CN111691012B - Electric control type polyacrylonitrile precursor microwave pre-oxidation process - Google Patents
Electric control type polyacrylonitrile precursor microwave pre-oxidation process Download PDFInfo
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- CN111691012B CN111691012B CN202010747014.5A CN202010747014A CN111691012B CN 111691012 B CN111691012 B CN 111691012B CN 202010747014 A CN202010747014 A CN 202010747014A CN 111691012 B CN111691012 B CN 111691012B
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- polyacrylonitrile
- carbon black
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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
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/12—Carbon filaments; Apparatus specially adapted for the manufacture thereof
- D01F9/14—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments
- D01F9/20—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products
- D01F9/21—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D01F9/22—Carbon filaments; Apparatus specially adapted for the manufacture thereof by decomposition of organic filaments from polyaddition, polycondensation or polymerisation products from macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from polyacrylonitriles
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/73—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof
- D06M11/74—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with carbon or compounds thereof with carbon or graphite; with carbides; with graphitic acids or their salts
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
- D06M2101/18—Synthetic fibres consisting of macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M2101/26—Polymers or copolymers of unsaturated carboxylic acids or derivatives thereof
- D06M2101/28—Acrylonitrile; Methacrylonitrile
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Or Physical Treatment Of Fibers (AREA)
Abstract
The invention relates to the technical field of carbon fibers, in particular to an electric control type polyacrylonitrile precursor microwave pre-oxidation process, which comprises the following steps: s1: dissolving a hydrolyzed adhesive into deionized water to form an adhesive solution; s2: mixing a set amount of carbon black with deionized water to form a suspension; s3: immersing polyacrylonitrile protofilament in the bonding solution, and taking out the polyacrylonitrile protofilament before complete drying; s4: immersing polyacrylonitrile protofilament into the suspension, taking out the polyacrylonitrile protofilament after the polyacrylonitrile protofilament is immersed for a set time, and completely drying the polyacrylonitrile protofilament; s5: feeding polyacrylonitrile protofilament into a microwave oxidation furnace for oxidation under set conditions. According to the invention, the carbon material wave-absorbing substance is coated on the surface of the polyacrylonitrile protofilament which does not absorb waves, and the carbon black can absorb microwave quantity after entering a microwave oxidation furnace, so that the surface of the polyacrylonitrile protofilament obtains heat energy to realize pre-oxidation, the control of the pre-oxidation effect can be effectively realized by reasonably controlling the microwave power and the pre-oxidation time, and meanwhile, the cost of protofilament treatment can be effectively reduced in the pre-oxidation stage by reasonably controlling the power supply.
Description
Technical Field
The invention relates to the technical field of carbon fibers, in particular to an electric control type polyacrylonitrile precursor microwave pre-oxidation process.
Background
Carbon fibers (carbon fibers) are fibrous carbon materials, and carbon elements in their chemical composition account for 90% or more of the total mass. The carbon fiber and the composite material thereof have a series of excellent performances of high specific strength, high specific modulus, high temperature resistance, corrosion resistance, fatigue resistance, creep resistance, electric conduction, heat transfer, small thermal expansion coefficient and the like, and can be used as a structural material for bearing load and a functional material for playing a role. Therefore, carbon fibers and their composites have developed very rapidly in recent years.
There are many kinds of raw materials which can be used for producing carbon fibers, and they are mainly classified into two main types according to their sources, one is artificial fibers such as viscose, rayon, lignin fibers, etc., and the other is synthetic fibers which are raw materials purified from natural resources such as petroleum, etc., and they are spun into filaments after being treated, such as acrylic fibers, pitch fibers, polyacrylonitrile fibers, etc. The charring yield of the polyacrylonitrile-based carbon fiber is higher than that of the viscose fiber and can reach more than 45 percent, and the polyacrylonitrile-based carbon fiber is the carbon fiber with the widest application field and the largest yield because the production process, the solvent recovery, the three-waste treatment and other aspects are simpler than the viscose fiber, the cost is low, the raw material source is rich, and the mechanical properties, especially the tensile strength, the tensile modulus and the like of the polyacrylonitrile-based carbon fiber are the first of three carbon fibers.
