CN1710160A - Method for preparing meta aromatic polyamide fiber - Google Patents
Method for preparing meta aromatic polyamide fiber Download PDFInfo
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- CN1710160A CN1710160A CN 200510026893 CN200510026893A CN1710160A CN 1710160 A CN1710160 A CN 1710160A CN 200510026893 CN200510026893 CN 200510026893 CN 200510026893 A CN200510026893 A CN 200510026893A CN 1710160 A CN1710160 A CN 1710160A
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Abstract
The polymer solution made by condensation polymerization of low-temperature solution is conducted wet spinning, formed in coagulating bath after extrusion step, the formed fiber is conducted wet stretching, then washed by water to remove the salt and solvent on fabric, dried and finally dry stretched. The characteristic lays in that in the extrusion step the spinning solution is directly fed into two-screw extruder, then de-foamed and extruded from the spinning nozzle passing through the measurement pump; In the water-washing step the supersonic device is used to thoroughly wash out the salt and solvent in fabric. Advantages: high efficiency, reduced ash content. The ash content is bellow 1000ppm, the tensile strength is more than 3.5 N/dtex and the extension rate at break is 20-69%.
Description
Technical field
The present invention relates to a kind of method for preparing meta-aromatic polyamide fiber, relate to more precisely a kind of enhance productivity and effectively reduce the fiber content of ashes between the preparation method of bit-type fully aromatic polyamide fiber.Belong to the fiber production field.
Background technology
Between the bit-type fully aromatic polyamide fiber have excellent heat resistance and flame resistant, and excellent high temperature electrical insulation capability, it has the textile processibility energy similar with cotton fiber simultaneously, thus be widely used in the occasion of high temperature resistant and anti-heated kang flame, as protective clothing, high heat filter fabric etc.
The preparation method of existing position fully aromatic polyamide fiber mainly contains two kinds:
1. use 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 neutralizes with calcium hydroxide, obtain containing the spinning solution of the poly of calcium chloride, calcium chloride content wherein is that benchmark is about 45% with the polymer.Above-mentioned spinning solution prepares the mpd-i fiber with dry-spinning process, shown in United States Patent (USP) 3360595.
2. be cosolvent with the polymer powder that interfacial polymerization or emulsion polymerisation obtain with the calorize calcium of polymer benchmark below 15% with m-phenylene diamine (MPD) and m-phthaloyl chloride, 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.
As in the common solvent spinning technology in order to make continuous the extruding of fiber, spinning solution need be through 3-5 hour vacuum defoamation, for poly (m-phenylene isophthalmide) spinning dope, because the system apparent viscosity is higher, compare with the typical solutions spinning technique, isotactic polypropylene nitrile fiber as usual, deaeration process are difficult.
In above two kinds of methods, first method particularly, owing to contain more calcium chloride in the spinning solution, though through being shaped, the wet stretching and process such as common washing still can not thoroughly be removed, and makes in the finished fiber content of inorganic salts higher.When fiber was used for field of electronic materials, residual ionic species can influence the insulating properties of material greatly in the fiber.Residual solvent also can influence the tensile property of fiber in the hot-stretch step simultaneously, and the color of resultant fiber also can yellowing.Common way is washed exactly on a large scale, but this method is limited to the removal effect of salt in the fiber and solvent, and the use of big water gaging can increase the cost that solvent recovery and the three wastes are handled.
Summary of the invention
The purpose of this invention is to provide a kind of method for preparing meta-aromatic polyamide fiber,, and go out to hang down bit-type fully aromatic polyamide fiber between ash with explained hereafter provided by the invention with bit-type fully aromatic polyamide fiber production efficiency between effective raising.
Of the present invention position fully aromatic polyamide fiber production technology comprises following steps, spinning solution is the polymer solution that m-phenylene diamine (MPD) and m-phthaloyl chloride obtain by the cryogenic fluid prepolymerization, this solution directly enters double screw extruder by the polymer storage tank and extrudes, carry out wet spinning, the stretching of in boiling water, wetting of fiber after the shaping, wash through the wet fiber that stretches, to remove salt and the solvent on the fiber, the fiber after the washing carries out drying, hot-stretch.It is characterized in that:
1) saved the deaeration process of spinning solution, after being incorporated into double screw extruder in the technological process, owing to set up bigger pressure at the head section of double screw extruder, thereby when making that spinning solution is pushed ahead in double screw extruder, wherein the bubble that is comprised but produces reciprocal motion under pressure, sloughs from the rear portion of screw rod.Its result makes spinning solution through after the double screw extruder, becomes even bubble-free clear solution, can realize extruding continuously of fiber.
