CN114232109B - Method for preparing polyether ketone fiber based on nondestructive dissolution wet method - Google Patents
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/06—Wet spinning methods
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- D—TEXTILES; PAPER
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- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/02—Heat treatment
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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
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- D01F6/66—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyethers
- D01F6/665—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyethers from polyetherketones, e.g. PEEK
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Abstract
The invention discloses a method for preparing a polyether ketone fiber based on a nondestructive dissolution wet method. The preparation method of the invention comprises the following steps: 1. dissolving the polyetherketoneketone in a fluorine-based or chlorine-based polar solvent at room temperature in a nondestructive manner to obtain a uniform polyetherketoneketone solution spinning solution; 2. carrying out wet spinning on the spinning solution, injecting the spinning solution into a coagulating bath through a needle head with a narrow diameter and a large length-diameter ratio for molding, and then carrying out drafting, drying and winding to obtain the as-spun polyether ketone fiber; 3. and carrying out multistage hot drawing on the as-spun polyether-ketone fiber, then winding and collecting, and carrying out high-temperature treatment and shaping to obtain the high-performance polyether-ketone fiber. The invention adopts fluorine-based or chlorine-based polar solvent to realize the nondestructive dissolution of the polyether ketone, so as to form uniform and stable colloid solution; in the spinning process, the polyether ketone forms a firm network structure under the shearing action, so that the shape and the volume of the fiber can be kept unchanged; the obtained polyether-ketone fiber has the excellent characteristics of light weight, high strength, high temperature resistance, flame retardance and the like.
Description
Technical Field
The invention relates to a method for preparing a polyether ketone fiber based on a nondestructive dissolution wet method, and belongs to the technical field of preparation of functional thermal fibers.
Background
The polymer fiber is an important component of the polymer material and plays a very important role in social life and industrial production. Among them, as one of the special fibers, a high temperature resistant fiber capable of being used for a long period of time at 180 ℃ or more or maintaining good physical properties for a certain period of time at a higher temperature has been attracting high attention.
With the high-speed development of the fields of aerospace, fire protection, nuclear industry and the like in China, the demand for high-temperature-resistant special fibers is increasing, and further optimization of the comprehensive performance of the special fibers is needed; the existing thermosetting resin has the problems of insufficient toughness, high-temperature resistant thermoplastic resin, high fiber difficulty and the like, and limits the development of high-temperature resistant special fibers.
Among thermoplastic special engineering plastics which are commercialized at present, polyaryletherketone polymers have the highest heat resistance grade. Polyaryletherketone is a semi-crystalline thermoplastic plastic and has the advantages of low density, high mechanical property, high temperature heat stability, electric insulation, chemical corrosion resistance and the like. Among the polyaryletherketone families, polyetheretherketone and polyetherketoneketone are the most widely used. In comparison, polyetherketoneketone contains more ketone bonds, has a molecular structure with a difference between the p-benzene and m-benzene ratios, has a higher glass transition temperature and melting temperature, a wider thermal control window and better mechanical properties, and has been paid more attention in recent years. The development of the high-temperature special fiber with high mechanical property based on the polyether ketone has a slight significance for transformation and upgrading of the high-performance fiber industry in China, and can be widely applied to various fields.
