CN104233499A - Preparation method of aromatic polyarmide fiber containing heterlcyclic rings - Google Patents
Preparation method of aromatic polyarmide fiber containing heterlcyclic rings Download PDFInfo
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- CN104233499A CN104233499A CN201310239246.XA CN201310239246A CN104233499A CN 104233499 A CN104233499 A CN 104233499A CN 201310239246 A CN201310239246 A CN 201310239246A CN 104233499 A CN104233499 A CN 104233499A
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Abstract
The invention provides a preparation method of aromatic polyarmide fiber containing heterlcyclic rings. The preparation method is characterized by comprising the specific steps of (1) extruding filtered and defoamed aromatic polyarmide solution containing the heterlcyclic rings from spinneret orifices under the nitrogen pressure of 0.2-0.5MPa, entering a DMAc aqueous solution after passing through air gaps, and curing to obtain nascent fiber; (2) carrying out wet drawing on the nascent fiber obtained in the step (1) in the DMAc aqueous solution, washing with water, drying, and carrying out hot drawing, so as to obtain the aromatic polyarmide fiber containing the heterlcyclic rings. The preparation method provided by the invention has the advantages that the high-performance aromatic polyarmide fiber with the strength being more than 25.0cN/dtex and the tensile modulus being more than 700.0cN/dtex can be obtained, and simultaneously the obtained fiber is smooth in surface and high in section roundness.
Description
Technical field
The present invention relates to aromatic polyamide fibre and manufacture method thereof, particularly a kind of preparation method of the aromatic polyamide fibre containing heterocycle of high-strength and high-modulus.
Background technology
Heteroaromatic polyamide fiber is a kind of high strength, high-modulus, resistant to elevated temperatures organic fiber, decomposition temperature reaches 560 DEG C, intensity containing the aromatic polyamide fibre of heterocycle high (higher than common aromatic polyamide fibre 20 ~ 40%), heat resistance good (shrinking hardly at 400 ~ 450 DEG C), fire resistance good (limited oxygen index 37 ~ 43%).In high-end applications field, can as high-speed aircraft machine engine, bulletproof armour etc.; Can be widely used equally in national economy field, such as can increase material as structure containing the aromatic polyamide fibre of heterocycle and exotic material can play its speciality at civil area.
The polymer architecture of heteroaromatic polyamide fiber is:
Be with p-phenylenediamine (PPD) (PPD), 5 (6)-amino-2-(4-aminophenyl) benzimidazole (DAPBI) and paraphthaloyl chloride (TPC) three kinds of monomers, carry out low temperature solution polymerization and obtain.
CN101921395 discloses a kind of method preparing heteroaromatic polyamide fiber, adopt wet spinning process to make fiber, polymer solution sprays into coagulation forming in coagulating bath by spinneret cap and obtains as-spun fibre, as-spun fibre carries out plastic elongation with the draw ratio of 50-150% again in plasticization drawing bath, then through washing, oils, dry, after heat treatment and surface treatment, be wound into cylinder, obtain golden yellow heterocycle aramid fiber.
The defect of said method is adopted to be in the process of setting of wet spinning, spinning solution thread directly enters coagulating bath through spinneret orifice, because the double diffusion process between solvent and non-solvent unavoidably makes as-spun fibre have skin-core structure, inside can produce cavity, this microdefect can not be eliminated completely in the follow-up process such as wet stretching, drying, hot-stretch, which prevent the further raising of heteroaromatic polyamide fiber mechanical property.Simultaneously when wet spinning, spinning speed is low, and concentration of dope is little, which dictates that low production efficiency, no matter and be all very little by improving proposition speed or improving the space that spinning solution enhances productivity.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of high-performance heterocyclic aromatic polyamide fibre, the employing of the method simultaneously can also improve the concentration of spinning speed and spinning solution, thus significantly improve the preparation efficiency of this fiber, fiber prepared by the present invention has smooth surface, the feature that cross section roundness is high.
In order to solve the problems of the technologies described above, the invention provides a kind of preparation method of the aromatic polyamide fibre containing heterocycle, it is characterized in that, concrete steps comprise:
The first step: by through to filter and the aromatic polyamide solution of heterocycle of containing of deaeration is extruded from spinneret orifice under the nitrogen pressure of 0.2-0.5MPa, enter again in the DMAc aqueous solution to solidify behind air gap to obtain as-spun fibre;
Second step: the as-spun fibre of first step gained is carried out in the aqueous solution of DMAc wet stretching, after washing and drying, carry out hot-stretch, obtain the aromatic polyamide fibre containing heterocycle.