Pre-oxidation needs to be carried out for nearly one hundred minutes from polyacrylonitrile protofilament to the final carbon fiber forming layer, the existing pre-oxidation process is a process with huge carbon fiber cost consumption, and the reduction of the carbon fiber production cost is seriously restricted.
In view of the above problems, the designer actively makes research and innovation based on the practical experience and professional knowledge that the product engineering is applied for many years, so as to create an electrically controlled polyacrylonitrile precursor microwave pre-oxidation process, which is more practical.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: the electrically controlled polyacrylonitrile precursor microwave pre-oxidation process is provided, and the production cost of the polyacrylonitrile precursor pre-oxidation process is effectively reduced.
In order to achieve the purpose, the invention adopts the technical scheme that:
an electric control type polyacrylonitrile precursor microwave pre-oxidation process comprises the following steps:
s1: preparing a bonding solution, and melting a hydrolytic adhesive into deionized water to form the bonding solution;
s2: preparing carbon black coating liquid, and mixing a set amount of carbon black with deionized water to form suspension;
s3: immersing polyacrylonitrile precursor with a clean surface into the bonding solution prepared in the step S1, and taking out the polyacrylonitrile precursor before completely drying;
s4: immersing the polyacrylonitrile precursor fiber dried for a set time into the suspension, taking out the polyacrylonitrile precursor fiber after the polyacrylonitrile precursor fiber is immersed for a set time, and completely drying the polyacrylonitrile precursor fiber;
s5: and sending the dried polyacrylonitrile protofilament into a microwave oxidation furnace for pre-oxidation under a set condition.
Further, preparing a carbon black coating liquid comprises the following steps:
s11: weighing a set amount of carbon black powder and placing the carbon black powder into a container with an opening at the top;
s12: and in the compressible cavity at the bottom of the container, deionized water mixed with an organic dispersant is injected into the container from the porous position at the bottom of the container for a plurality of times, all mixed solution in the container is sucked out from the hole position to the compressible cavity after each injection, the mixed solution is injected again according to the set pressure, and the injection amount increases progressively relative to the last injection amount each time until all the mixed solution is injected into the container.
Further, the method also comprises the following steps:
s13: and carrying out ultrasonic treatment on the mixed solution in the container to form a carbon black suspension.
Further, the ultrasonic treatment time is 1-1.5 hours.
Further, the suspension is subjected to cyclic reciprocal oscillation while the polyacrylonitrile filaments are immersed in the suspension.
Further, the carbon black is acetylene black.
Further, the mass ratio of the carbon black to the deionized water is 10-15: 100.
further, the organic dispersant is hydroxymethyl cellulose.
Further, the mass ratio of the organic dispersant to the deionized water is 0.2-0.4: 100.
further, the dipping time of the polyacrylonitrile protofilament in the suspension is 15-20 minutes.
The invention has the beneficial effects that: according to the invention, the carbon material wave-absorbing substance is coated on the surface of the polyacrylonitrile protofilament which does not absorb waves, and the carbon black can absorb microwave quantity after entering a microwave oxidation furnace, so that the surface of the polyacrylonitrile protofilament obtains heat energy to realize pre-oxidation, the control of the pre-oxidation effect can be effectively realized by reasonably controlling the microwave power and the pre-oxidation time, the cost of protofilament treatment is effectively reduced in the pre-oxidation stage, and meanwhile, the cost of protofilament treatment can be effectively reduced in the pre-oxidation stage by reasonably controlling the power supply.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments described in the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart of an electrically controlled polyacrylonitrile precursor microwave pre-oxidation process;
FIG. 2 is a schematic diagram of a process for coating carbon black on the surface of polyacrylonitrile protofilament;
FIG. 3 is a schematic diagram of a process for preparing a carbon black coating liquid.