From the aspect of the spinning property of the polymer, the polyaryletherketone polymer generally has the problems of strong dissolution resistance, high melting temperature, poor melt fluidity and the like, so that not only is wet spinning difficult to realize, but also a plurality of difficulties are faced when the melt spinning technology is directly adopted. The main solution at present is to blend polyaryletherketone with inorganic lubricant, polyester and the like to reduce melt viscosity so as to improve processing performance, but the mechanical performance of the fiber is also reduced due to blending. The other method is to improve the dissolving capacity of the fiber by means of sulfonation, chloromethylation, ring-opening polymerization, multi-component copolymerization and the like aiming at the characteristic of indissolvable property, and spinning is carried out by adopting a solution method. However, the chemical modification of the polymer damages the original structure of the polymer, and the heat resistance, mechanical property or chemical corrosion resistance of the polymer is obviously reduced. Therefore, the preparation method of the polyaryletherketone fiber still takes the melt extrusion and the derivation process (such as melt electrostatic spinning) as the main process (document 1:M.H.G.Deeg.Process of making an aromatic polyetherketone fiber product.US patent 1985,US4747988; document 2: wang Guibin, zhang Haibo, ren Dianfu, zhang Yunhe, guan Shaowei, jiang Zhenhua, zhang Shuling, wu Zhongwen. Spinning-grade polyether-ether-ketone resin special material and the preparation method thereof; chinese patent application ZL 20080050213. X; document 3: wang Guibin, she Guangdou, zhang Shuling, jiang Zhenhua, chen Xun, kong)Melt spinning hot stretching shaping preparation method of polyether-ether-ketone fiber, chinese patent No. ZL200810050363.0; document 4: R.I.Shekar, T.M.Kotresh, P.M.D.Rao, K.Kumar.Properties of high modulus PEEK yarns for aerospace applications.j.appl.polym.sci.2009,112 (4), 2497; document 5: v is provided.
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The effect of melt spinning process parameters on the spinnability of polyeththeretherketone.j. Appl. Polym. Sci.2012,126 (5), 1564; document 6: deng Depeng, li Yunlong, gu Yuanchao, wang Ronghai, zhang Qingxin, liu Yong. Electrospinning to produce polyetherketoneketone ultrafine fibers engineering plastics applications 2016,44 (4), 44; document 7: luan Jiashuang, xu Zhiping, wang Guibin, zhang Mei, zhang Shuling, li Yonggang, cap, yang Yanchao, ma Yali A polyether-ether-ketone spun yarn and its preparation method, chinese patent ZL201710052321. X).
In addition, regarding the polyetherketoneketone fibers and polyetherketoneketone composite fibers, only the company of Axmas, inc. (the United states) and the company of Di-human aramid, inc. (the Netherlands) have filed in China related invention patents, wherein: patent CN102333910a discloses a method for preparing a polyetherketoneketone composite fiber by melt spinning, wherein multi-wall nanotubes containing elements such as carbon, nitrogen, boron, phosphorus, silicon, tungsten and the like are dispersed into a polyetherketoneketone matrix, and the polyetherketoneketone composite fiber is prepared by melt spinning; patent 201080007055.5 provides a method for preparing a composite fiber comprising polyetherketoneketone and mineral nanotubes, wherein various mineral nanotubes are mixed with a polyetherketoneketone matrix in a melt compounding manner, and then the composite fiber is prepared by melt spinning; the patent CN110249083A is the only Chinese patent for preparing the polyether-ketone fiber by wet spinning at present, is the application of PCT International patent WO 2018/087121 in China, and adopts concentrated sulfuric acid to dissolve the polyether-ketone to obtain a spinning solution, and the spinning solution enters a coagulating bath through a spinneret to prepare the polyether-ketone fiber. However, the method still has a series of technical problems to limit the development and application of the method: 1) Dissolution of polyetherketoneketone in concentrated sulfuric acid is actually a sulfonation process of a polymer (document 1: R.Y.M.Huang, P.Shao, C.M.Burns, X.Feng.Sulfonation of poly (ether ether ketone) (PEEK): kinetic study and organization.J.appl.Polym.Sci.2001, 82 (11), 2651; document 2: B.Li, T.Liu, Z.C.W.Tang, J.Jia, w. -h.zhong.novel hydration induced flexible sulfonated poly (etherketoneketone) foam with super dielectric reagents.j.mate.chem.2011, 21 (35), 13546) the polyetherketoneketone has undergone sulphonation reaction during dissolution, which has a great influence on the properties of the spun fibres; 2) The dissolution of polyetherketoneketone in concentrated sulfuric acid requires an additional mechanical mixing process, such as the patent recommends the use of kneaders or extruders to facilitate the mixing process, which means that achieving uniform mixing or dissolution remains difficult; 3) The spinning dope is preferably carried out at a temperature of 50 to 90 ℃, which on the one hand can further promote the sulfonation of the polyetherketoneketone in the temperature region, and on the other hand requires additional temperature control equipment, which brings difficulty to the stability of wet spinning; 4) Residual acid exists in the polyether-ketone fiber obtained by wet spinning, and the pH value of the coagulating bath is required to be increased to promote the neutralization; 5) The obtained fiber structure has poor uniformity, the mechanical strength is lower than 80MPa, and the fiber structure is difficult to be widely applied. Based on the above problems, there is a need to develop efficient, stable wet spinning to produce high performance polyetherketoneketone fibers.
