reach 1000N.
Example 2
In a reaction kettle equipped with intensive stirring and jacket freezing, 1 part of phenylenediamine is added into 7.5 parts of dried dimethylacetamide, and after 30min of dissolution, 0.2 part of carbon nano tube with the diameter of 60nm and the length of 10um is added and stirred for 30 min; controlling the temperature at 0-10 ℃, continuously and slowly adding 1.88 parts of isophthaloyl dichloride to carry out polycondensation reaction, continuously neutralizing a byproduct hydrogen chloride by using 0.70 part of calcium hydroxide dimethylacetamide (the ratio of calcium hydroxide to dimethylacetamide is 1: 1.5-2.5) mixed solution, controlling the temperature to be lower than 30 ℃, and generating a poly (m-phthaloyl chloride-m-phenylenediamine) colloidal polymer with the polymer concentration of 16 wt%, the [ eta ] of 1.63 and the pH value of 6.8; the polymer is bright black and has good quality.
The components of the prepared coagulating solution are as follows: 50% of lithium chloride and glycerol: 8 percent and the balance of water.
The polymer is simultaneously injected into high-speed mixing equipment through a metering pump and a solidification solution conveyed by the metering pump at the rotating speed of 3000rpm to obtain the aramid ultra-short fiber.
The method comprises the steps of washing the aramid ultrashort fibers, and washing and cleaning the aramid ultrashort fibers in common pulping to obtain the carbon nanotube aramid fibrids, wherein the fibrids formed by the method are bright black, the mechanical beating degree of the product is 39SR, the fiber form is long when the product is observed under a fiberscope, the forming is good, the wet product can be used for manufacturing paper sheets, and the tearing strength can reach 1500N.
The above are merely examples of the present application and are not intended to limit the present application. Various modifications and changes may occur to those skilled in the art. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application should be included in the scope of the claims of the present application.
Claims (10)
1. The preparation method of the carbon nanotube aramid fibrid is characterized by comprising the following steps:
obtaining a carbon nano tube aramid polymer;
obtaining a solidification solution;
mixing the carbon nanotube aramid polymer and the solidification solution at a high speed to obtain aramid ultrashort fibers;
and washing the aramid fiber ultrashort fibers to obtain the carbon nanotube aramid fiber fibrids.
2. The method for preparing the carbon nanotube aramid fibrid as claimed in claim 1, wherein the step of obtaining the carbon nanotube aramid polymer specifically comprises the steps of:
placing an amide polar organic solvent in a polymerization apparatus filled with nitrogen;
adding m-phenylenediamine and a carbon nano tube into the amide polar organic solvent for dissolving to obtain a mixed solution;
performing polycondensation reaction on the isophthaloyl dichloride and the mixed solution at the temperature of 0-20 ℃ to obtain a byproduct hydrogen chloride;
and (3) carrying out a neutralization reaction on the byproduct hydrogen chloride by using alkaline earth metal oxide, hydroxide or ammonia gas at the temperature of lower than 30 ℃ to obtain the carbon nano tube aramid polymer.
3. The preparation method of the carbon nanotube aramid fibrid as claimed in claim 2, wherein the carbon nanotube material accounts for 5% -40% of the absolute dry content of the aramid fiber; the diameter of the carbon nano is 60-100nm, and the length is 3-10 um.
4. The method for preparing the carbon nanotube aramid fibrid according to claim 2, wherein the concentration of the carbon nanotube aramid polymer is 8-20%, the viscosity is 1.2-2.2, and the temperature is 0-60 degrees.
5. The method for preparing the carbon nanotube aramid polymer according to claim 1, wherein in the step of obtaining the coagulation solution, specifically:
the coagulating solution is a mixture of at least one inorganic salt, an alcohol substance and water, wherein the mass ratio of the inorganic salt to the alcohol substance is (10-70%): (1-10%) and the balance of water.
6. The method of claim 5, wherein the temperature of the coagulation solution is 0 to 90 degrees.
7. The method for preparing the carbon nanotube aramid fibrids as claimed in claim 5, wherein the inorganic salt comprises one or more of calcium chloride, lithium chloride, magnesium chloride or sodium chloride, and the alcohol comprises one or more of glycerol, ethylene glycol, butanediol and the like.
8. The method for preparing the carbon nanotube aramid fibrid according to claim 1, wherein in the step of mixing the carbon nanotube aramid polymer and the coagulation solution at a high speed to obtain the aramid ultra-short fiber, the method specifically comprises:
mixing a carbon nanotube aramid polymer and a solidification solution according to a mass ratio of 1: (5-30) in a sealed high-speed stirring device, and mixing at a high speed of 1000-3000rpm to obtain the aramid ultrashort fibers.
9. The method for preparing the carbon nanotube aramid fibrid according to claim 1, wherein the step of washing the aramid ultra-short fiber to obtain the carbon nanotube aramid fibrid specifically comprises:
and washing the aramid ultra-short fibers by adopting paper pulp washing equipment to obtain the carbon nanotube aramid fibrids, wherein the paper pulp washing equipment comprises a belt type pulp washer or a rotary drum pulp washer.
10. A carbon nanotube aramid fibrid characterized by being prepared by the method for preparing the carbon nanotube aramid fibrid of any one of claims 1 to 9.
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| CN115627556A (en) * | 2022-10-17 | 2023-01-20 | 株洲时代新材料科技股份有限公司 | High-conductivity meta-aramid fibrid resin and preparation method of fibrid thereof |
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