2) in water-washing process, introduce ultrasonic device, improved washing efficiency, accelerated washing speed.In fact the process of washing is exactly the salt in detergent water and the fiber and the double diffusion process of solvent, in the presence of hyperacoustic, will accelerate this process, and effective especially for removing of the salt that is included in fibrous inside.Can reduce simultaneously the amount of slurry, promptly improve the content of solvent in the washes, in follow-up solvent recovery process, can effectively improve and reclaim yield and cut down the consumption of energy, thereby reduce production costs.
Double screw extruder used in the present invention, in order effectively to make spinning solution deaeration in extrusion, the head pressure of double screw extruder should be at 300kPa-4000kPa, and optimum is at 600kPa-1700Kpa; The diameter of extruder is 20-135mm, and draw ratio is 1: 24-1: 60.
In the production technology of of the present invention bit-type fully aromatic polyamide fiber, the polymer solution that is obtained by low temperature solution polymerization comprises the meta-aromatic polyamide of 15-20wt%, the calcium chloride of 7-9wt%, 1-2wt% water, solvent is N,N-dimethylacetamide (DMAC).
In the production technology of of the present invention bit-type fully aromatic polyamide fiber, the coagulating bath that wet spinning is used is the aqueous solution that comprises the DMAC of the calcium chloride of 5-25wt% and 25-60wt%, and coagulation bath temperature is 20-80 ℃.
In the production technology of of the present invention position fully aromatic polyamide fiber, the drawing medium in the wet stretching step is a water, and temperature is 60-100 ℃, and total drawing ratio is 2.0-3.5 times, divides and carries out for 1-3 time.
In the production technology of of the present invention position fully aromatic polyamide fiber, ultrasonic water-washing step can comprise drip washing and embathe two big classes.
In the production technology of of the present invention bit-type fully aromatic polyamide fiber, the drawing medium in the xeothermic stretching step is preferably nitrogen, and temperature is at 270-350 ℃, and draw ratio is 1.5-4.0.
In of the present invention the bit-type fully aromatic polyamide fiber, the content of ashes of fiber is below 1000ppm, and the tensile strength of fiber is greater than 3.5cN/dtex, and elongation at break is 20-60%.
The method of bit-type aromatic polyamide fibre is between preparation provided by the invention:
Obtain polymer solution through low temperature solution polymerization through after filtering by m-phenylene diamine (MPD) and m-phthaloyl chloride, need not to carry out deaeration, directly enter double screw extruder.In double screw extruder, the screw rod of two mutual arranged side by side, homodromal, tight engagement is with material, be that spinning solution constantly is fed forward, keep higher head pressure simultaneously, make the bubble in the solution move backward, the spinning solution homogeneous transparent of being extruded by head does not have bubble, simultaneously because double screw extruder good heat transfer performance can also make spinning solution reach spinning temperature rapidly in this process.
The key of this double screw extruder is to set up higher head pressure, make the spinning solution deaeration, and spinning solution itself does not produce chemical change and physical change except that temperature therein, so as long as satisfy the needs of output, the diameter and the draw ratio of screw rod do not had special requirement.Simultaneously because the spinning slurry temperature below 100 ℃, can adopt the chuck attemperating unit.
After being extruded by double screw extruder, spinning solution, carries out wet spinning through measuring pump and spinning head.Be introduced into coagulating bath and make fibre forming, coagulating bath is made up of the aqueous solution of calcium chloride and N,N-dimethylacetamide, and wherein the content of calcium chloride optimum is 15-25wt%, and the content of N,N-dimethylacetamide is 30-40wt%.The temperature of coagulating bath is excellent with 20-50 ℃.
