CN107629206A - A kind of preparation method of Fanglun l414 fiber - Google Patents
A kind of preparation method of Fanglun l414 fiber Download PDFInfo
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- CN107629206A CN107629206A CN201710962241.8A CN201710962241A CN107629206A CN 107629206 A CN107629206 A CN 107629206A CN 201710962241 A CN201710962241 A CN 201710962241A CN 107629206 A CN107629206 A CN 107629206A
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Abstract
The invention discloses a kind of preparation method of Fanglun l414 fiber, belongs to aramid fiber production technical field of improvement.This method passes through the preparation of spinning solution, the spinning of polymer and post-processing step, simultaneously by adding organic bases acid absorbent, cosolvent and nitrogen, and the control of the parameter such as temperature, time, concentration, it is effectively increased polymer viscosity and yield, simultaneously, Fanglun l414 fiber quality is improved, to meet the market demand.
Description
Technical field
The present invention relates to a kind of preparation method of Fanglun l414 fiber, specifically, being related to a kind of improvement Fanglun l414 fiber
The preparation method of performance, belong to aramid fiber production technical field of improvement.
Background technology
Fanglun 1414, also known as Fanglun l414, PPTA fibers, prepare polymer used in this fiber
Monomer is the full contraposition Nomex that p-phenylenediamine forms with paraphthaloyl chloride condensation polymerization, and its molecular structure amide group exists
Phenyl ring aligns（Isosorbide-5-Nitrae）Position.Its polymer monomer is：
Its polymer is：
Fanglun l414 fibre density is low, specific strength is high, high temperature resistant, non-ignitable, not molten, creep resistance, stable performance, Fanglun l414 conduct
Special fibre and composite obtain a wide range of applications in fields such as space flight, aviation, traffic, communications.Nearly ten years, aramid fiber
1414 characteristic is progressively recognized, and demand is growing day by day.According to relevant information, will exceed to China's demand in 2005
More than 2kt/a, its main application and demand are：（1）Communication cable enhancing fiber about 200t/a；（2）Pressure storage tank increases
Strong fiber about 200t/a；（3）High intensity rope, cable about 200t/a；（4）Flak jackets, the helmet, knee-pad 200-300t/a；（5）High pressure-volume
Device reinforcing fiber about 200t/a；（6）Fanglun slurry cake（Instead of short fiber asbestos, rubber plastic enhancing fiber）It will exceed
300t/a；（7）Military special type aramid fiber 50t/a；（8）Colliery, harbour flame-retardant conveyor belt about 100-200t/a；（9）Sports goods
（Racing boat, yacht, racket etc.）About 200t/a；（10）Sedan limousine, mine load-carrying carriage wheel warp about 200k/a；In addition,
Special high temperature-resistant film, paper, tellite, low linear expansion coefficient material, aramid fiber/aluminum composite plate material etc. have preferably
Application prospect.Because the mechanical property of aramid fiber and heat resistance etc. are very excellent, there is excellent sexual valence lattice ratio plus it again,
The market competitiveness is powerful.
The content of the invention
Present invention address that the market demand, and propose a kind of preparation method of Fanglun l414 fiber.In Fanglun l414
In the preparation technology of fiber, by adding organic bases acid absorbent, cosolvent and nitrogen, polymer viscosity and production are effectively increased
Amount, meanwhile, improve Fanglun l414 fiber quality.
In order to realize above-mentioned technical purpose, following technical scheme is proposed：
A kind of preparation method of Fanglun l414 fiber, using p-phenylenediamine and paraphthaloyl chloride as reaction monomers, including following step
Suddenly：
A. the preparation of spinning solution
After weighing p-phenylenediamine, first p-phenylenediamine is dissolved in intensive polar solvent, under agitation add etc. the amount of material to benzene
Dimethyl chloride, meanwhile, cosolvent is additionally added, polymerisation 2-3h occurs under conditions of -3-4 DEG C, post-consumer polymer is through separating, washing
Wash and dry, obtain PPTA, i.e. spinning solution；
B. the spinning of polymer
The concentrated sulfuric acid is added in the spinning solution generated to step A, is dissolved, and is heated to 75-85 DEG C, spray is then directed at by conduit
Silk device；In spinning appts, pressing plate, spinning head spinneret；The fiber that spinning head sprays passes through air layer, and 8-12 DEG C successively
Coagulating bath, then exported by guide wheel, carry out 3-5 washing, after drying, at a temperature of 400-440 DEG C, protected with nitrogen, progress
Supplement heat treatment, after collected by bobbins, obtain as-spun fibre；
C. post-process
After the as-spun fibre that step B is generated carries out 2-3 washing, stretched in boiling water, after stretching, at 45-55 DEG C
Wash in hot water, be then dried, after drying, then stretched under the conditions of 250-300 DEG C, crimp or cut off, obtain PPTA fibers.