Disclosure of Invention
The invention solves the technical problems that: there is currently only a related art for preparing polyetherketoneketone (composite) fibers by melt spinning, whereas wet spinning achieved using concentrated sulfuric acid is a sulfonation means based on polyetherketoneketone polymers, which is dissolved as sulfonated polyetherketoneketone, and thus there is no related art for wet spinning by non-destructive dissolution of polyetherketoneketone. In addition, the spinning method is carried out at high temperature or a mechanical mixing process is required to be introduced, so that the steps are complicated, the cost is high, and the obtained fiber mechanics has the problems of poor structural uniformity, low strength, poor performance and the like.
In order to solve the technical problems, the invention provides a method for preparing a polyether ketone fiber based on nondestructive dissolution, which comprises the following steps:
step 1: adopting fluorine-based or chlorine-based polar solvent to dissolve the polyether ketone in a nondestructive manner to obtain spinning solution;
step 2: carrying out wet spinning on the spinning solution obtained in the step 1, injecting the wet spinning solution into a coagulating bath for coagulating and forming, and pre-drafting, drying and winding to obtain a primary spinning polyether ketone fiber;
step 3: and (3) winding and collecting the as-spun polyether-ketone fiber obtained in the step (2) after multistage hot drawing, and performing heat treatment and shaping to obtain the polyether-ketone fiber.
Preferably, in the polyetherketoneketone in the step 1, the molar ratio of the para-position structure to the ortho-position structure (abbreviated as para-position to ortho-position structure ratio, or T/I ratio) is 50:50, 60:40, 70:30, 80:20 or 100:0, and the polyetherketoneketone is powder with the particle size less than or equal to 300 μm.
Preferably, the fluorine base solvent in the step 1 is trifluoroacetic acid and/or 3, 3-trifluoro-2, 2-dimethylpropionic acid; the chlorine base solvent is at least one of p-chlorophenol, dichloroacetic acid and dichloropropionic acid.
More preferably, the fluorine base solvent is trifluoroacetic acid and the chlorine base solvent is p-chlorophenol.
Preferably, the process parameters of the dissolution in the step 1 are as follows: stirring speed is 1200-1800 rpm, stirring time is 6-12 h, and stirring temperature is 25-50 ℃; the concentration of the polyether ketone in the spinning solution is 5-22 wt%.
Preferably, the wet spinning in the step 2 adopts a needle with a narrow diameter and a large length-diameter ratio, wherein the inner diameter of the needle is 0.1-0.5 mm, and the length of the needle is 50-100 mm; the technological parameters of the injection are as follows: the extrusion rate is 0.05-2 mL/min, and the extrusion temperature is 25-30 ℃.
Preferably, the coagulation bath in the step 2 is water or ethanol, wherein water is preferred when trifluoroacetic acid, 3-trifluoro-2, 2-dimethylpropionic acid, dichloroacetic acid and dichloropropionic acid are selected as solvents, and ethanol is preferred when parachlorophenol is selected as a solvent.
Preferably, the temperature of the coagulation bath in the step 2 is 5 to 40 ℃, and the time required for the molding is 0.5 to 2 minutes.