Detailed Description
The invention is further described below with reference to the accompanying drawings. The following examples are only for illustrating the technical solutions of the present invention more clearly, and the protection scope of the present invention is not limited thereby.
As shown in fig. 1, an electrically controlled polyacrylonitrile precursor microwave pre-oxidation process includes:
s1: preparing a bonding solution, and melting a hydrolytic adhesive into deionized water to form the bonding solution;
s2: preparing a carbon black coating liquid, mixing a set amount of carbon black with deionized water, wherein the mass ratio of the carbon black to the deionized water is 10-15: 100, forming a suspension;
s3: immersing polyacrylonitrile precursor with a clean surface into the bonding solution prepared in the step S1, and taking out the polyacrylonitrile precursor before completely drying;
s4: immersing the polyacrylonitrile precursor fiber dried for a set time into the suspension, taking out the polyacrylonitrile precursor fiber after the polyacrylonitrile precursor fiber is immersed for the set time, and completely drying the polyacrylonitrile precursor fiber;
s5: and (3) sending the dried polyacrylonitrile protofilament into a microwave oxidation furnace for pre-oxidation under a set condition.
According to the invention, the carbon material wave-absorbing substance is coated on the surface of the polyacrylonitrile protofilament which does not absorb waves, and the carbon black can absorb microwave quantity after entering a microwave oxidation furnace, so that the surface of the polyacrylonitrile protofilament obtains heat energy to realize pre-oxidation, the control of the pre-oxidation effect can be effectively realized by reasonably controlling the microwave power and the pre-oxidation time, the cost of protofilament treatment is effectively reduced in the pre-oxidation stage, and meanwhile, the cost of protofilament treatment can be effectively reduced in the pre-oxidation stage by reasonably controlling the power supply.
After the bonding solution and the suspension are prepared, the filaments are first immersed in the bonding solution to form a bonding layer on the surface, as shown in fig. 2 (a) to (b), and taken out before the bonding layer is completely dried, in order to form a protective layer having toughness on the surface of the filaments and to simultaneously achieve the purpose of heat soaking through the protective layer. In the specific implementation process, the precursor is easy to break due to the non-uniformity and instantaneous increase of heat, in the embodiment, the adhesive layer is used as a protective layer which is completely covered without interruption, so that on one hand, the precursor can be protected to a certain extent through the toughness of the precursor in the process of instantaneous increase of the microwave quantity absorbed by the carbon black, and the probability of breakage is reduced; on the other hand, the purpose of soaking can be achieved through the arrangement of the level, and heat from the carbon black is dispersed through the adhesive layer, so that the protofilament can be heated more uniformly in the heating process of the protofilament, the fracture condition of the protofilament can be effectively relieved, in the implementation process, the wave absorbing process of the carbon black on the surface of the protective layer cannot be influenced by the level, the wave absorbing efficiency of the carbon black can be improved, and the purpose of saving energy is further achieved.
After the adhesive layer is formed, drying to a certain degree is required to ensure the stability of the shape of the adhesive layer, but the adhesive layer cannot be completely dried, so that the adhesive effect on the carbon black is influenced, and the specific drying time needs to be comprehensively determined according to the solid content of the suspension, the dipping time in the suspension, the drying power and the like; as shown in fig. 2 (c), the carbon black on the surface is uniformly coated, i.e., it is stably pre-oxidized in a microwave oxidation oven.
In the present invention, in order to achieve adhesion of the protective layer to the carbon black, continuous dipping is required to avoid the influence of drying after the precursor is taken out, and thus the effect of coating the carbon black is not affected. In order to avoid the influence on the precursor, the oscillation time and amplitude need to be controlled, and the method can be realized by oscillating a container for containing the suspension, wherein the immersion time of the polyacrylonitrile precursor in the suspension is 15-20 minutes.