Further, the intensive polar solvent is HMPA/NMP systems or DMAc/HMPA systems.
Further, in the polymerization process of step A, addition liquid nitrogen improves synthetic system and changed as protective gas
Heat.
Further, in the polymerization process of step A, organic bases acid absorbent is added, is washed and is neutralized.
Further, the organic bases acid absorbent includes pyridine.
Further, the cosolvent includes the chloride of alkali metal or alkaline-earth metal.
Further, in step B, the concentrated sulfuric acid containing 22-26% in the coagulating bath.
After testing：PPTA polymerization gained viscosity is 22.1-23.7dL/g.
Using the technical program, the advantageous effects brought are：
1）In the preparation technology of Fanglun l414 fiber, by adding organic bases acid absorbent, cosolvent and nitrogen, Yi Jiwen
The control of the parameters such as degree, time, concentration, polymer viscosity and yield are effectively increased, meanwhile, Fanglun l414 fiber quality is improved,
To meet the market demand；
2）In the present invention, this polymerisation is exothermic reaction, but because activation energy is small, therefore reaction heat is little.To carry out reaction
Completely, it is necessary to remove the small molecule HCl of generation in time, add organic bases acid absorbent（Such as：Pyridine etc.）.With PPTA points
Subchain constantly increases, and its solubility in nmp solvent constantly reduces, and this is due to that PPTA molecules interchain forms hydrogen bond and cohesion
Can increase it is therefore, ultimately result in PPTA and separated out from solvent to precipitate and stop chain propagation reaction, do not reach required viscosity,
For this reason, it may be necessary to add cosolvent（The mainly chloride of alkali metal or alkaline-earth metal, such as LiCl, CaCl2）, increase PPTA dissolvings
Property.LiCl energy and HMPA（HMPA）, the amide type solvent such as NMP form polarity complex compound, this polarity complex compound is again
It can be acted on the ketonic oxygen on PPTA strands and amido hydrogen, so as to weaken the hydrogen bond of PPTA molecule interchains, improve PPTA
Dissolution degree in a solvent, be advantageous to the raising of polymer molecular weight；
3）In the present invention, because intensive polar solvent has very strong solvability, obtained PPTA inherent viscosities are relatively low,
Can be with LiCl, CaCl of amine formation complex compound further being added into the dicyandiamide solution based on HMPA2Deng when, the system exists
When PPTA reaches higher molecular weight, holding homogeneous system still is able to, PPTA polymerize the inherent viscosity reached in the dicyandiamide solution
For 22.1-23.7dL/g；
4）In the present invention, using low-temperature polycondensation method, and liquid nitrogen is added, synthetic system heat exchange, controls Fanglun l414 cellulose fibrils
Change degree.It is proposed addition liquid nitrogen with promote Fanglun l414 synthetic system exchange heat method, this law can obtain more low reaction temperatures and
The hot speed of more rapid traverse, be advantageous to suppress the sudden and violent poly- phenomenon at polycondensation reaction initial stage, analysis result is shown, the addition and phase transformation of liquid nitrogen are also
Reactant can be promoted to be vigorously mixed, the improvement of mass transfer effect, be also beneficial to significantly improve product quality；
5）In the present invention, Fanglun l414 fibrous fracture intensity（CN/dtex）>=21, elongation at break（%）≤ 3.7, regain
（%）≤ 6, density（g/cm3）≥1.53.
Embodiment
It is clearly and completely described below by the technical scheme in the embodiment of the present invention, it is clear that described reality
Apply the part of the embodiment that example is only the present invention, rather than whole embodiments.It is general based on the embodiment in the present invention, this area
All other embodiment that logical technical staff is obtained under the premise of creative work is not made, belong to what the present invention protected
Scope.
