CN101922062B - Preparation method for meta-aromatic polyamide fiber - Google Patents
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Abstract
The invention relates to a preparation method for meta-aromatic polyamide fiber, comprising the following steps: (1) enabling metaphenylene diamine and m-phthaloyl chloride to be subject to low-temperature solution polymerization in an amide solvent, and utilizing calcium hydroxide to neutralize hydrogen chloride generated in the polymerization process; (2) after filtering, defoaming and metering the obtained spinning serous fluid, spraying into a multistage coagulating bath through the spinning nozzle of a spinneret orifice with the diameter of 0.08 mm, carrying out solidification and shaping step by step, and finally completely solidifying the fiber; and (3) carrying out moist heat drawing, washing, drying, dry heat drawing and heat shaping on solidified as-formed fiber to obtain the needed meta-aromatic polyamide fiber. The invention improves the fiber tensile strength, and the prepared fiber have round, even and compact cross section and excellent mechanical property, thereby enabling the prepared fiber to have better application prospect.
Description
Technical field
The invention belongs to wet spinning and prepare fiber art, particularly relate to a kind of preparation method of meta-aromatic polyamide fiber.
Background technology
Meta-aromatic polyamide fiber has excellent heat resistance and flame resistant property; And excellent high temperature electrical insulating property; Also have the spinning property similar simultaneously with cotton fiber, thus be widely used in occasions such as high temperature resistant and fire prevention, and protective clothing, high temperature filter material and electrically insulating material.
The preparation method of existing meta-aromatic polyamide fiber mainly contains two kinds:
(1) with m-phenylene diamine (MPD) and m-phthaloyl chloride at N; Low temperature solution polymerization in the N-two formyl acetamides (DMAc); The hydrogen chloride that reaction generates has the calcium hydroxide neutralization; Obtain containing the spinning solution of the poly of calcium chloride, calcium chloride content wherein is that benchmark is about 45wt% with the polymer.Above-mentioned spinning solution is used for dry spinning or wet spinning technology prepares the mpd-i fiber, shown in United States Patent (USP) 3360595.
(2) use m-phenylene diamine (MPD) and m-phthaloyl chloride to be cosolvent with the calcium chloride below the polymer benchmark 15wt% with the polymer powder that interfacial polymerization or emulsion polymerisation obtain; Be dissolved in the amide solvent; The polymer solution that obtains is that coagulating bath is carried out wet spinning and prepared fiber with the amide solvent aqueous solution that contains inorganic salts, shown in United States Patent (USP) 3006889 and 3640970.The solidification forming of the fiber in the wet spinning process of above-mentioned two kinds of methods is vital.The process of setting of fiber is a double diffusion process, that is: coagulating agent (like water) is to the fibrous inside diffusion, and solvent (like amide solvent) or cosolvent (like calcium chloride) are to the outside diffusion of fiber.Existing wet spinning technology all is that the mode that adopts a step to solidify is carried out solidification forming to fiber, accomplishes the double diffusion process.One-step method is solidified and possibly caused: can cause fiber to solidify not exclusively when the solvent in the coagulating bath is too much, thereby cause the as-spun fibre doubling, influence follow-up tensile property or cause the denier irregularity of finished fiber to increase; When solvent is very few, can cause process of setting too fast, thereby cause the fibrous inside cavity to be increased, micropore increases, and influences the mechanical property of finished fiber.Though under certain coagulating bath proportioning, can obtain the less fiber of interior void under the condition of one-level coagulating bath, the micropore of the fiber of this moment is bigger, and is fine and close inadequately, and is easy to form skin-core structure, influences fibre property.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of meta-aromatic polyamide fiber, with the effective mechanical property that further improves meta-aromatic polyamide fiber, thereby makes it that better application prospect arranged.
The preparation method of a kind of meta-aromatic polyamide fiber of the present invention comprises:
(1) m-phenylene diamine (MPD) and m-phthaloyl chloride with equivalent than in amide solvent through low temperature solution polymerization, the hydrogen chloride that produces in the polymerization process is neutralized by calcium hydroxide, thereby makes the pH value of solution 6.0～8.0, the spinning solution that polymerization obtains;
(2) spinning slurry that obtains is through filtration, deaeration; Temperature is controlled at 60 ℃; Spinning solution is through being measured by measuring pump under the nitrogen pressure of 0.2～0.5MPa; From diameter is that the spinning head ejection back of 0.08mm spinneret orifice gets into multistage coagulating bath and carries out progressively coagulation forming, reaches fiber at last and solidifies fully and solidify;
(3) after the as-spun fibre after solidifying carries out damp and hot stretching, washing, drying, xeothermic stretching, HEAT SETTING, obtain required meta-aromatic polyamide fiber.
