CN101285214B - Process for spinning low salt-containing aramid fiber 1313spinning solution by wet method - Google Patents
Process for spinning low salt-containing aramid fiber 1313spinning solution by wet method Download PDFInfo
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- CN101285214B CN101285214B CN2008100347685A CN200810034768A CN101285214B CN 101285214 B CN101285214 B CN 101285214B CN 2008100347685 A CN2008100347685 A CN 2008100347685A CN 200810034768 A CN200810034768 A CN 200810034768A CN 101285214 B CN101285214 B CN 101285214B
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Abstract
The invention relates to a method for spinning aramid fiber 1313 with low salt content by wet spinning. The method comprises the following steps of: prepolymerizing m-phenylenediamine (MPD) and part m-phthaloyl chloride (IPC); adding the preformed polymer and the rest m-phthaloyl chloride into a double-screw extruder to extrude the aramid fiber 1313 containing chlorine hydride; extruding spinning dope into a aqueous coagulation bath after neutralizing the chlorine hydride with calcium hydroxide; crimping and cutting coagulated tows into the required fiber length via hot water drawing, water rinsing, drying, dry-heat drawing and heat setting after being taken out of the coagulation bath to receive a finished fiber. The method is convenient and simple, can improve the molecular weight of products and the evenness of polycondensate, and reduce the salt content of the final spinning solution.
Description
Technical field
The invention belongs to aramid fiber 1313 process for spinning fibre by wet method field, particularly relate to a kind of aramid fiber 1313 process for spinning fibre by wet method of hyposaline.
Background technology
Aramid fiber 1313 has excellent heat resistance and flame resistant, and excellent high temperature electrical insulation capability, is used for preparation anti-flame material of fire prevention and high temperature insulating materials, as fiber, and paper etc.
The method of existing preparation aramid fiber 1313 is normally:
(1) interfacial polymerization
M-phenylene diamine (MPD) and m-phthaloyl chloride are at the poor solvent of aramid fiber 1313, as reacting in the oxolane, then with the aqueous solution high-speed mixing that contains acid absorbent, after finishing, reaction generates the aramid fiber 1313 of powder type, this polymer powder carries out spinning after being dissolved in amide solvent, adds the salt as cosolvent during dissolving as required.
This method intermittently operated, polymer must be separated dissolving again from polymerization system, be more difficult to get stable spinning solution.As United States Patent (USP) 3640970.
(2) low temperature solution polymerization
M-phenylene diamine (MPD) and m-phthaloyl chloride in amide solvent under lower temperature polymerization prepare aramid fiber 1313, hydrogen chloride as accessory substance neutralizes in solution, comprises above-mentioned neutralization and the polymer solution that is dissolved in the calcium chloride in the polymerization system that generates can be directly used in dry spinning.As United States Patent (USP) 3063966.The shortcoming of this method is owing to contain the salt of high concentration, then to be difficult to obtain the strong fiber of high machinery as using wet spinning, and owing to contain the CaCl of high concentration
2, all pipe-line systems and solvent recovery unit are all wanted the height anticorrosion, have greatly increased the investment and the line service amount of equipment, got fiber have naturally than higher production cost.
For addressing the above problem, Chinese patent publication number CN1219986 discloses a kind of wet-spinning method of aramid polymer of high saliferous, be to adopt to pass through one modulation step later on again by coagulating bath at fiber, the concentration of solvent makes the fiber plasticizing in the fiber thereby keep, fiber is under the effect of drafting tension, and the cavity of all existence all diminishes.The shortcoming of the method is that long filament productivity ratio is lower than the method that adopts the spinning solution that is substantially free of salt.
In addition, also attempted multiple different types of neutralizer, as described in Chinese patent publication number 1341169A, adopted the alkali metal hydroxide that produces the salt that is insoluble to office and solvent when comprising a kind of and hcl reaction, and be eliminated by filtration.Though the method can make the spinning solution of low saline salinity, under the polymer molecular weight condition with higher, filtration can be had any problem.
And polymerisation in solution all is to adopt discontinuous mode basically, and reaction heat is difficult for removing, and hot-spot then easily causes the difference of molecular weight.The method of United States Patent (USP) 3287324 disclosed continuous polymerizations adopts the once reinforced method of acyl chlorides, is difficult for grasping etc. mole ratio.
The method of existing preparation virtue wheel 1313 fibers has dry spinning and wet spinning.
Summary of the invention
The aramid fiber 1313 process for spinning fibre by wet method that the purpose of this invention is to provide a kind of hyposaline, it is the polymerization main reactor that this method adopts double screw extruder, easy and simple to handle, provide a kind of part to remove the method for the hydrogen chloride gas of small molecule by-product in the aramid fiber 1313 polymerization system.Because the extruding between the screw rod helps hydrogen chloride gas and discharges, and is got rid of by steam vent, thereby in neutralization procedure, generate less salt from polymerization system.