Embodiment 1
A kind of preparation method of Fanglun l414 fiber, using p-phenylenediamine and paraphthaloyl chloride as reaction monomers, including following step
Suddenly：
A. the preparation of spinning solution
After weighing p-phenylenediamine, first p-phenylenediamine is dissolved in intensive polar solvent, under agitation add etc. the amount of material to benzene
Dimethyl chloride, meanwhile, be additionally added cosolvent, under conditions of -3 DEG C occur polymerisation 2h, post-consumer polymer separating, washing and
Dry, obtain PPTA, i.e. spinning solution；
B. the spinning of polymer
The concentrated sulfuric acid is added in the spinning solution generated to step A, is dissolved, and is heated to 75 DEG C, spinneret is then directed at by conduit
Device；In spinning appts, pressing plate, spinning head spinneret；The fiber that spinning head sprays pass through air layer successively, and 8 DEG C are coagulated
Gu bath, then exported by guide wheel, 3 washings are carried out, after drying, at a temperature of 440 DEG C, is protected with nitrogen, carries out supplement heat treatment,
Collected afterwards by bobbins, obtain as-spun fibre；
C. post-process
After the as-spun fibre that step B is generated carries out 2 washings, stretched in boiling water, after stretching, in 45 DEG C of hot water
Washing, is then dried, and after drying, then is stretched under the conditions of 250 DEG C, crimps or cut off, obtain PPTA fibers.
Embodiment 2
A kind of preparation method of Fanglun l414 fiber, using p-phenylenediamine and paraphthaloyl chloride as reaction monomers, including following step
Suddenly：
A. the preparation of spinning solution
After weighing p-phenylenediamine, first p-phenylenediamine is dissolved in intensive polar solvent, under agitation add etc. the amount of material to benzene
Dimethyl chloride, meanwhile, be additionally added cosolvent, under conditions of 4 DEG C occur polymerisation 3h, post-consumer polymer separating, washing and
Dry, obtain PPTA, i.e. spinning solution；
B. the spinning of polymer
The concentrated sulfuric acid is added in the spinning solution generated to step A, is dissolved, and is heated to 85 DEG C, spinneret is then directed at by conduit
Device；In spinning appts, pressing plate, spinning head spinneret；The fiber that spinning head sprays pass through air layer successively, and 12 DEG C are coagulated
Gu bath, then exported by guide wheel, 5 washings are carried out, after drying, at a temperature of 400 DEG C, is protected with nitrogen, carries out supplement heat treatment,
Collected afterwards by bobbins, obtain as-spun fibre；
C. post-process
After the as-spun fibre that step B is generated carries out 3 washings, stretched in boiling water, after stretching, in 55 DEG C of hot water
Washing, is then dried, and after drying, then is stretched under the conditions of 300 DEG C, crimps or cut off, obtain PPTA fibers.
Embodiment 3
A kind of preparation method of Fanglun l414 fiber, using p-phenylenediamine and paraphthaloyl chloride as reaction monomers, including following step
Suddenly：
A. the preparation of spinning solution
After weighing p-phenylenediamine, first p-phenylenediamine is dissolved in intensive polar solvent, under agitation add etc. the amount of material to benzene
Dimethyl chloride, meanwhile, cosolvent is additionally added, polymerisation 2.5h, post-consumer polymer separating, washing occur under conditions of 0 DEG C
And dry, obtain PPTA, i.e. spinning solution；
B. the spinning of polymer
The concentrated sulfuric acid is added in the spinning solution generated to step A, is dissolved, and is heated to 80 DEG C, spinneret is then directed at by conduit
Device；In spinning appts, pressing plate, spinning head spinneret；The fiber that spinning head sprays pass through air layer successively, and 10 DEG C are coagulated
Gu bath, then exported by guide wheel, 4 washings are carried out, after drying, at a temperature of 430 DEG C, is protected with nitrogen, carries out supplement heat treatment,
Collected afterwards by bobbins, obtain as-spun fibre；
C. post-process
After the as-spun fibre that step B is generated carries out 2-3 washing, stretched in boiling water, after stretching, in 50 DEG C of hot water
Middle washing, is then dried, and after drying, then is stretched under the conditions of 280 DEG C, crimps or cut off, obtain PPTA fibers.
