CN100395381C - Method of continuously preparing poly terephthaloyl-p-phenylene diamine fibre - Google Patents
Method of continuously preparing poly terephthaloyl-p-phenylene diamine fibre Download PDFInfo
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- CN100395381C CN100395381C CNB2005100257083A CN200510025708A CN100395381C CN 100395381 C CN100395381 C CN 100395381C CN B2005100257083 A CNB2005100257083 A CN B2005100257083A CN 200510025708 A CN200510025708 A CN 200510025708A CN 100395381 C CN100395381 C CN 100395381C
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Abstract
The present invention discloses a method for continuously preparing poly(p-phenylene terephthalamide) fibers. The method comprises the procedures: 1. concentrated sulfuric acid with the concentration of 98 to 100% and dry poly(p-phenylene terephthalamide) resin (PPTA) with the logarithmic viscosity of 4.0 to 8.5 dl/g are continuously added in a double-screw extruder 1, wherein the weight percentage of PPTA is from 14 to 24%, and mixing temperature is from 50 to 100 DEG C: 2. the components continuously enter a double-screw extruder 2 after being thoroughly mixed, temperature is regulated to 50 to 100 DGE C, stay time is from 10 to 60 minutes, and the components are extruded after thorough mixing, temperature regulation and deaeration; 3. poly(p-phenylene terephthalamide) fibers are obtained through the normal procedures of spray, wet spinning, etc. after spinning solution is metered and filtered. The present invention has the advantages of short time for material mixing, temperature regulation and deaeration, high mixing uniformity of materials, reaction of continuous and stable spinning in short time and improved production efficiency.
Description
Technical field
The present invention relates to a kind of fiber preparation method, particularly relate to a kind of method of continuously preparing poly poly P phenylene diamine terephthalamide fiber.
Background technology
As everyone knows, the Fanglun 1414 is a kind of typical aromatic polyamide fibre, be called Fanglun l414 or PPTA fiber again, it has high-strength, Gao Mo, excellent properties such as high temperature resistant, it is a class tec fiber with the fastest developing speed in the fibrous material in recent years, mainly use on fabrics for industrial use, particularly many product requirement lightweights, high performance occasion can only be used PPTA (PPTA) fiber.
Last century, early seventies was that PPTA/H has at first invented in E.I.Du Pont Company by U.S.A
2SO
4Liquid crystal solution is done the method for spray-wet spinning, has made the PPTA fiber of this high-strength and high-modulus, but still exists PPTA/H so far
2SO
4The stirring of the preparation process medium-high viscosity solution of spinning liquid crystal solution and deaeration difficult technologies problem, generally, the PPTA resin dissolves under 80～90 ℃ of conditions in 99～100% sulfuric acid, needs 3 hours at least, and PPTA/H
2SO
4The deaeration of spinning liquid crystal solution often needs the longer time, reaches tens hours to tens hours, and not only bad for the industrial production of serialization, and PPTA degrading in dissolving and the deaeration process for a long time easily, thereby influences the intensity of PPTA fiber.
A kind of semicontinuous Fanglun 1414's of preparation method is disclosed in the Chinese invention patent 200310109240, after mixing in PPTA resin and the concentrated sulfuric acid adding mixing drum, carry out double screw extruder, solve the problem of the long and spinning solution deaeration difficulty of the dissolution time of PPTA resin in the concentrated sulfuric acid, but for industrialization is produced, also had the problem that stirs difficulty and be difficult for mixing in the mixed process.
Summary of the invention
Technical problem to be solved by this invention is: a kind of method of continuously preparing poly poly P phenylene diamine terephthalamide fiber is provided, to remedy the deficiencies in the prior art and defective, meets the needs of production.
In order to solve the problems of the technologies described above the technical solution adopted in the present invention be: a kind of method of continuously preparing poly poly P phenylene diamine terephthalamide fiber may further comprise the steps:
(1) be 98～100% the concentrated sulfuric acid with concentration and dry logarithmic viscosity number is that the PPTA resin of 4.0～8.5dl/g adds first double screw extruder continuously, wherein the percentage by weight of PPTA resin is 14～24%, mixing temperature is 50～100 ℃, the time of staying is 1～10 minute, and the shear rate of first double screw extruder is 300～2000s
-1
(2) above material enters second double screw extruder continuously after fully mixing, and regulating temperature is 50～100 ℃, and the time of staying is 10～60 minutes, extruding spinning solution after fully mixing, temperature adjustment, the deaeration;
(3) after spinning solution metering, the filtration, obtain poly-paraphenylene terephthalamide's diphenylamines fiber through doing conventional steps such as spray-wet spinning.
As optimized technical scheme: the concentrated sulfuric acid adopts liquid meter charging system weighing, and the PPTA resin adopts the metering of high accuracy weight-loss type continuous metering electronic scale.