The aramid fiber 1313 process for spinning fibre by wet method of a kind of hyposaline of the present invention comprises the following steps:
(1) preparation of the aramid fiber 1313 spinning solution of hyposaline
A) prepolymerization of m-phenylene diamine (MPD) (MPD) and m-phthaloyl chloride (IPC)
The m-phthaloyl chloride of m-phenylene diamine (MPD) and mole ratios such as being less than carries out earlier precondensation in polar organic solvent, the prepolymerization temperature is-20 ℃～30 ℃, generation contains the prepolymer that accessory substance is a hydrogen chloride, the consumption of IPC is 50%～80% of total consumption, and feed way can be powder or molten condition;
B) prepolymer after filtering and residue IPC join in the double screw extruder as main reactor, set up the pressure of 0.2-5.0MPa in screw rod, and then by release pressure, extrude the aramid fiber 1313 that contains hydrogen chloride;
C) hydrogen chloride that previous step is generated in rapid with in the calcium hydroxide and after, the aramid fiber 1313 spinning solution can be directly used in spinning;
(2) process for spinning fibre by wet
D) after spinning solution mixes and criticizes, be solidified as tow in the solution in a kind of moisture solidifying by double screw extruder in blending tank;
E) previous step is rapid tow stretches and washing through boiling water, to remove salt and the solvent on the tow;
F) tow after the washing curls, cuts into desired fibre length after super-dry, xeothermic stretching and HEAT SETTING, obtains finished fiber.
Described step a) Semi-polarity organic solvent is that amide solvent is dimethylacetylamide (DMAC) or N-Methyl pyrrolidone (NMP).
The draw ratio of double screw extruder is 1: 10～1: 70 in the described step b), preferred 1: 40～1: 60, the temperature of control twin-screw main reactor is at 0 ℃～70 ℃, between preferred 10 ℃～50 ℃, the time that the polymerization procedure reactant stops in double screw extruder is 5～35 minutes, stopping temperature is 0 ℃～70 ℃, preferred 0 ℃～20 ℃.
The molar concentration of MPD in polymerization system is 0.6～1.2mol/l in the described step b), preferred 0.8～1.0mol/l.
Polymer concentration is 12～20% in the aramid fiber 1313 spinning solution of described step c), and comprising calcium chloride is 3～30% of poly, the logarithmic viscosity number of aramid fiber 1313 is 1.7dl/s-2.3dl/s, its logarithmic viscosity number measured value is to be solvent with the concentrated sulfuric acid, be made into the solution of 0.5g/100ml, adopt Ubbelohde viscometer,, be calculated as follows in 30 ℃ of mensuration:
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.
The diameter of double screw extruder spinneret orifice is 0.05～0.2mm in the described step d), and extruder temperature is controlled at 50～80 ℃, and the moisture solution that solidifies is to contain 15～25%CaCl
2With 25～40% Semi-polarity amide solvents be the aqueous solution of dimethylacetylamide (DMAC) or N-Methyl pyrrolidone (NMP), coagulation bath temperature is 20～80 ℃, the speed that tow goes out coagulating bath is 5～20m/min, and the immersion length of tow in coagulating bath is 1.5～2m.
Boiling water stretches and is divided into two sections stretchings in the described step e), and boiling water stretching general times is 2～4 times, and the fiber of this moment also contains more solvent and salt, needs to drop to residual solvent levels and calcium chloride content minimum through water-washing step.
Drying is that tow carries out drying at 100 ℃-140 ℃ in the described step f), and xeothermic stretching is that the multiple with 1.5～3 stretches in 270～350 ℃ heat stretching machine.
Described step e), f) in total drawing ratio be 4～6.
The fibre strength 2.5cN/dtex-5.8cN/dtex of described finished fiber, extension at break are 20～65%.
Beneficial effect of the present invention:
(1) the self-cleaning type double screw extruder that adopts of the present invention is made up of two intermeshing screw rods, contains the reverse thread groove on the forward screw thread, so material reaches abundant mixing at short notice, thereby can improve the uniformity of the molecular weight and the condensation polymer of product;
(2) because the extruding of screw rod reaches the exhaust apparatus of in position installing, by vacuumizing the low-molecular material hydrogen chloride that continuous eliminating reaction produces, reduce the hydrogen chloride content in the reflection system, thereby reduced the consumption of further neutralizer, and then reduced the salt content of final spinning solution;
(3) because the polymer solution by double screw extruder still contains the hydrogen chloride of part, so select the calcium hydroxide neutralization for use, the calcium chloride of generation is dissolved in the reaction system, stable favourable to spinning solution.