Embodiment 4
A kind of preparation method of Fanglun l414 fiber, using p-phenylenediamine and paraphthaloyl chloride as reaction monomers, including following step
Suddenly：
A. the preparation of spinning solution
After weighing p-phenylenediamine, first p-phenylenediamine is dissolved in intensive polar solvent, under agitation add etc. the amount of material to benzene
Dimethyl chloride, meanwhile, be additionally added cosolvent, under conditions of -3 DEG C occur polymerisation 3h, post-consumer polymer separating, washing and
Dry, obtain PPTA, i.e. spinning solution；
B. the spinning of polymer
The concentrated sulfuric acid is added in the spinning solution generated to step A, is dissolved, and is heated to 75 DEG C, spinneret is then directed at by conduit
Device；In spinning appts, pressing plate, spinning head spinneret；The fiber that spinning head sprays pass through air layer successively, and 12 DEG C are coagulated
Gu bath, then exported by guide wheel, 3 washings are carried out, after drying, at a temperature of 440 DEG C, is protected with nitrogen, carries out supplement heat treatment,
Collected afterwards by bobbins, obtain as-spun fibre；
C. post-process
After the as-spun fibre that step B is generated carries out 3 washings, stretched in boiling water, after stretching, in 45 DEG C of hot water
Washing, is then dried, and after drying, then is stretched under the conditions of 250 DEG C, crimps or cut off, obtain PPTA fibers.
Further, the intensive polar solvent is HMPA/NMP systems.
Further, in the polymerization process of step A, addition liquid nitrogen improves synthetic system and changed as protective gas
Heat.
Further, in the polymerization process of step A, organic bases acid absorbent is added, is washed and is neutralized.
Further, the organic bases acid absorbent is pyridine.
Further, the cosolvent is LiCl.
Further, in step B, 22% concentrated sulfuric acid is contained in the coagulating bath.
Embodiment 5
A kind of preparation method of Fanglun l414 fiber, using p-phenylenediamine and paraphthaloyl chloride as reaction monomers, including following step
Suddenly：
A. the preparation of spinning solution
After weighing p-phenylenediamine, first p-phenylenediamine is dissolved in intensive polar solvent, under agitation add etc. the amount of material to benzene
Dimethyl chloride, meanwhile, be additionally added cosolvent, under conditions of 4 DEG C occur polymerisation 2h, post-consumer polymer separating, washing and
Dry, obtain PPTA, i.e. spinning solution；
B. the spinning of polymer
The concentrated sulfuric acid is added in the spinning solution generated to step A, is dissolved, and is heated to 75 DEG C, spinneret is then directed at by conduit
Device；In spinning appts, pressing plate, spinning head spinneret；The fiber that spinning head sprays pass through air layer successively, and 12 DEG C are coagulated
Gu bath, then exported by guide wheel, 5 washings are carried out, after drying, at a temperature of 420 DEG C, is protected with nitrogen, carries out supplement heat treatment,
Collected afterwards by bobbins, obtain as-spun fibre；
C. post-process
After the as-spun fibre that step B is generated carries out 2 washings, stretched in boiling water, after stretching, in 45 DEG C of hot water
Washing, is then dried, and after drying, then is stretched under the conditions of 250-300 DEG C, crimps or cut off, obtain PPTA fibers.
Further, the intensive polar solvent is DMAc/HMPA systems.
Further, in the polymerization process of step A, addition liquid nitrogen improves synthetic system and changed as protective gas
Heat.
Further, in the polymerization process of step A, organic bases acid absorbent is added, is washed and is neutralized.
Further, the organic bases acid absorbent is pyridine.
Further, the cosolvent is CaCl2。
Further, in step B, the concentrated sulfuric acid containing 22-26% in the coagulating bath.
Embodiment 6
A kind of preparation method of Fanglun l414 fiber, using p-phenylenediamine and paraphthaloyl chloride as reaction monomers, including following step
Suddenly：
A. the preparation of spinning solution
After weighing p-phenylenediamine, first p-phenylenediamine is dissolved in intensive polar solvent, under agitation add etc. the amount of material to benzene
Dimethyl chloride, meanwhile, be additionally added cosolvent, under conditions of -1 DEG C occur polymerisation 2h, post-consumer polymer separating, washing and
Dry, obtain PPTA, i.e. spinning solution；
B. the spinning of polymer
The concentrated sulfuric acid is added in the spinning solution generated to step A, is dissolved, and is heated to 80 DEG C, spinneret is then directed at by conduit
Device；In spinning appts, pressing plate, spinning head spinneret；The fiber that spinning head sprays pass through air layer successively, and 10 DEG C are coagulated
Gu bath, then exported by guide wheel, 4 washings are carried out, after drying, at a temperature of 430 DEG C, is protected with nitrogen, carries out supplement heat treatment,
Collected afterwards by bobbins, obtain as-spun fibre；
C. post-process
After the as-spun fibre that step B is generated carries out 3 washings, stretched in boiling water, after stretching, in 50 DEG C of hot water
Washing, is then dried, and after drying, then is stretched under the conditions of 280 DEG C, crimps or cut off, obtain PPTA fibers.