More preferably, the temperature of the coagulation bath is 25 to 30 ℃.
Preferably, the pre-stretching in the step 2 is specifically: and (3) guiding the polyether-ketone fibers obtained by solidification forming out of a solidification bath, drawing the fibers through 3-5 guide rails, wherein the drawing multiple is 1-2 times, and the drawing time is 1-5 min, so that the fibers are naturally dried, and winding and collecting the fibers after pre-drawing.
Preferably, the heat drawing in the step 3 is that the as-spun polyether ketone fiber obtained in the step 2 is heat drawn by a horizontal tube furnace, the length of the furnace body of the horizontal tube furnace is 50-90 cm, the heat drawing adopts three-stage heat drawing, and specific technological parameters are as follows: the first stage drawing temperature is 200-220 ℃, the drawing multiple is 2-3.5 times, the second stage drawing temperature is 230-250 ℃, the drawing multiple is 1.5-2 times, the third stage drawing temperature is 240-260 ℃, and the drawing multiple is 1.5-2 times.
Preferably, the temperature of the heat treatment shaping in the step 3 is 240-300 ℃ and the time is 1-5 h.
More preferably, the temperature of the heat treatment setting is 250-280 ℃ and the time is 1.5-2 h.
The invention also provides the polyether ketone fiber prepared by the method based on nondestructive dissolution, and the mass density of the polyether ketone fiber is lower than 0.9g/cm 3 The porosity is higher than 30%, the tensile breaking strength is higher than 600MPa, the thermal weight loss temperature is higher than 450 ℃, and the flame retardant grade is V-0.
The design idea of the invention is as follows:
(1) The fluorine-based or chlorine-based polar solvent is used for nondestructively dissolving the polyether ketone, so that the polyether ketone is truly dissolved, the sulfonation reaction caused by dissolving the polyether ketone by adopting concentrated sulfuric acid is avoided, and the excellent physical properties of the polyether ketone are fully maintained in the fiber;
(2) The polyether ketone solution forms a firm network structure under the shearing action of the wet spinning process, and the rigidity of molecules of the polyether ketone solution is combined, so that the fiber shape and the volume of the polyether ketone fiber can be kept unchanged in the forming process (the phase separation of the solvent and the polyether ketone occurs in the forming process), and the generation of a microporous structure is more favorably induced by the phase separation;
(3) The polymer molecules in the polyether ketone fiber not only construct a compact network structure, but also form a rich micropore structure, thereby realizing organic integration of various properties, such as light weight, high strength, high temperature resistance, flame retardance and the like.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention uses fluorine-based or chlorine-based polar solvent to dissolve the polyetherketoneketone in a nondestructive way, prepares the as-spun polyetherketoneketone fiber by regulating and controlling the concentration of spinning solution, the specification of a needle, the extrusion rate, the type of a coagulating bath and the pre-drawing rate in the wet spinning process, and then obtains the high-performance polyetherketoneketone fiber through hot drawing and high-temperature setting treatment, and the difference is that the fiber volume can shrink obviously in the wet spinning process of other polymers, and the unique molecular rigidity and entanglement characteristic of the polyetherketoneketone ensures that the fiber volume is kept unchanged in the phase separation process of fiber forming, thereby constructing a rich microporous structure in the fiber, and further optimizing and regulating in the hot drawing process; the polyether-ketone fiber prepared by the invention has the excellent characteristics of light weight, high strength, high temperature resistance, flame retardance and the like.
2. Because the polyaryletherketone polymer is generally difficult to dissolve, the related wet spinning process is very deficient, and the higher melting temperature of the polyaryletherketone polymer also brings a plurality of difficulties to melt spinning, the invention realizes new breakthrough of the polyetherketoneketone wet spinning, realizes the efficient and stable preparation process, has sufficient regulation and control space for the microstructure of the fiber, provides possibility for developing various types of fiber products, and has wide application prospect.