Description of drawings
Fig. 1 is a hyposaline PPTA spinning solution flow chart.
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 and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications 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.
The part and the percentage that relate in the following example except that special instruction is arranged, are weight portion.
Fiber number is measured according to GB/T14335-93.
Fracture strength and extension at break are measured according to GB/T14337-93.
Embodiment 1: the spinning solution preparation
1 part of refining MPD is dissolved among 10.92 parts the DMAC of drying of new distillation, add 1.7 parts of 60 ℃ of refining IPC down at-10 ℃ and carry out precondensation, generation contains the prepolymer of hydrogen chloride, keep temperature to be lower than 0 ℃, react after 20 minutes and the IPC of remaining 0.18 part of molten state to enter diameter be 30mm, draw ratio is 1: 60, and rotating speed is the double screw extruder of 200rpm.The temperature of control double-screw reactor is below 50 ℃, and vacuumizes by exhaust outlet, extrudes water white condensate in about 15 minutes, the subsequent neutralization, Ca (OH)
2Amount be 0.4 part.Finally obtain containing polymer 16.1%, η
InhBe 2.01, with respect to condensate CaCl
2Content is 14.8% spinning solution, and the later solution that neutralizes carries out the adjustment of pH value, mixes, and deaeration is filtered, and enters next step spinning.
Embodiment 2: the spinning solution preparation
1 part of refining MPD is dissolved among 10.92 parts the DMAC of drying of new distillation, in the general reactor that is having agitator under-18 ℃, add the refining IPC of 1.6 parts of molten states and carry out precondensation, generation contains the prepolymer of hydrogen chloride, keep temperature to be lower than 0 ℃, react after 22 minutes and the IPC of remaining 0.28 part of molten state to enter diameter be 50mm, draw ratio is 1: 50, and rotating speed is the double screw extruder of 180rpm.The temperature of control double-screw reactor is below 55 ℃, and vacuumizes by exhaust outlet, extrudes water white condensate in about 17 minutes, generate contain the prepolymer of hydrogen chloride after, the subsequent neutralization, Ca (OH)
2Amount be 0.25 part.Finally obtain containing polymer 15.5%, η
InhBe 1.88, with respect to condensate CaCl
2Content is 10.1% spinning solution, and the later solution that neutralizes carries out the adjustment of pH value, mixes, and deaeration is filtered, and enters next step spinning.
Embodiment 3: fiber production
With a kind of spinning solution for preparing of spinning solution example, be the spinneret orifice of 0.07mm by diameter, adopting temperature is that 8 ℃ coagulating bath solidifies that (solidifying solution is to contain 15～25%CaCl
2With 25～40% Semi-polarity amide solvents be the aqueous solution of DMAC or NMP), and stretch 1.8 times through 78 ℃ hot water, enter fiber through stretching together embathes 6 minutes in 98 ℃ hot water after in 286 ℃ the heat pipe and further stretch 2.1 times, after curl, HEAT SETTING, and cut-out, obtain finished fiber, the intensity of fiber is 3.5cN/dtex, and extension at break is 33%.
Embodiment 4: fiber production
With 2 kinds of spinning solutions that prepare of spinning solution example, be the spinneret orifice of 0.06mm by diameter, adopting temperature is that 10 ℃ coagulating bath solidifies that (solidifying solution is to contain 15～25%CaCl
2With 25～40% Semi-polarity amide solvents be the aqueous solution of DMAC or NMP), and stretch 1.5 times through 83 ℃ hot water, enter fiber through stretching together embathes 5.5 minutes in 98 ℃ hot water after in 288 ℃ the heat pipe and further stretch 2.6 times, after curl, HEAT SETTING, and cut-out, obtain finished fiber, the intensity of fiber is 3.55cN/dtex, and extension at break is 36%.