Polymerisation in solution in the said step (1) requires to comprising the meta-aromatic polyamide of 15～25wt%; The calcium chloride of 7～11wt%; The water of 1～2wt%, all the other are amide solvent, wherein amide solvent is N ' N-dimethylacetylamide (DMAc) or N-Methyl pyrrolidone (NMP).
The logarithmic viscosity number of polymer is 1.5-2.2 in the spinning solution in the said step (1).
Progression >=2 that multistage coagulating bath in the said step (2) is selected for use.
It is H that said multistage coagulating bath specifically consists of the one-level coagulation bath composition
2O 20～40wt%, amide solvent 50～70wt%, calcium chloride 5～15wt%, bathing temperature is 0～30 ℃.The secondary coagulation bath composition is H
2O30～50wt%, amide solvent 40～60wt%, calcium chloride 0～10wt%, bathing temperature is 20～50 ℃.Coagulation bath composition greater than secondary is H
2O40～60wt%, amide solvent 30～50wt%, calcium chloride 0～5wt%, bathing temperature is 40～70 ℃.
The temperature of the damp and hot stretching in the said step (3) is 60～100 ℃, and damp and hot stretch bath is the aqueous solution of the amide solvent identical with coagulating bath, and the concentration of amide solvent is 0～20wt%, and draw ratio is 2.0～4.0, divides and carries out for 1～3 time.
The temperature of the xeothermic stretching in the said step (3) is 270～350 ℃, is drawing medium with nitrogen, and draw ratio is 1.0～4.0.
The temperature of the HEAT SETTING in the said step (3) is 270～350 ℃, is medium with nitrogen, draw ratio 1.001～1.005.
The tensile strength of the fiber that obtains is greater than 4.5cN/dtex, and elongation at break is 20～60wt%.
Description of drawings
Fig. 1 is the cross sectional shape of fiber sample S1, and wherein (a) is for amplifying 500 times, (b) for amplifying 2000 times;
Fig. 2 is fiber sample B1
*Cross sectional shape;
Fig. 3 is the cross sectional shape of fiber sample B2, and wherein (a) is for amplifying 500 times, (b) for amplifying 2000 times;
Fig. 4 is the cross sectional shape of fiber sample B3, and wherein (a) is for amplifying 500 times, (b) for amplifying 2000 times.
Beneficial effect
Compared with former spinning technique; The present invention adopts the new technological flow of multistage coagulating bath method to make the process of setting of fiber carry out step by step, for the different phase of process of setting, adopts different coagulation bath condition to realize different curing rates; Thereby can both realize well solidifying inside and outside making fiber; Can realize that the fibre section even structure is fine and close, no skin-core structure, thereby the TENSILE STRENGTH of raising fiber.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in the restriction scope of the present invention.Should be understood that in addition those skilled in the art can do various changes or modification to the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
The refining m-phenylene diamine (MPD) (MPD) of 1 parts by weight is dissolved among the DMAc of drying of new distillation of 8.7 parts by weight; Carried out precondensation at-10 ℃ of refining m-phthaloyl chlorides (IPC) that add 1.7 parts by weight down; The IPC that generation contains behind the prepolymer of hydrogen chloride with remaining 0.18 parts by weight carries out polymerization; The temperature of control reactor obtains water white condensate reaction below 50 ℃ 1 hour.The subsequent neutralization, the Ca (OH) that neutralization is used
2Parts by weight be 0.685.Finally obtain containing polymer 18.1wt%, logarithmic specific concentration viscosity η
InhBe 1.86, CaCl
2Content is the spinning solution of 8.26wt%.Deaeration, with temperature be controlled at 60 ℃ of spinning solutions through under the nitrogen pressure of 0.2～0.5MPa by after the measuring pump metering, be that the spinnerets of 0.08mm spinneret orifice is extruded and got in the one-level coagulating bath through 300 bore dias, this coagulation bath composition is H
2O 40wt%, DMAc50wt%, calcium chloride 10wt%, bathing temperature is 20 ℃, immersion length is 1.5m; Meta-aromatic polyamide coagulated yarn through solidifying in advance solidifies through solidifying the coagulating bath of roller entering secondary again, and coagulation bath composition is H
2O50wt%, DMAc45wt%, calcium chloride 5wt%, bathing temperature is 30 ℃, immersion length is 1.5m; The last meta-aromatic polyamide coagulated yarn that solidifies basically gets into three grades of coagulating baths and carries out final set, and coagulation bath composition is H
2O60wt%, DMAc 38wt%, calcium chloride 2wt%, bathing temperature is 60 ℃, immersion length is 1.5m.Get into wet stretch bath through the meta-aromatic polyamide coagulated yarn that solidifies for three times; Temperature is 100 ℃, and draw ratio is 2.0 times, and the coagulated yarn after the stretching is through washing after oven dry under 150 ℃ the temperature; Draw ratio with 2.0 in 300 ℃ heat pipe carries out xeothermic stretching; Under 320 ℃, carry out HEAT SETTING, oiling at last makes finished fiber, is numbered S1.