Drawings
FIG. 1 is the spinning dope obtained in step 1 of example 1;
FIG. 2 is a drawing of the as-spun polyether ketone fibers obtained in step 3 of example 1;
FIG. 3 is a heat-set polyetherketoneketone fiber obtained in step 5 of example 1;
FIG. 4 is a cross-sectional electron microscope scanning image of the polyether ketone fibers prepared in example 1;
FIG. 5 is a mechanical test result of the polyether ketone fiber prepared in example 1;
FIG. 6 is a thermal weight loss test result of the polyether-ketone fiber prepared in example 1 in an air environment;
FIG. 7 is a flame retardant test result of the polyether ketone fiber prepared in example 1.
Detailed Description
In order to make the present invention more comprehensible, preferred embodiments accompanied with the present invention are described in detail below.
Example 1
The embodiment provides a method for preparing a polyether ketone fiber based on a nondestructive dissolution wet method, which specifically comprises the following steps:
1) Firstly, preparing a polyether ketone solution, dissolving polyether ketone (T/I ratio is 60:40) in trifluoroacetic acid at room temperature (25 ℃) with concentration of 12.5wt%, stirring at 1500rpm for 6 hours, and obtaining a uniform and stable spinning solution, as shown in figure 1.
2) The polyether ketone solution is injected into pure water coagulation bath with the temperature of room temperature by adopting an injection needle with the inner diameter of 0.15mm and the length of 60cm, and the extrusion rate is 0.2mL/min. The time that the fiber passed in the coagulation bath was 50s.
3) The solidified and formed fiber is led out of a coagulating bath, is subjected to pre-drawing under the action of drawing through 5 guide rails, the drawing time is 2min, and is directly collected on a winding drum after drawing, so that the natural drying primary spinning polyether ketone fiber is obtained, and the drawing is shown in figure 2.
4) The initially spun polyether-ketone fiber is led out from a winding drum, is subjected to hot drawing treatment through a horizontal tube furnace, and is collected on another winding drum. A tubular furnace with the length of 80cm is adopted, three-stage (secondary) hot drawing is adopted, wherein the first-stage drawing temperature is 210 ℃, the drawing multiple is 2 times, the second-stage drawing temperature is 240 ℃, the drawing multiple is 2 times, and the third-stage drawing temperature is 260 ℃, and the drawing multiple is 1.5 times.
5) And (3) putting the polyether-ketone fiber after hot drawing and the winding drum into a hot oven for high-temperature heat setting treatment, wherein the heat setting temperature is 280 ℃, and the heat setting time is 1.5h, so that the heat-set polyether-ketone fiber is obtained, and the heat-set polyether-ketone fiber is shown in figure 3.
The polyether ketone fiber obtained by the steps has uniform diameter of 52 mu m and mass density of 0.85g/cm 3 (corresponding to 34.6% of porosity), the tensile breaking strength is 650MPa, the thermal weight loss temperature is higher than 455 ℃, and the flame retardant grade is V-0. Fig. 4 to 7 show the cross-sectional electron microscope scanning photographs, the mechanical test curves, the weightlessness test curves and the flame-retardant test results of the fiber.
Example 2
The embodiment provides a method for preparing a polyether ketone fiber based on a nondestructive dissolution wet method, which specifically comprises the following steps:
1) Firstly, preparing a polyether ketone solution, dissolving polyether ketone (T/I ratio is 60:40) in trifluoroacetic acid at the temperature of 40 ℃ to obtain a uniform and stable spinning stock solution, wherein the concentration is 22wt%, the stirring speed is 1800rpm, and the stirring time is 6 hours.
2) The polyether ketone solution was injected into a pure water coagulation bath at 40℃at room temperature using an injection needle having an inner diameter of 0.5mm and a length of 50cm, and the extrusion rate was 2mL/min. The time that the fiber passed in the coagulation bath was 2min.