Preferably, the chemical constitution of the aromatic polyamide containing heterocycle in the described first step comprises the first repetitive and the second repetitive, and its structural formula is as follows respectively:
First repetitive:
Second repetitive:
Wherein, the content of the second repetitive is more than 30 % by mole, and is greater than 5.0dL/g containing the reduced inherent viscosity of the aromatic polyamide of heterocycle.
Preferably, the Zero shear viscosity of aromatic polyamide solution at 50 DEG C containing heterocycle in the described first step is 300-500Pas.
Preferably, the length of the air gap in the described first step is 5-16mm.
Preferably, the temperature of the DMAc aqueous solution in the described first step is 10-50 DEG C, and concentration is 10-50wt%.
Preferably, the temperature of the DMAc aqueous solution in described second step is 10-50 DEG C, and concentration is 0.5-30wt%, and the wet multiple stretched is 1.5-2.5.
Preferably, the temperature of described hot-stretching step is 350-500 DEG C, take nitrogen as protective gas, and the multiple of hot-stretch is 1.0-1.5.
High polymer spinning slurry is a kind of viscoelastic body, not only toughness but also flexible, and a kind of outstanding behaviours of this characteristic in process is exactly die orifice extrusion swelling, and along with the increase of polymer molecular weight and concentration, the reduction of temperature, this phenomenon is more obvious.In wet spinning process, stoste thread goes out spinneret orifice and just directly enters coagulating bath later, and there will be obvious die orifice extrusion swelling phenomenon, cause larger shower nozzle negative stretch, spinning speed can only maintain lower level.Simultaneously in order to reduce the extrusion swelling of die orifice, the concentration of polymer slurries can not be too high, and this directly can have influence on production efficiency.And adopt method of the present invention, from spinneret orifice extrude containing the aromatic polyamide strand of heterocycle first after one section of air layer, deformation modulus less before utilizing grout cures, make it that huge elongation deformation occur, make strand can abundant orientation fully fixing after entering coagulating bath, effectively improve spinning speed, concentration can be adopted higher simultaneously, the spinning solution that viscosity is larger, improves spinning efficiency.
It is more than 25.0cN/dtex that the present invention can obtain intensity, and stretch modulus is the high-performance aromatic polyamide fibre of more than 700.0cN/dtex, and the fiber surface simultaneously obtained is smooth, and cross section roundness is high.
Detailed description of the invention
In the methods of the invention, aromatic polyamide solution containing heterocycle adopts the preparation of low temperature solution polymerization method, concrete steps are: be dissolved in by lithium chloride and be made in mixed solvent in the DMAc of the drying of new distillation, refining p-phenylenediamine (PPD) (PPDA) and 5 (6)-amino-2-(4-aminophenyl) benzimidazole (DAPBI) are dissolved in wherein at-10 DEG C, then add refining m-phthaloyl chloride (TPC) and carry out precondensation, keep system temperature lower than 10 DEG C, react after 15-30 minute, system is warming up to 60-80 DEG C, reaction 1-2h obtains the polymer solution of pale yellow transparent.
The above-mentioned aromatic polyamide solution containing heterocycle is through filtration, deaeration and temperature adjustment.Slurries extrude before temperature depend on the extruded velocity of the reduced inherent viscosity of polymer, the concentration orifice diameter of solution and solution.In order to obtain the final fiber of excellent performance and ensure the stability of spinning process, the Zero shear viscosity at polymer solution 50 DEG C controls at 300-500Pas.Then this spinning solution under the pressure of 0.2-0.5MPa after measuring pump metering is extruded downwards from spinneret orifice first through one section of air layer, then enter solidification forming in coagulating bath.The length of air layer controls at 5-20mm according to the difference of polymer solution.The aqueous solution consisting of DMAc of coagulating bath used, concentration is 10-50%, 10-50 DEG C.The concentration of coagulating bath and temperature will be worked in coordination to ensure that strand solidifies the mitigation of double diffusion process but is unlikely to solidify and thoroughly do not produced doubling.
The aromatic polyamide strand containing heterocycle of solidification forming enters wet stretch bath and carries out 1.5-2.5 stretching doubly, suitably to improve the mechanical property of as-spun fibre to carry out follow-up washing and oven dry smoothly, avoids fracture of wire.Go out in the as-spun fibre of coagulating bath and contain more solvent DMAc, due to plasticization, make fiber can when stretching lower than when vitrification point.Wet stretch bath is the aqueous solution of DMAc, and concentration is 0.5-30wt%, and temperature is 10-50 DEG C.