As a preference of the above embodiment, the preparation of the carbon black coating liquid comprises the steps of:
s11: weighing a set amount of carbon black powder into a container with an open top, as shown in fig. 3 (a);
s12: in a compressible cavity at the bottom of the container, deionized water mixed with an organic dispersing agent is injected into the container from a porous position at the bottom of the container for a plurality of times, wherein the organic dispersing agent is hydroxymethyl cellulose, and the mass ratio of the organic dispersing agent to the deionized water is 0.2-0.4: 100, respectively; as shown in fig. 3 (b), in the above-mentioned injecting process, after selecting a proper pressure, the mixed liquid is sprayed from bottom to top in a spray shape under the restriction of the hole site and the pressure, so that the carbon black at the bottom of the container is rolled up and mixed into the liquid; after each injection, the mixed solution in the container is completely sucked out from the hole positions to the compressible cavity and then injected again according to the set pressure, as shown in (c) in fig. 3, in the sucking-out process, as the negative pressure exists in the compressible cavity, the mixed solution in the container can be sucked out in a jet shape, and in the process, the carbon black in the liquid in the container and the carbon black in the compressible cavity are mixed and tend to be uniform; during the process of injecting the liquid into the container, the injection amount of each time is increased relative to the last injection amount until all the mixed solution is injected into the container, as shown in fig. 3 (d).
In the above preferred embodiment, the carbon black is mixed from the top and bottom direction, as opposed to the conventional planar annular stirring, and the precipitation of the carbon black is effectively improved and uniform dispersion thereof is achieved; meanwhile, compared with stirring under normal pressure, the mixing effect under the pressurization condition is better.
As a preference of the above embodiment, in order to further improve the uniformity of the mixed solution, the method further comprises the following steps:
s13: and carrying out ultrasonic treatment on the mixed solution in the container to form a suspension of the carbon black, wherein in the specific implementation process, the ultrasonic treatment time is 1-1.5 hours.
In the invention, the carbon black is acetylene carbon black, the carbon black of the type presents regular spherical particles when being observed in a TEM picture, the size is in a nanometer level, and the acetylene carbon black is easy to agglomerate to form an aggregation state structure, so that the acetylene carbon black has a larger surface area and is easier to cause the polarization of an interface.
It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. An electric control type polyacrylonitrile precursor microwave pre-oxidation process is characterized by comprising the following steps:
s1: preparing a bonding solution, and dissolving a hydrolyzed bonding agent into deionized water to form the bonding solution;
s2: preparing carbon black coating liquid, and mixing a set amount of carbon black with deionized water to form suspension;
s3: immersing polyacrylonitrile precursor with a clean surface into the bonding solution prepared in the step S1, drying after the bonding layer is formed, and taking out before complete drying;
s4: immersing the polyacrylonitrile precursor fiber dried for a set time into the suspension, taking out the polyacrylonitrile precursor fiber after the polyacrylonitrile precursor fiber is immersed for a set time, and completely drying the polyacrylonitrile precursor fiber;
s5: and sending the dried polyacrylonitrile protofilament into a microwave oxidation furnace for pre-oxidation under a set condition.
2. The microwave pre-oxidation process of the electrically controlled polyacrylonitrile precursor as claimed in claim 1, wherein the preparation of the carbon black coating liquid comprises the following steps:
s11: weighing a set amount of carbon black powder and placing the carbon black powder into a container with an opening at the top;
s12: and in the compressible cavity at the bottom of the container, deionized water mixed with an organic dispersant is injected into the container from the porous position at the bottom of the container for a plurality of times, all mixed solution in the container is sucked out from the hole position to the compressible cavity after each injection, the mixed solution is injected again according to the set pressure, and the injection amount increases progressively relative to the last injection amount each time until all the mixed solution is injected into the container.
3. The electrically controlled polyacrylonitrile precursor microwave pre-oxidation process of claim 2, characterized by further comprising the following steps:
s13: and carrying out ultrasonic treatment on the mixed solution in the container to form a carbon black suspension.