Claims (7)
1. the aramid fiber 1313 process for spinning fibre by wet method of a hyposaline comprises the following steps:
(1) preparation of the aramid fiber 1313 spinning solution of hyposaline
A) prepolymerization of m-phenylene diamine (MPD) MPD and m-phthaloyl chloride IPC
The m-phthaloyl chloride IPC of m-phenylene diamine (MPD) and mole ratios such as being less than carries out earlier precondensation in polar organic solvent, the prepolymerization temperature is-20 ℃～30 ℃, generation contains the prepolymer that accessory substance is a hydrogen chloride, and the consumption of m-phthaloyl chloride IPC is 50%～80% of total consumption; Described polar organic solvent is an amide solvent: dimethylacetylamide or N-Methyl pyrrolidone;
B) prepolymer after filtering and residue m-phthaloyl chloride IPC join in the double screw extruder as main reactor, m-phthaloyl chloride IPC adopts the fusion feeding manner, in screw rod, set up the pressure of 0.2-5.0MPa, and then, extrude the aramid fiber 1313 that contains hydrogen chloride by release pressure;
C) hydrogen chloride that previous step is generated in rapid with in the calcium hydroxide and after, the aramid fiber 1313 spinning solution can be directly used in spinning; Wherein the gained spinning solution is with respect to condensate CaCl
2Content is 14.8% or 10.1%;
(2) process for spinning fibre by wet
D) spinning solution is solidified as tow by double screw extruder in a kind of moisture solidifying in the solution; The diameter of described double screw extruder spinneret orifice is 0.05～0.2mm, and extruder temperature is controlled at 50-80 ℃, and the moisture solution that solidifies is to contain 15～25%CaCl
2With 25～40% amide solvents: the aqueous solution of dimethylacetylamide or N-Methyl pyrrolidone solvent, coagulation bath temperature are 20～80 ℃, and the speed that tow goes out coagulating bath is 5～20m/min, and the immersion length of tow in coagulating bath is 1.5～2m;
E) previous step is rapid tow stretches and washing through boiling water, to remove salt and the solvent on the tow;
F) tow after the washing curls, cuts into desired fibre length after super-dry, xeothermic stretching and HEAT SETTING, obtains finished fiber.
2. the aramid fiber 1313 process for spinning fibre by wet method of hyposaline according to claim 1, it is characterized in that: the draw ratio of double screw extruder is 1: 10～1: 70 in the described step b), the temperature of control twin-screw main reactor is at 0 ℃～70 ℃, the time that the polymerization procedure reactant stops in double screw extruder is 5～35 minutes, and stopping temperature is 0 ℃～70 ℃.
3. the aramid fiber 1313 process for spinning fibre by wet method of hyposaline according to claim 2, it is characterized in that: the draw ratio of described double screw extruder is 1: 40～1: 60, the temperature of control twin-screw main reactor is between 10 ℃～50 ℃, the time that the polymerization procedure reactant stops in double screw extruder is 5～35 minutes, and stopping temperature is 0 ℃～20 ℃.
4. the aramid fiber 1313 process for spinning fibre by wet method of hyposaline according to claim 1, it is characterized in that: the molar concentration of m-phenylene diamine (MPD) MPD in polymerization system is 0.6～1.2mol/l in the described step b).
5. the aramid fiber 1313 process for spinning fibre by wet method of hyposaline according to claim 4, it is characterized in that: the molar concentration of described m-phenylene diamine (MPD) MPD in polymerization system is 0.8～1.0mol/l.
6. the aramid fiber 1313 process for spinning fibre by wet method of hyposaline according to claim 1 is characterized in that: boiling water stretches and is divided into two sections stretchings in the described step e), and boiling water stretching general times is 2～4 times.
7. the aramid fiber 1313 process for spinning fibre by wet method of hyposaline according to claim 1, it is characterized in that: drying is that tow carries out drying 100 ℃-140 ℃ temperature in the described step f), xeothermic stretching is that the multiple with 1.5～3 stretches in 270～350 ℃ heat stretching machine, step e), f) in total drawing ratio be 4～6.
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| CN103526321B (en) * | 2013-09-27 | 2016-02-03 | 东莞市灿森新材料有限公司 | A kind of preparation method of high-performance polyisophthaloyl metaphenylene diamine fiber |
| CN107522858A (en) * | 2017-09-07 | 2017-12-29 | 湖南化工研究院有限公司 | Meta-aramid resin polymerization liquid and preparation method thereof, meta-aramid resin and meta-aramid fibre fibrid |
| CN109666978A (en) * | 2018-03-23 | 2019-04-23 | 盐城德安德新材料科技有限公司 | A method of preparing the dedicated meta-aramid fibers of aramid fiber sewing thread |
| CN113105624B (en) * | 2021-03-30 | 2022-12-06 | 山东聚芳新材料股份有限公司 | Preparation method of aramid 1314 (carbon fiber-carbon copolymer) fibrid |
| CN114059182A (en) * | 2021-11-15 | 2022-02-18 | 赣州龙邦材料科技有限公司 | Aramid fiber and preparation method and application thereof |
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Address after: 201620 Shanghai, Songjiang new town, North Road, No. 2999 people Patentee after: Donghua University Patentee after: SRO ARAMID FIBER (JIANGSU) CO., LTD. Address before: 201620 Shanghai, Songjiang new town, North Road, No. 2999 people Patentee before: Donghua University Patentee before: Shengou(Suzhou) Safety Protection Material Co., Ltd. |