The screw diameter of described first double screw extruder is 25～90mm, and draw ratio is 8～20, can be in the same way, also incorgruous rotation, and rotating speed is 150～300rpm.
The screw diameter of described second double screw extruder is 25～145mm, and draw ratio is 30～60, and screw speed is 10～200rpm, and the time of staying of material in this screw extruder is 10～60 minutes.
Two screw rods of described first double screw extruder are made up of to the deep trouth threaded block multistage bull or single head just (or anti-), on the forward screw thread, also have the reverse shallow thread groove of bull, therefore material has strong back mixing effect therein, automatic cleaning action is good and shear rate is high, can reach 300～2000s
-1, material can reach microcosmic at short notice to be mixed, thereby can improve PPTA and H
2SO
4Mixing uniformity.
The first half of two intermeshing screw rods in described second double screw extruder, from the screw rod total length that enters the mouth 30～80% part, kneading piece and a spot of reverse thread cover by various forward thread bush, different rotation directions are formed, wherein, the total length of kneading piece accounts for more than 30% of this partial-length.
The latter half of two intermeshing screw rods is made up of the thread bush that reduces gradually along Way out pitch in described second double screw extruder.
The invention has the beneficial effects as follows: mixing of materials, temperature adjustment, deaeration time weak point, the mixture homogeneity height of material can be realized continuous, stable spinning in the short time, has improved production efficiency.
The specific embodiment
Below in conjunction with specific embodiment the present invention is further elaborated.
Embodiment 1
Adopting liquid meter charging system and high accuracy weight-loss type continuous metering electronic scale that 100% concentrated sulfuric acid and PPTA (PPTA) powder are added diameter with the speed of 71.08g/min and 16.6g/min respectively is Φ 40, draw ratio is 15, incorgruous rotation, rotating speed is in first double screw extruder of 200rpm, after fully mixing, entering diameter continuously is 55mm, draw ratio is 60, rotating speed is in second double screw extruder of 40rpm, the extruder temperature of controlling first double screw extruder and second double screw extruder is 85 ℃, extrude abundant mixing continuously, adjustment is good, bubble takes off most spinning solution, through metering, after the filtration, send into spinning head, the spinneret cap specification is Φ 0.06 * 300 hole, through the air gap of 5cm layer, enter the coagulating bath spin duct, coagulation bath temperature is 5 ℃, and spinning speed is 120m/min, 6 times of jet stretches, spun tow is after the washing neutralization, send into annealing device, 400 ℃ of 10 seconds of following heat treatment, reoiling is wound into tube, measure according to GB, the intensity of gained PPTA (PPTA) fiber is 2.71GPa, and initial modulus is 182GPa, and extension at break is 1.41%.
Embodiment 2
Adopting liquid meter charging system and high accuracy weight-loss type continuous metering electronic scale that 99% concentrated sulfuric acid and PPTA (PPTA) powder are added diameter with the speed of 71.08g/min and 16.6g/min respectively is Φ 25, draw ratio is 8, rotation in the same way, rotating speed is in first double screw extruder of 150rpm, after fully mixing, entering diameter continuously is 25mm, draw ratio is 30, rotating speed is in second double screw extruder of 200rpm, the extruder temperature of controlling first double screw extruder and second double screw extruder is 50 ℃, extrude abundant mixing continuously, adjustment is good, bubble takes off most spinning solution, through metering, after the filtration, send into spinning head, the spinneret cap specification is Φ 0.06 * 300 hole, through the air gap of 5cm layer, enter the coagulating bath spin duct, coagulation bath temperature is 5 ℃, and spinning speed is 120m/min, 6 times of jet stretches, spun tow is after the washing neutralization, send into annealing device, 400 ℃ of 10 seconds of following heat treatment, reoiling is wound into tube, measure according to GB, the intensity of gained PPTA (PPTA) fiber is 2.75GPa, and initial modulus is 185GPa, and extension at break is 1.41%.
Embodiment 3
Adopting liquid meter charging system and high accuracy weight-loss type continuous metering electronic scale that 98% concentrated sulfuric acid and PPTA (PPTA) powder are added diameter with the speed of 70.08g/min and 20.6g/min respectively is Φ 90, draw ratio is 20, incorgruous rotation, rotating speed is in first double screw extruder of 300rpm, after fully mixing, entering diameter continuously is 145mm, draw ratio is 60, rotating speed is in second double screw extruder of 10rpm, the extruder temperature of controlling first double screw extruder and second double screw extruder is 100 ℃, extrude abundant mixing continuously, adjustment is good, bubble takes off most spinning solution, through metering, after the filtration, send into spinning head, the spinneret cap specification is Φ 0.06 * 300 hole, through the air gap of 5cm layer, enter the coagulating bath spin duct, coagulation bath temperature is 5 ℃, and spinning speed is 120m/min, 6 times of jet stretches, spun tow is after the washing neutralization, send into annealing device, 400 ℃ of 10 seconds of following heat treatment, reoiling is wound into tube, measure according to GB, the intensity of gained PPTA (PPTA) fiber is 2.73GPa, and initial modulus is 183GPa, and extension at break is 1.31%.