3) And (3) guiding the coagulated and formed fiber out of a coagulating bath, passing through 5 guide rails, pre-drawing under the action of traction, wherein the drawing multiple is 1.1 times, the drawing time is 2 minutes, and directly collecting the drawn fiber on a winding drum to obtain the natural dry as-spun polyether ketone fiber.
4) The initially spun polyether-ketone fiber is led out from a winding drum, is subjected to hot drawing treatment through a horizontal tube furnace, and is collected on another winding drum. A tubular furnace with the length of 80cm is adopted, three-stage (secondary) hot drawing is adopted, wherein the first-stage drawing temperature is 210 ℃, the drawing multiple is 3 times, the second-stage drawing temperature is 240 ℃, the drawing multiple is 2 times, and the third-stage drawing temperature is 260 ℃, and the drawing multiple is 1.5 times.
5) And (3) putting the polyether-ketone fiber after hot drawing and the winding drum into a hot oven for high-temperature heat setting treatment, wherein the heat setting temperature is 280 ℃, and the heat setting time is 2 hours, so that the heat-set polyether-ketone fiber is obtained.
The polyether ketone fiber obtained by the steps has the diameter of 160 mu m and the mass density of 0.87g/cm 3 (corresponding to 33.1% of porosity), the tensile breaking strength is 605MPa, the thermal weight loss temperature is higher than 455 ℃, and the flame retardant grade is V-0.
Example 3
The embodiment provides a method for preparing a polyether ketone fiber based on a nondestructive dissolution wet method, which specifically comprises the following steps:
1) Preparing a polyether ketone solution, dissolving polyether ketone (T/I is 50:50) in p-chlorophenol at 50 ℃ with the concentration of 8.5wt%, and stirring at 1200rpm for 12 hours to obtain a uniform and stable wet spinning solution.
2) The same procedure as in step 2) of example 1 was followed, except that the coagulation bath was ethanol.
3) -5): steps 3) -5) as in example 1.
The polyether ketone fiber obtained by the steps has the diameter of 38 mu m and the mass density of 0.84g/cm 3 (corresponding to 35.4 percent of porosity), tensile breaking strength is 675MPa, thermal weight loss temperature is higher than 455 ℃, and flame retardant grade is V-0 grade.
Example 4
The embodiment provides a method for preparing a polyether ketone fiber based on a nondestructive dissolution wet method, which specifically comprises the following steps:
1) Preparing a polyether ketone solution, dissolving polyether ketone (T/I ratio is 70:30) in parachlorophenol at 50 ℃ with concentration of 12wt%, stirring at 1800rpm for 9 hours, and obtaining a uniform and stable wet spinning stock solution.
2) The same procedure as in step 2) of example 1 was followed, except that the coagulation bath was ethanol.
3) -5): steps 3) -5) as in example 1.
The polyether ketone fiber obtained by the steps has the diameter of 59 mu m and the mass density of 0.86g/cm 3 (corresponding pore space)The rate is 33.8 percent), the tensile breaking strength is 685MPa, the thermal weight loss temperature is higher than 455 ℃, and the flame retardant grade is V-0 grade.
Comparative example 1
1) And (3) preparing a polyether ketone solution, namely dissolving polyether ketone (T/I ratio is 60:40) in trifluoroacetic acid at room temperature, wherein the concentration is 4.5wt%, and the stirring speed is 1200rpm, and the stirring time is 6 hours, so that a uniform and stable spinning stock solution is obtained.
2) In the same manner as in step 2) of example 1, continuous spinning was not formed, and a segmented polyetherketoneketone staple was obtained.
Comparative example 2
1) The same procedure as in step 1) of example 1 was followed.
2) The same operation as in step 2) of example 1 was performed except that the extrusion rate was 3mL/min, and the PEEK fiber was curled at high injection speed, and it was difficult to stably draw, and continuous spinning could not be formed.