DMAc content in the fiber of wet stretch bath reduces further, and through further washing is to wash away solvent DMAc and cosolvent lithium chloride to greatest extent, the fiber cleaned up enters xeothermic draw stage after being dried to over dry at 110 DEG C.The temperature of hot-stretch is preferably 350-550 DEG C, and more preferably at 400-500 DEG C, temperature is too high, and the large molecule of fiber can partly decompose, and makes the drawn yarn mechanical property that obtains undesirable.And temperature is lower than 350 DEG C, because spinning speed of the present invention is higher, if heat pipe temperature is on the low side, then polymer macromolecule chain has little time to carry out resetting to improve degree of crystallinity and the degree of orientation under external temperature field and the field of force, then cannot obtain the drawn yarn of excellent in mechanical performance.Because the temperature of xeothermic stretching is more than the vitrification point of the aromatic polyamide containing heterocycle, stretching 1.0-1.5 doubly just can make the structure of fiber be optimized, and performance is significantly improved, and draw ratio is greater than 1.5 times, easily produces fracture of wire.
Be more than 25.00cN/dtex according to the fracture strength of aromatic polyamide fibre containing heterocycle prepared by said method, elastic modelling quantity is more than 700.00cN/dtex.
For making the present invention become apparent, hereby with preferred embodiment, and be described in detail below." part " of the present invention, without specified otherwise, all refers to weight portion.
Embodiment 1:
2.86 parts of lithium chlorides are dissolved in the DMAc of the drying of the new distillation of 86.50 parts and are made into mixed solvent, 1 part of refining PPDA and 2.08 part DAPBI is dissolved in mixed solvent at-10 DEG C, then add 3.77 parts of refining TPC and carry out precondensation, keep system temperature lower than 10 DEG C, react after 30 minutes, system is warming up to 80 DEG C, and reaction 2h obtains the aromatic polyamide solution containing heterocycle of pale yellow transparent.The chemical constitution of the described aromatic polyamide containing heterocycle comprises the first repetitive and the second repetitive, and its structural formula is as follows respectively:
First repetitive:
Second repetitive:
Wherein, the content of the second repetitive is 36mol%, and is 5.5dL/g containing the reduced inherent viscosity of the aromatic polyamide of heterocycle, and solution concentration is 6.0%, and the Zero shear viscosity of aromatic polyamide solution at 50 DEG C containing heterocycle is 300-500Pas.
Aromatic polyamide solution containing heterocycle obtains spinning slurry through deaeration and filtration, by this slurries temperature adjustment to 90 DEG C, extrude from spinneret orifice under the nitrogen pressure of 0.5MPa behind the air gap that 10mm is long, to enter that concentration is 20%, temperature is solidify the DMAc aqueous solution of 30 DEG C to obtain as-spun fibre again; Spinneret cap has 100 spinneret orifices, and orifice diameter is 0.25mm.Jet stretch is 1.5 times.It is 30 DEG C that coagulating bath as-spun fibre out enters temperature; concentration is carry out wet stretching in the DMAc aqueous solution of 40%; wet draw ratio is 2.0 times; drawn yarn is after washing and drying; the hot case entering 450 DEG C carries out xeothermic stretching, take nitrogen as protective gas, and draw ratio is 1.2 times; obtain the aromatic polyamide fibre containing heterocycle, finally with the rolling of 30.0m/min speed.The aromatic polyamide fibre fracture strength containing heterocycle prepared is like this 30.2cN/dtex, and extension at break is 3.1% elastic modelling quantity is 763.5cN/dtex.
Embodiment 2:
Containing the aromatic polyamide solution of heterocycle with embodiment 1.
Aromatic polyamide solution containing heterocycle obtains spinning slurry through deaeration and filtration.By this slurries temperature adjustment to 90 DEG C, entering concentration again extrude the air gap grown through 5mm from spinneret orifice under the nitrogen pressure of 0.5MPa after is 20%, and temperature is solidify in the DMAc aqueous solution of 30 DEG C to obtain as-spun fibre.Spinneret cap has 100 spinneret orifices, and orifice diameter is 0.25mm.Jet stretch is 1.5 times.It is 30 DEG C that coagulating bath as-spun fibre out enters temperature; concentration is carry out wet stretching in the DMAc aqueous solution of 40%; wet draw ratio is 2.0 times; drawn yarn is after washing and drying; the hot case entering 450 DEG C carries out xeothermic stretching, take nitrogen as protective gas, and draw ratio is 1.2 times; obtain the aromatic polyamide fibre containing heterocycle, finally with the rolling of 30.0m/min speed.The aromatic polyamide fibre fracture strength containing heterocycle prepared is like this 27.8cN/dtex, and extension at break is 3.3% elastic modelling quantity is 715.5cN/dtex.