Further, the intensive polar solvent is HMPA/NMP systems.
Further, in the polymerization process of step A, addition liquid nitrogen improves synthetic system and changed as protective gas
Heat.
Further, in the polymerization process of step A, organic bases acid absorbent is added, is washed and is neutralized.
Further, the organic bases acid absorbent is pyridine.
Further, the cosolvent is LiCl.
Further, in step B, 24% concentrated sulfuric acid is contained in the coagulating bath.
Claims (7)
1. a kind of preparation method of Fanglun l414 fiber, using p-phenylenediamine and paraphthaloyl chloride as reaction monomers, its feature exists
In：Comprise the following steps：
A. the preparation of spinning solution
After weighing p-phenylenediamine, first p-phenylenediamine is dissolved in intensive polar solvent, under agitation add etc. the amount of material to benzene
Dimethyl chloride, meanwhile, cosolvent is additionally added, polymerisation 2-3h occurs under conditions of -3-4 DEG C, post-consumer polymer is through separating, washing
Wash and dry, obtain PPTA, i.e. spinning solution；
B. the spinning of polymer
The concentrated sulfuric acid is added in the spinning solution generated to step A, is dissolved, and is heated to 75-85 DEG C, spray is then directed at by conduit
Silk device；In spinning appts, pressing plate, spinning head spinneret；The fiber that spinning head sprays passes through air layer, and 8-12 DEG C successively
Coagulating bath, then exported by guide wheel, carry out 3-5 washing, after drying, at a temperature of 400-440 DEG C, protected with nitrogen, progress
Supplement heat treatment, after collected by bobbins, obtain as-spun fibre；
C. post-process
After the as-spun fibre that step B is generated carries out 2-3 washing, stretched in boiling water, after stretching, at 45-55 DEG C
Wash in hot water, be then dried, after drying, then stretched under the conditions of 250-300 DEG C, crimp or cut off, obtain PPTA fibers.
2. the preparation method of Fanglun l414 fiber according to claim 1, it is characterised in that：The intensive polar solvent is
HMPA/NMP systems or DMAc/HMPA systems.
3. the preparation method of Fanglun l414 fiber according to claim 1, it is characterised in that：In the polymerisation of step A
During, addition liquid nitrogen is as protective gas.
4. the preparation method of Fanglun l414 fiber according to claim 1, it is characterised in that：In the polymerisation of step A
During, organic bases acid absorbent is added, is washed and is neutralized.
5. the preparation method of Fanglun l414 fiber according to claim 4, it is characterised in that：The organic bases acid absorbs
Agent includes pyridine.
6. the preparation method of Fanglun l414 fiber according to claim 1, it is characterised in that：The cosolvent includes alkali gold
The chloride of category or alkaline-earth metal.
7. the preparation method of Fanglun l414 fiber according to claim 1, it is characterised in that：In step B, the solidification
The concentrated sulfuric acid containing 22-26% in bath.
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Cited By (3)
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| CN109705529A (en) * | 2018-12-26 | 2019-05-03 | 蓝星（成都）新材料有限公司 | A kind of preparation method based on Fanglun l414 fibrous composite |
| CN110029405A (en) * | 2019-04-08 | 2019-07-19 | 东华大学 | A kind of preparation method of high uniformity p-aramid fiber |
| CN114959935A (en) * | 2022-07-07 | 2022-08-30 | 北京珺政慧通科技有限公司 | Modified para-aramid fiber and preparation method thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109705529A (en) * | 2018-12-26 | 2019-05-03 | 蓝星（成都）新材料有限公司 | A kind of preparation method based on Fanglun l414 fibrous composite |
| CN109705529B (en) * | 2018-12-26 | 2021-04-27 | 蓝星（成都）新材料有限公司 | Preparation method of aramid fiber 1414 fiber-based composite material |
| CN110029405A (en) * | 2019-04-08 | 2019-07-19 | 东华大学 | A kind of preparation method of high uniformity p-aramid fiber |
| CN114959935A (en) * | 2022-07-07 | 2022-08-30 | 北京珺政慧通科技有限公司 | Modified para-aramid fiber and preparation method thereof |
| CN114959935B (en) * | 2022-07-07 | 2024-02-09 | 北京珺政慧通科技有限公司 | Modified para-aramid fiber and preparation method thereof |
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