While the invention has been described with respect to preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (6)
1. A method for preparing a polyetherketoneketone fiber based on non-destructive dissolution, which is characterized by comprising the following steps:
step 1: adopting fluorine-based or chlorine-based polar solvent to dissolve the polyether ketone in a nondestructive manner to obtain spinning solution;
step 2: carrying out wet spinning on the spinning solution obtained in the step 1, injecting the wet spinning solution into a coagulating bath for coagulating and forming, and pre-drafting, drying and winding to obtain a primary spinning polyether ketone fiber;
step 3: winding and collecting the as-spun polyether-ketone fiber obtained in the step 2 after multistage hot drawing, and performing heat treatment and shaping to obtain the polyether-ketone fiber;
in the polyetherketoneketone in the step 1, the molar ratio of the para-benzene position structure to the ortho-benzene position structure is 50:50, 60:40, 70:30, 80:20 or 100:0, and the polyetherketoneketone is powder with the particle size less than or equal to 300 mu m;
the fluorine base solvent in the step 1 is trifluoroacetic acid and/or 3, 3-trifluoro-2, 2-dimethylpropionic acid; the chlorine base polar solvent is at least one of p-chlorophenol, dichloroacetic acid and dichloropropionic acid;
the dissolved technological parameters in the step 1 are as follows: stirring speed is 1200-1800 rpm, stirring time is 6-12 h, and stirring temperature is 25-50 ℃; the concentration of the polyether ketone in the spinning solution is 5-22 wt%;
the wet spinning in the step 2 adopts a needle head with the inner diameter of 0.1-0.5 mm and the length of 50-100 mm; the technological parameters of the injection are as follows: the extrusion rate is 0.05-2 mL/min, and the extrusion temperature is 25-30 ℃;
the mass density of the polyether ketone fiber prepared in the step 3 is lower than 0.9g/cm 3 The porosity is higher than 30%, the tensile breaking strength is higher than 600MPa, the thermal weight loss temperature is higher than 450 ℃, and the flame retardant grade is V-0.
2. The method for preparing polyetherketoneketone fibers based on non-destructive dissolution according to claim 1, wherein the coagulation bath in step 2 is water or ethanol.
3. The method for preparing the polyetherketoneketone fiber based on non-destructive dissolution according to claim 1, wherein the temperature of the coagulation bath in the step 2 is 5 to 40 ℃, and the time required for the molding is 0.5 to 2min; the pre-drafting specifically comprises the following steps: and (3) guiding the polyether-ketone fibers obtained by solidification forming out of a solidification bath, drawing the fibers through 3-5 guide rails, wherein the drawing multiple is 1-2 times, and the drawing time is 1-5 min, so that the fibers are naturally dried, and winding and collecting the fibers after pre-drawing.
4. The method for preparing the polyetherketoneketone fiber based on nondestructive dissolution according to claim 1, wherein the hot drawing in the step 3 is that the as-spun polyetherketoneketone fiber obtained in the step 2 is hot drawn by a horizontal tube furnace, the length of the furnace body of the horizontal tube furnace is 50-90 cm, the hot drawing adopts three-stage hot drawing, and the specific technological parameters are as follows: the first stage drawing temperature is 200-220 ℃, the drawing multiple is 2-3.5 times, the second stage drawing temperature is 230-250 ℃, the drawing multiple is 1.5-2 times, the third stage drawing temperature is 240-260 ℃, and the drawing multiple is 1.5-2 times.
5. The method for preparing the polyetherketoneketone fiber based on non-destructive dissolution according to claim 1, wherein the heat treatment setting temperature in the step 3 is 240-300 ℃ for 1-5 hours.
6. The polyetherketoneketone fiber prepared by the process for preparing polyetherketoneketone fibers based on non-destructive dissolution according to any one of claims 1 to 5, wherein the polyetherketoneketone fiber has a mass density of less than 0.9g/cm 3 The porosity is higher than 30%, the tensile breaking strength is higher than 600MPa, the thermal weight loss temperature is higher than 450 ℃, and the flame retardant grade is V-0.
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