Embodiment 3:
Containing the aromatic polyamide solution of heterocycle with embodiment 1.
Aromatic polyamide solution containing heterocycle obtains spinning slurry through deaeration and filtration, by this slurries temperature adjustment to 90 DEG C, extrude from spinneret orifice under the nitrogen pressure of 0.5MPa behind the air gap that 16mm is long, to enter that concentration is 20%, temperature is solidify the DMAc aqueous solution of 30 DEG C to obtain as-spun fibre again; Spinneret cap has 100 spinneret orifices, and orifice diameter is 0.25mm.Jet stretch is 2.0 times.It is 30 DEG C that coagulating bath as-spun fibre out enters temperature; concentration is carry out wet stretching in the DMAc aqueous solution of 40%; wet draw ratio is 1.2 times; drawn yarn is after washing and drying; the hot case entering 450 DEG C carries out xeothermic stretching, take nitrogen as protective gas, and draw ratio is 1.2 times; obtain the aromatic polyamide fibre containing heterocycle, finally with the rolling of 40.0m/min speed.The aromatic polyamide fibre fracture strength containing heterocycle prepared is like this 31.5cN/dtex, and extension at break is 3.3% elastic modelling quantity is 815.5cN/dtex.
Embodiment 4:
Containing the aromatic polyamide solution of heterocycle with embodiment 1.
Aromatic polyamide solution containing heterocycle obtains spinning slurry through deaeration and filtration.This slurries temperature adjustment to 90 DEG C, entering DMAc concentration from the spinneret orifice air layer extruded through 18mm is 20%, and temperature is in the coagulating bath of 30 DEG C.Because air layer is too large, spinning slurry is in the easily cross flow of spinneret cap surface, and spinning situation is unstable.
Comparative example 1:
2.86 parts of lithium chlorides are dissolved in the DMAc of the drying of the new distillation of 133 parts and are made into mixed solvent, 1 part of refining PPDA and 2.08 part DAPBI is dissolved in wherein at-10 DEG C, then add 3.77 parts of refining TPC and carry out precondensation, keep system temperature lower than 10 DEG C, react after 30 minutes, system is warming up to 80 DEG C, and reaction 2h obtains the aromatic polyamide solution containing heterocycle of pale yellow transparent.The reduced inherent viscosity measuring polymer is 5.41dL/g, and solution concentration is 4.0%.Solution obtains spinning slurry through deaeration and filtration.This slurries temperature adjustment to 60 DEG C, being directly expressed into concentration from spinneret orifice is 20%, and temperature is in the DMAc aqueous solution of 30 DEG C.Spinneret cap has 100 spinneret orifices, and orifice diameter is 0.15mm.Shower nozzle negative stretch is-30% (namely jet stretch is 0.7).It is 30 DEG C that coagulating bath strand out enters temperature; concentration is stretch in the DMAc aqueous solution of 40%; draw ratio is 2.0 times; drawn yarn is through washing and drying; the hot case entering 400 DEG C carries out xeothermic stretching; take nitrogen as protective gas, draw ratio is 1.2 times, finally with the rolling of 20.0m/min speed.
The aromatic polyamide fibre fracture strength containing heterocycle prepared is like this 24.80cN/dtex, and extension at break is 3.4%, and elastic modelling quantity is 626.5cN/dtex.
Comparative example 2:
2.86 parts of lithium chlorides are dissolved in the DMAc of the drying of the new distillation of 133 parts and are made into mixed solvent, 1 part of refining PPDA and 2.08 part DAPBI is dissolved in wherein at-10 DEG C, then add 3.77 parts of refining TPC and carry out precondensation, keep system temperature lower than 10 DEG C, react after 30 minutes, system is warming up to 80 DEG C, and reaction 2h obtains the aromatic polyamide solution containing heterocycle of pale yellow transparent.The reduced inherent viscosity measuring polymer is 5.41dL/g, and solution concentration is 4.0%.Solution obtains spinning slurry through deaeration and filtration.This slurries temperature adjustment to 60 DEG C, extrudes from spinneret orifice behind the air gap that 4mm is long, to enter that concentration is 20%, temperature is solidify the DMAc aqueous solution of 30 DEG C to obtain as-spun fibre again under 0.5MPa nitrogen pressure; Spinneret cap has 100 spinneret orifices, and orifice diameter is 0.25mm.Jet stretch is 2.0 times.Due to coagulating bath liquid fluctuating, spinning curing condition is unstable, and spinning is intermittent, cannot obtain normal fiber.