Embodiment 2
The refining m-phenylene diamine (MPD) (MPD) of 1 parts by weight is dissolved among the NMP of drying of new distillation of 8.7 parts by weight; Carried out precondensation at-10 ℃ of refining m-phthaloyl chlorides (IPC) that add 1.7 parts by weight down; The IPC that generation contains behind the prepolymer of hydrogen chloride with remaining 0.18 parts by weight carries out polymerization; The temperature of control reactor obtains water white condensate reaction below 50 ℃ 1 hour.The subsequent neutralization, the Ca (OH) that neutralization is used
2Parts by weight be 0.685.Finally obtain containing polymer 18.1%, logarithmic specific concentration viscosity η
InhBe 1.86, CaCl
2Content is 8.26% spinning solution.Deaeration, with temperature be controlled at 60 ℃ of spinning solutions through under the nitrogen pressure of 0.2～0.5MPa by after the measuring pump metering, be that the spinnerets of 0.08mm spinneret orifice is extruded and got in the one-level coagulating bath through 300 bore dias, this coagulation bath composition is H
2O20wt%, NMP70wt%, calcium chloride 10wt%, bathing temperature is 30 ℃, immersion length is 1.5m; Meta-aromatic polyamide coagulated yarn through solidifying in advance solidifies through solidifying the coagulating bath of roller entering secondary again, and coagulation bath composition is H
2O35wt%, NMP60wt%, calcium chloride 5wt%, bathing temperature is 40 ℃, immersion length is 1.5m.The meta-aromatic polyamide coagulated yarn that solidifies through secondary gets into wet stretch bath; Temperature is 80 ℃; Draw ratio is 3.0 times, and after oven dry under 150 ℃ the temperature, the draw ratio with 3.0 in 280 ℃ heat pipe carries out xeothermic stretching to the coagulated yarn after the stretching through washing; Under 320 ℃, carry out HEAT SETTING, oiling at last makes finished fiber.The tensile strength of product fiber is 4.8cNdex
-1, extension at break is 30%.