The undrawn yarn that comes out from coagulating bath is introduced stretchings of wet of wet stretch bath, owing to a large amount of solvent that is contained has reduced the vitrification point of polymer, makes Fanglun 1313 carrying out the plasticising stretching below 100 ℃.Drawing medium is a water, and draft temperature is preferably at 80-100 ℃, and optimum is 93-100 ℃.For undrawn yarn is stretched fully, should adopt multistage stretching, consider short technological process, choose 2 grades and be stretched as suitable, total draw ratio and be controlled at 2.0-3.5, be excellent wherein with 2.0-3.0.
Through still residual many solvents and salt in the wet fiber that stretches, must remove by washing.Traditional fiber washing technology is that the simple a large amount of water of employing extracts salt in the fiber and solvent, and efficient is lower.The present invention introduces ultrasonic unit in water-washing process, ultrasonic intensity is 15W/dm
2-120W/dm
2, optimum at 18W/dm
2-70W/dm
2, wash time is 3-30 minute, is preferably 6-20 minute, under action of ultrasonic waves, can reinforcing fibre in the diffusion of salt and solvent, reduce the consumption of water, shorten washing process, and help reducing greatly the content of ashes of final product.
Fiber after the washing through 100 ℃ or above temperature drying to remove moisture.Enter xeothermic stretching step then, this step makes mechanical strength and the suitable fracture elongation that having of fiber is good.Carry out in the xeothermic 270-350 of being stretching in ℃ the heat pipe.Xeothermic stretching is optimum to be drawing medium with nitrogen, avoiding the oxidation of fiber under the drawing by high temperature situation, favourable for the conservation degree of the raising of fibre machinery performance and fiber colour.The multiple of xeothermic stretching is controlled at 1.5-4.0 according to the requirement of tensile strength and fiber number.
The logarithm ratio of resin dense sticking be to be solvent with the concentrated sulfuric acid, be made into the solution of 0.5g/100ml, adopt dark type viscometer, in 30 ℃ of mensuration, be calculated as follows:
η
inh＝ln(t/t
0)/c
T in the formula
0Be the solvent delivery time, t is the solution delivery time, and c is a polymer solution concentration, and unit is g/100ml.
Fiber number is measured according to GB/T14335-93.
Fracture strength and extension at break are measured according to GB/T14337-93.
Ash content is measured according to FZ/T50010.5-1998.
The present invention compared with prior art has following benefit:
1. cancellation spinning solution deaeration process is carried out ultrasonic washing to the wet later fiber that stretches, and has shortened technological process, enhances productivity.
2. ultrasonic washing can effectively reduce the content of salt and solvent in the fiber, reduces the content of ashes of finished fiber.
3. the consumption of water in the minimizing water-washing process helps improving the yield of solvent recovery.
Description of drawings
Fig. 1 be between the position fully aromatic polyamide fiber the production technology main flow chart.
The specific embodiment
Embodiment 1
The refining m-phenylene diamine (MPD) (MPD) of one weight portion is dissolved among the DMAC of drying of new distillation of 8.7 weight portions, carry out precondensation at-10 ℃ of refining m-phthaloyl chlorides (IPC) of molten state that add 1.7 weight portions down, generation contains behind the prepolymer of hydrogen chloride and the IPC of remaining 0.18 weight portion adds and has in the general reactor of agitator, and IPC adds in 30 minutes with molten condition.The temperature of control reactor obtains water white condensate reaction below 50 ℃ 1 hour, the subsequent neutralization, the Ca (OH) that neutralization is used
2Weight be 0.6851 part.Finally obtain containing polymer 18.1%, logarithmic specific concentration viscosity η
InhBe 1.68, CaCl
2Content is 8.26% spinning solution.Spinning solution is controlled to be 60 ℃ through excess temperature, draw ratio is behind 1: 40 the double screw extruder, extrude by the spinnerets that is the spinneret orifice of 0.08mm by 300 bore dias by measuring pump metering back that to enter temperature be in 20 ℃ the coagulating bath, this coagulating bath contains DMAC and the calcium chloride of 25wt% and the water of 40wt% of 35wt%, immersion length is 1.5m, and the speed that fiber goes out coagulating bath is 6m/min.Drawing of fiber does not enter the wet stretch bath of one-level then, and temperature is 100 ℃, and draw ratio is 2.0, enters the wet stretch bath of secondary then, and temperature is 100 ℃, and draw ratio is 1.25 times.The fiber that stretches through wetting is at 25W/dm
2The ultrasonic wave of intensity exists down washes 10min with 100 ℃ water logging.Washing fiber well is after 150 ℃ of following dryings, and the draw ratio with 2.0 in 300 ℃ heat pipe carries out xeothermic stretching.The fiber number of resulting Fanglun 1313 is 2.0 dtexs (dtex), and tensile strength is 3.5 lis of ox/dtexs (cN/dtex), and elongation at break is 42%, and the ash content of fiber is 963ppm.