Can see from comparative example 1, owing to adopting the spinning process be directly immersed in by spinnerets in coagulating bath, in process of setting, spinning solution thread directly enters coagulating bath through spinneret orifice, because the double diffusion process between solvent and non-solvent unavoidably makes as-spun fibre have skin-core structure, inside can produce cavity, this microdefect is in follow-up wet stretching, dry, can not eliminate completely in the processes such as hot-stretch, which prevent the raising of heteroaromatic polyamide fiber mechanical property, simultaneously due to the resistance of coagulating bath, make spinning speed low (only having the 1/2-2/3 of embodiment), this just determines low production efficiency, as can be seen from comparative example 2, when the employing air gap spinning process adopting comparative example identical, if gap is too small, due to the fluctuation of coagulating bath liquid level, unstable spinning situation can be produced, make technical process unstable.
Claims (7)
1., containing a preparation method for the aromatic polyamide fibre of heterocycle, it is characterized in that, concrete steps comprise:
The first step: by through to filter and the aromatic polyamide solution of heterocycle of containing of deaeration is extruded from spinneret orifice under the nitrogen pressure of 0.2-0.5MPa, enter again in the DMAc aqueous solution to solidify behind air gap to obtain as-spun fibre;
Second step: the as-spun fibre of first step gained is carried out in the aqueous solution of DMAc wet stretching, after washing and drying, carry out hot-stretch, obtain the aromatic polyamide fibre containing heterocycle.
2. the preparation method of the aromatic polyamide fibre containing heterocycle as claimed in claim 1, is characterized in that, the chemical constitution of the aromatic polyamide containing heterocycle in the described first step comprises the first repetitive and the second repetitive, and its structural formula is as follows respectively:
First repetitive:
Second repetitive:
Wherein, the content of the second repetitive is more than 30 % by mole, and is greater than 5.0dL/g containing the reduced inherent viscosity of the aromatic polyamide of heterocycle.
3. the preparation method of the aromatic polyamide fibre containing heterocycle as claimed in claim 1, is characterized in that, the Zero shear viscosity of aromatic polyamide solution at 50 DEG C containing heterocycle in the described first step is 300-500Pas.
4. the preparation method of the aromatic polyamide fibre containing heterocycle as claimed in claim 1, it is characterized in that, the length of the air gap in the described first step is 5-16mm.
5. the preparation method of the aromatic polyamide fibre containing heterocycle as claimed in claim 1, it is characterized in that, the temperature of the DMAc aqueous solution in the described first step is 10-50 DEG C, and concentration is 10-50wt%.
6. the preparation method of the aromatic polyamide fibre containing heterocycle as claimed in claim 1, it is characterized in that, the temperature of the DMAc aqueous solution in described second step is 10-50 DEG C, and concentration is 0.5-30wt%, and the wet multiple stretched is 1.5-2.5.
7. the preparation method of the aromatic polyamide fibre containing heterocycle as claimed in claim 1, it is characterized in that, the temperature of described hot-stretching step is 350-500 DEG C, take nitrogen as protective gas, and the multiple of hot-stretch is 1.0-1.5.
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| CN112575395A (en) * | 2020-12-04 | 2021-03-30 | 四川辉腾科技股份有限公司 | Heterocyclic aramid fiber solidification forming device and process thereof |
| CN112812373A (en) * | 2021-01-13 | 2021-05-18 | 江西龙泰新材料股份有限公司 | High-strength conductive aramid fiber core material and forming process thereof |
| CN113668091A (en) * | 2020-05-13 | 2021-11-19 | 中蓝晨光化工研究设计院有限公司 | High-strength high-elongation heterocyclic aromatic polyamide fiber and preparation process thereof |
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| CN112812373A (en) * | 2021-01-13 | 2021-05-18 | 江西龙泰新材料股份有限公司 | High-strength conductive aramid fiber core material and forming process thereof |
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