Embodiment 3
The refining m-phenylene diamine (MPD) (MPD) of 1 parts by weight is dissolved among the DMAc of drying of new distillation of 10 parts by weight; Carried out precondensation at-10 ℃ of refining m-phthaloyl chlorides (IPC) that add 1.7 parts by weight down; The IPC that generation contains behind the prepolymer of hydrogen chloride with residue 0.18 parts by weight carries out polymerization; The temperature of control reactor obtains water white condensate reaction below 50 ℃ 1 hour.The subsequent neutralization, the Ca (OH) that neutralization is used
2Parts by weight be 0.685.Finally obtain containing polymer 15.8, logarithmic specific concentration viscosity η
InhBe 1.71, CaCl
2Content is 7.21 spinning solution.Deaeration, with temperature be controlled at 60 ℃ of spinning solutions through under the nitrogen pressure of 0.2～0.5MPa by after the measuring pump metering, be that the spinnerets of 0.08mm spinneret orifice is extruded and got in the one-level coagulating bath through 300 bore dias, this coagulation bath composition is H
2O 30wt%, DMAc55wt%, calcium chloride 15wt%, bathing temperature is 10 ℃, immersion length is 1.5m; Meta-aromatic polyamide coagulated yarn through solidifying in advance solidifies through solidifying the coagulating bath of roller entering secondary again, and coagulation bath composition is H
2O40wt%, DMAc50wt%, calcium chloride 10wt%, bathing temperature is 30 ℃, immersion length is 1.5m; The last meta-aromatic polyamide coagulated yarn that solidifies basically gets into three grades of coagulating baths and carries out final set, and coagulation bath composition is H
2O55wt%, DMAc40wt%, calcium chloride 5wt%, bathing temperature is 50 ℃, immersion length is 1.5m.Get into wet stretch bath through the meta-aromatic polyamide coagulated yarn that solidifies for three times; Temperature is 60 ℃; Draw ratio is 4.0 times, and after oven dry under 150 ℃ the temperature, the draw ratio with 4.0 in 350 ℃ heat pipe carries out xeothermic stretching to the coagulated yarn after the stretching through washing; Under 320 ℃, carry out HEAT SETTING, oiling at last makes finished fiber.The tensile strength of product fiber is 5.4cNdex
-1, extension at break is 38%.
Comparative example 1
The preparation of spinning solution is with embodiment 1.Spinning process is also basically with embodiment 1, and different is that the one-level coagulating bath is adopted in coagulating bath, only carries out solidification forming with a coagulating bath to extruding strand, and coagulation bath composition is H
2O40wt%, amide solvent 50wt%, calcium chloride 10wt%, bathing temperature is 20 ℃, immersion length is 2.0m.The gained fiber is numbered B1.
Comparative example 2
The preparation of spinning solution is with embodiment 1.Spinning process is also basically with embodiment 1, and different is that the one-level coagulating bath is adopted in coagulating bath, only carries out solidification forming with a coagulating bath to extruding strand, and coagulation bath composition is H
2O50wt%, amide solvent 45wt%, calcium chloride 5wt%, bathing temperature is 10 ℃, immersion length is 2.0m.The gained fiber is numbered B2.
Comparative example 3
The preparation of spinning solution is with embodiment 1.Spinning process is also basically with embodiment 1, and different is that the one-level coagulating bath is adopted in coagulating bath, only carries out solidification forming with a coagulating bath to extruding strand, and coagulation bath composition is H
2O60wt%, amide solvent 38wt%, calcium chloride 2wt%, bathing temperature is 10 ℃, immersion length is 2.0m.The gained fiber is numbered B3.
Table 1: the TENSILE STRENGTH of each fiber sample
| The fiber sample numbering | Tensile strength/cNdex -1 | Extension at break/% |
| S1 | 5.6 | 36 |
| B1 * | - | - |
| B2 | 3.5 | 40 |
| B3 | 2.2 | 25 |
*: the fiber doubling
Table 2: the cross sectional shape of each fiber sample
Claims (9)
1. the preparation method of a meta-aromatic polyamide fiber comprises:
(1) m-phenylene diamine (MPD) and m-phthaloyl chloride with equivalent than in amide solvent through low temperature solution polymerization, the hydrogen chloride that produces in the polymerization process is neutralized by calcium hydroxide, thereby makes the pH value of solution 6.0～8.0, the spinning solution that polymerization obtains;
(2) spinning slurry that obtains is through filtration, deaeration; Temperature is controlled at 60 ℃; Spinning solution is through being measured by measuring pump under the nitrogen pressure of 0.2～0.5MPa; From diameter is that the spinning head ejection back of 0.08mm spinneret orifice gets into multistage coagulating bath and carries out progressively coagulation forming, reaches fiber at last and solidifies fully and solidify;
(3) after the as-spun fibre after solidifying carries out damp and hot stretching, washing, drying, xeothermic stretching, HEAT SETTING, obtain required meta-aromatic polyamide fiber.
2. the preparation method of a kind of meta-aromatic polyamide fiber according to claim 1; It is characterized in that: the polymerisation in solution in the said step (1) requires to comprising the meta-aromatic polyamide of 15～25wt%; The calcium chloride of 7～11wt%; The water of 1～2wt%, all the other are amide solvent, wherein amide solvent is N ' N-dimethylacetylamide DMAc or N-Methyl pyrrolidone NMP.