4. The microwave pre-oxidation process of the electrically controlled polyacrylonitrile precursor as claimed in claim 3, wherein the ultrasonic treatment time is 1-1.5 hours.
5. An electronically controlled polyacrylonitrile filament microwave pre-oxidation process according to claim 1, characterized in that the suspension is oscillated cyclically and reciprocally while the polyacrylonitrile filament is immersed in the suspension.
6. The electrically controlled polyacrylonitrile precursor microwave pre-oxidation process is characterized in that the carbon black is acetylene carbon black.
7. The microwave pre-oxidation process of the electrically controlled polyacrylonitrile precursor as claimed in claim 2, wherein the mass ratio of the carbon black to the deionized water is 10-15: 100.
8. the electrically controlled polyacrylonitrile precursor microwave pre-oxidation process of claim 2, wherein the organic dispersant is hydroxymethyl cellulose.
9. The microwave pre-oxidation process of the electrically controlled polyacrylonitrile precursor as claimed in claim 7, wherein the mass ratio of the organic dispersant to the deionized water is 0.2-0.4: 100.
10. the electrically controlled polyacrylonitrile precursor microwave pre-oxidation process of claim 5, wherein the polyacrylonitrile precursor is immersed in the suspension for 15-20 minutes.
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Citations (7)
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| CN101760807A (en) * | 2009-11-24 | 2010-06-30 | 中复神鹰碳纤维有限责任公司 | Method for reducing production of preoxidized broken filament during preparation of polyacrylonitrile-based carbon fiber |
| CN105413504A (en) * | 2016-01-12 | 2016-03-23 | 北京峰迪克机械设备有限公司 | Solid-powder dissolving and adding device |
| CN206152667U (en) * | 2016-11-01 | 2017-05-10 | 武汉东湖学院 | Biological emulsion paint production of environment -friendly is with raw materials instant dispersed device |
| CN107858829A (en) * | 2017-11-28 | 2018-03-30 | 东华大学 | A kind of method that microwave oxidizing process prepares preoxidized polyacrylonitrile silk |
| CN109072541A (en) * | 2016-06-30 | 2018-12-21 | 松本油脂制药株式会社 | Fibre finish and its utilization |
| CN208362539U (en) * | 2018-04-18 | 2019-01-11 | 昆明理工大学 | A kind of microwave heating polyacrylonitrile prepares the device of oxidization fiber |
| CN111088559A (en) * | 2018-10-23 | 2020-05-01 | 中国石油化工股份有限公司 | Preparation method of low-silicon-content polyacrylonitrile-based carbon fiber |
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2020
- 2020-07-29 CN CN202010747014.5A patent/CN111691012B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101760807A (en) * | 2009-11-24 | 2010-06-30 | 中复神鹰碳纤维有限责任公司 | Method for reducing production of preoxidized broken filament during preparation of polyacrylonitrile-based carbon fiber |
| CN105413504A (en) * | 2016-01-12 | 2016-03-23 | 北京峰迪克机械设备有限公司 | Solid-powder dissolving and adding device |
| CN109072541A (en) * | 2016-06-30 | 2018-12-21 | 松本油脂制药株式会社 | Fibre finish and its utilization |
| CN206152667U (en) * | 2016-11-01 | 2017-05-10 | 武汉东湖学院 | Biological emulsion paint production of environment -friendly is with raw materials instant dispersed device |
| CN107858829A (en) * | 2017-11-28 | 2018-03-30 | 东华大学 | A kind of method that microwave oxidizing process prepares preoxidized polyacrylonitrile silk |
| CN208362539U (en) * | 2018-04-18 | 2019-01-11 | 昆明理工大学 | A kind of microwave heating polyacrylonitrile prepares the device of oxidization fiber |
| CN111088559A (en) * | 2018-10-23 | 2020-05-01 | 中国石油化工股份有限公司 | Preparation method of low-silicon-content polyacrylonitrile-based carbon fiber |
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