The comparative result that conventional spinning method, semicontinuous spinning process (200310109240) and the inventive method is spinned the 2Kg Fanglun 1414 respectively is as shown in table 1.
Table 1 with traditional spinning, semicontinuous spinning process and the inventive method relatively
| Sample | Intensity (GPa) | Modulus (GPa) | Mixing, dissolving, spinning time |
| Conventional spinning method | 2.62 | 181 | 12.5 hour |
| Semicontinuous spinning process | 2.60 | 180 | 4 hours |
| The embodiment of the invention 1 | 2.71 | 182 | 2 hours |
Claims (5)
1. the method for a continuously preparing poly poly P phenylene diamine terephthalamide fiber is characterized in that, may further comprise the steps:
(1) be 98～100% the concentrated sulfuric acid with concentration and dry logarithmic viscosity number is that the PPTA resin of 4.0～8.5dl/g adds first double screw extruder continuously, wherein the percentage by weight of PPTA resin is 14～24%, mixing temperature is 50～100 ℃, the time of staying is 1～10 minute, and the shear rate of first double screw extruder is 300～2000s
-1
(2) above material enters second double screw extruder continuously after fully mixing, and regulating temperature is 50～100 ℃, and the time of staying is 10～60 minutes, extruding spinning solution after fully mixing, temperature adjustment, the deaeration;
(3) after spinning solution metering, the filtration, obtain poly-paraphenylene terephthalamide's diphenylamines fiber through doing conventional steps such as spray-wet spinning.
2. preparation method according to claim 1 is characterized in that: the concentrated sulfuric acid adopts liquid meter charging system weighing, and the PPTA resin adopts the metering of high accuracy weight-loss type continuous metering electronic scale.
3. preparation method according to claim 1 is characterized in that: the screw diameter of described first double screw extruder is 25～90mm, and draw ratio is 8～20, and in the same way or incorgruous rotation, rotating speed is 150～300rpm.
4. preparation method according to claim 1 is characterized in that: two screw rods of described first double screw extruder are made up of to the deep trouth threaded block multistage bull or single head just (or anti-), also have the reverse shallow thread groove of bull on the forward screw thread.
5. preparation method according to claim 1, it is characterized in that: the screw diameter of described second double screw extruder is 25～145mm, draw ratio is 30～60, screw speed is 10～200rpm, the time of staying of material in this screw extruder is 10～60 minutes, the first half of two intermeshing screw rods, from the screw rod total length that enters the mouth 30～80% part, be by various forward thread bush, the kneading piece of different rotation directions, and a spot of reverse thread cover is formed, wherein, the total length of mediating piece accounts for more than 30% of this partial-length, the latter half of two intermeshing screw rods is made up of the thread bush that reduces gradually along Way out pitch.
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| CNB2005100257083A CN100395381C (en) | 2005-05-10 | 2005-05-10 | Method of continuously preparing poly terephthaloyl-p-phenylene diamine fibre |
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| CNB2005100257083A CN100395381C (en) | 2005-05-10 | 2005-05-10 | Method of continuously preparing poly terephthaloyl-p-phenylene diamine fibre |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101220530B (en) * | 2007-01-08 | 2011-06-22 | 上海艾麦达化纤科技有限公司 | Production of uniform polyphenylene terephthalamide fibre |
| CN101555631B (en) * | 2008-04-10 | 2011-04-06 | 中国神马集团有限责任公司 | Industrial method for preparing PPTA spinning slurry with solid sulphuric acid |
| CN101871129A (en) * | 2009-04-27 | 2010-10-27 | 盐城市兰邦工业纤维有限公司 | Preparation method of alkali-soluble hydroxyethylcellulose fiber spinning solution with high solid content |
| DE102009036915A1 (en) * | 2009-08-11 | 2011-02-24 | List Holding Ag | Process for treating a monomer, pre-polymer, polymer or a corresponding mixture |
| CN102268743B (en) * | 2011-05-06 | 2013-04-03 | 上海舟汉纤维材料科技有限公司 | Device and method for efficiently dissolving poly(p-phenytene terephthalamide) resin |
| CN102953128B (en) * | 2012-04-16 | 2016-05-18 | 王泽� | The continuous spinning system of PPTA |
| CN105696104B (en) * | 2016-04-21 | 2018-01-16 | 中芳特纤股份有限公司 | A kind of preparation method of black system para-aramid fiber |
| CN109295506B (en) * | 2018-09-13 | 2020-07-28 | 清华大学 | Para-aramid spinning solution preparation system and preparation method thereof |
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| US5582911A (en) * | 1990-12-27 | 1996-12-10 | Michelin Recherche Et. Technique, S.A. | Aramid monofilament having a slightly structured skin--process for producing this monofilament |
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