3. the preparation method of a kind of meta-aromatic polyamide fiber according to claim 1, it is characterized in that: the logarithmic viscosity number of polymer is 1.5-2.2 in the spinning solution in the said step (1).
4. the preparation method of a kind of meta-aromatic polyamide fiber according to claim 1 is characterized in that: progression >=2 that the multistage coagulating bath in the said step (2) is selected for use.
5. the preparation method of a kind of meta-aromatic polyamide fiber according to claim 4, it is characterized in that: it is H that said multistage coagulating bath specifically consists of the one-level coagulation bath composition
2O 20～40wt%, amide solvent 50～70wt%, calcium chloride 5～15wt%, bathing temperature is 0～30 ℃; The secondary coagulation bath composition is H
2O30～50wt%, amide solvent 40～60wt%, calcium chloride 0～10wt%, bathing temperature is 20～50 ℃; Coagulation bath composition greater than secondary is H
2O40～60wt%, amide solvent 30～50wt%, calcium chloride 0～5wt%, bathing temperature is 40～70 ℃.
6. the preparation method of a kind of meta-aromatic polyamide fiber according to claim 1; It is characterized in that: the temperature of the damp and hot stretching in the said step (3) is 60～100 ℃; Damp and hot stretch bath is the aqueous solution of the amide solvent identical with coagulating bath; The concentration of amide solvent is 0～20wt%, and draw ratio is 2.0～4.0, divides and carries out for 1～3 time.
7. the preparation method of a kind of meta-aromatic polyamide fiber according to claim 1, it is characterized in that: the temperature of the xeothermic stretching in the said step (3) is 270～350 ℃, is drawing medium with nitrogen, draw ratio is 1.0～4.0.
8. the preparation method of a kind of meta-aromatic polyamide fiber according to claim 1, it is characterized in that: the temperature of the HEAT SETTING in the said step (3) is 270～350 ℃, is medium with nitrogen, draw ratio 1.001～1.005.
9. the preparation method of a kind of meta-aromatic polyamide fiber according to claim 1, it is characterized in that: the tensile strength of the fiber that obtains is greater than 4.5cN/dtex, and elongation at break is 20～60wt%.
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| CN102560704A (en) * | 2011-01-01 | 2012-07-11 | 苏州兆达特纤科技有限公司 | One-step preparation method of aramid fibers for optical cable |
| CN102400242B (en) * | 2011-11-21 | 2014-05-07 | 圣欧芳纶（江苏）股份有限公司 | Method for preparing colored poly-m-phenyleneisophthalamide (PMIA) fibers |
| CN102517677A (en) * | 2011-12-08 | 2012-06-27 | 烟台泰和新材料股份有限公司 | Method for continuous production of polyisophthaloyl metaphenylene diamine spinning stock solution |
| WO2013105949A1 (en) * | 2012-01-11 | 2013-07-18 | E. I. Du Pont De Nemours And Company | Process for preparing yarn derived from aramid copolymer fiber having low residual sulfur |
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| CN105970306A (en) * | 2016-07-15 | 2016-09-28 | 圣欧芳纶（淮安）有限公司 | Production process for optimizing fiber performance through heat treatment |
| CN107815741A (en) * | 2017-07-24 | 2018-03-20 | 烟台泰和新材料股份有限公司 | A kind of meta-aramid filament preparation process |
| CN110079884B (en) * | 2019-05-08 | 2021-11-02 | 东华大学 | Preparation method of polyimide fibrid with high specific surface area |
| CN110565197B (en) * | 2019-09-20 | 2021-06-22 | 株洲时代新材料科技股份有限公司 | Preparation method of heterocyclic aramid 1313 fiber |
| CN110965384B (en) * | 2019-11-04 | 2022-03-22 | 赣州龙邦材料科技有限公司 | Aramid 1313 high-electrical-strength insulating paper and preparation method thereof |
| CN112111804B (en) * | 2020-09-17 | 2021-08-31 | 株洲时代新材料科技股份有限公司 | Meta-aromatic polyamide fiber and preparation method thereof |
| CN113684549A (en) * | 2021-08-19 | 2021-11-23 | 株洲时代新材料科技股份有限公司 | Spinning process of polyamide fiber |
| CN117107373B (en) * | 2023-10-18 | 2024-03-12 | 泰和新材集团股份有限公司 | Spinning method of differential meta-aramid filaments |
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