Embodiment 2
The preparation of spinning solution is with embodiment 1.The spinning solution of making is through excess temperature after to be controlled to be 60 ℃ draw ratio be 1: 24 double screw extruder, extrude by the spinnerets that is the spinneret orifice of 0.09mm by 360 bore dias by measuring pump metering back that to enter temperature be in 45 ℃ the coagulating bath, this coagulating bath contains DMAC and the calcium chloride of 7wt% and the water of 68wt% of 25wt%, immersion length is 1.5m, and the speed that fiber goes out coagulating bath is 6m/min.Drawing of fiber does not enter the wet stretch bath of one-level then, and temperature is 94 ℃, and draw ratio is 2.0, enters the wet stretch bath of secondary then, and temperature is 95 ℃, and draw ratio is 1.20 times.The fiber that stretches through wetting is at 80W/dm
2The ultrasonic wave of intensity exists down washes 10min with 100 ℃ water logging.Washing fiber well is after 150 ℃ of following dryings, and the draw ratio with 2.0 in 300 ℃ heat pipe carries out xeothermic stretching.The fiber number of resulting Fanglun 1313 is 2.1dtex, and tensile strength is 3.3cN/dtex, and elongation at break is 47%, and the ash content of fiber is 855ppm.
Embodiment 3
The preparation of spinning solution is with embodiment 1.The spinning solution of making is through excess temperature after to be controlled to be 60 ℃ draw ratio be 1: 60 double screw extruder, extrude by the spinnerets that is the spinneret orifice of 0.06mm by 400 bore dias by measuring pump metering back that to enter temperature be in 75 ℃ the coagulating bath, this coagulating bath contains DMAC and the calcium chloride of 20wt% and the water of 32wt% of 58wt%, immersion length is 1.5m, and the speed that fiber goes out coagulating bath is 6m/min.Drawing of fiber does not enter the wet stretch bath of one-level then, and temperature is 97 ℃, and draw ratio is 2.0, enters the wet stretch bath of secondary then, and temperature is 100 ℃, and draw ratio is 1.30 times.The fiber that stretches through wetting is at 118W/dm
2The ultrasonic wave of intensity exists down washes 10min with 100 ℃ water logging.Washing fiber well is after 150 ℃ of following dryings, and the draw ratio with 2.0 in 300 ℃ heat pipe carries out xeothermic stretching.The fiber number of resulting Fanglun 1313 is 1.8dtex, and tensile strength is 3.6cN/dtex, and elongation at break is 34%, and the ash content of fiber is 788ppm.
Comparative example 1:
Adopt and embodiment 1 similar prepared Fanglun 1313, unique difference is not adopt ultrasonic washing in the washing stage, just washes 10min with 100 ℃ water logging.The fiber number of resulting Fanglun 1313 is 2.0dtex, and tensile strength is 3.4cN/dtex, and elongation at break is 42%, and the ash content of fiber is 3452ppm.
Comparative example 2:
Adopt and embodiment 1 similar prepared Fanglun 1313, difference is that employed coagulating bath proportioning is in spinning process: the DMAC that contains 20wt%, the calcium chloride of 3wt% and the water of 77wt%, the washing stage is not adopted ultrasonic washing, just washes 10min with 100 ℃ water logging.The fiber number of resulting Fanglun 1313 is 2.0dtex, and tensile strength is 3.0cN/dtex, and elongation at break is 29%, and the ash content of fiber is 2911ppm.
Claims (10)
1, a kind of method for preparing meta-aromatic polyamide fiber, spinning solution is that m-phenylene diamine (MPD) and m-phthaloyl chloride obtain polymer solution by low temperature solution polymerization, it is characterized in that (1) this polymer storage tank directly enters double screw extruder and extrudes, carry out wet spinning, (2) fiber after the shaping carries out the wet method stretching in boiling water, (3) fiber that stretches through wet method then carries out ultrasonic washing, and the fiber after (4) washing carries out drying, hot-stretch.
2, by the described method for preparing meta-aromatic polyamide fiber of claim 1, the head pressure that it is characterized in that described double screw extruder is 300Kpa-4000Kpa.
3, by claim 1 or the 2 described methods that prepare meta-aromatic polyamide fiber, the head pressure that it is characterized in that described double screw extruder is 600Kpa-1700Kpa.
4, by the method for bit-type aromatic polyamide fibre between claim 1,2 or 3 described preparations, the diameter that it is characterized in that described double screw extruder is 20～135mm, and draw ratio is 1: 24～1: 60.
5, press the method for bit-type aromatic polyamide fibre between the described preparation of claim 1, it is characterized in that the prepolymerization spinning solution comprise 15-20wt% between the bit-type aromatic polyamide, the calcium chloride of 7-9wt%, 1-2wt% water, solvent is a N,N-dimethylacetamide.
6, press the method for bit-type fully aromatic polyamide fiber between the described preparation of claim 1, it is characterized in that in the wet-formed step, the aqueous solution of the calcium chloride that consists of 5-25% of coagulating bath and the N,N-dimethylacetamide of 25-60%, coagulation bath temperature are 20-80 ℃.
7, by the method for bit-type aromatic polyamide fibre between the described preparation of claim 1, it is characterized in that the bath temperature in the wet method stretching step is 60-100 ℃, total drawing ratio is 2.0-3.5 times, divides and carries out for 1-3 time.
8, by the method for bit-type aromatic polyamide fibre between the described preparation of claim 1, it is characterized in that described ultrasound intensity is 15-20w/dm
3, the time is 3-30 minute, temperature is 60-100 ℃; Ultrasonic washing is drip washing or embathes.
9, by the method for bit-type aromatic polyamide fibre between the described preparation of claim 1, the temperature that it is characterized in that described xeothermic stretching step is drawing medium at 270-350 ℃ with nitrogen, and draw ratio is 1.5-4.0.
10, by the method for bit-type aromatic polyamide fibre between the described preparation of claim 8, it is characterized in that the supersound washing time is 6-20 minute.
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| CN100455706C (en) * | 2006-11-17 | 2009-01-28 | 钟洲 | Prepn process of poly (m-phenylene isophthalmide) spinning dope |
| CN101922062A (en) * | 2010-04-23 | 2010-12-22 | 东华大学 | Preparation method for meta-aromatic polyamide fiber |
| CN101379231B (en) * | 2006-01-31 | 2011-12-28 | 帝人高科技产品株式会社 | Meta-type wholly aromatic polyamide fiber excellent in high-temperature processability, and method for producing the same |
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| CN102534840A (en) * | 2010-12-29 | 2012-07-04 | 钟洲 | Method for preparing meta-aramid fiber |
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| CN2036535U (en) * | 1988-08-23 | 1989-04-26 | 中国科学院山西煤炭化学研究所 | Smallsize wet spinning machine |
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| CA2369681C (en) * | 2000-02-16 | 2006-03-28 | Teijin Limited | Meta-type wholly aromatic polyamide filaments and process for producing same |
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| CN108939950A (en) * | 2018-07-23 | 2018-12-07 | 大连理工大学 | A kind of preparation method of aromatic polyamide film |
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Assignee: Shengou(Suzhou) Safety Protection Material Co., Ltd. Assignor: Donghua University Contract record no.: 2010310000114 Denomination of invention: Method for preparing meta aromatic polyamide fiber Granted publication date: 20080702 License type: Exclusive License Open date: 20051221 Record date: 20100716 |