CN105350109B - A kind of poly- phosphamide fiber and its fusion method preparation method - Google Patents
A kind of poly- phosphamide fiber and its fusion method preparation method Download PDFInfo
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- CN105350109B CN105350109B CN201510770454.1A CN201510770454A CN105350109B CN 105350109 B CN105350109 B CN 105350109B CN 201510770454 A CN201510770454 A CN 201510770454A CN 105350109 B CN105350109 B CN 105350109B
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Abstract
The present invention relates to a kind of poly- phosphamide fiber and its preparation method of melting, belong to chemical fibre forming processing technology field.Fiber composition is poly- phosphamide macromolecule, and its structural formula is：
Description
Technical field
The present invention relates to a kind of poly- phosphamide fiber and its fusion method preparation method, belong to chemical fibre forming processing technology
Field.
Background technology
A variety of industries such as petrochemical industry, natural gas, public security, fire-fighting are required to possess the cloth with fire retardant performance.
Flame-retarding blended fiber manufacture processing method mainly has two kinds：One kind is that cotton/terylene/nylon cloth prepares fire retardant by Final finishing
Material；Another is to prepare flame-retardant textile using aramid fiber blending.
It is fire-retardant, fireproof cloth various in style at present.Some conventional have fire resistance cloth such as spandex fibre cloth,
Polyacrylic and polyester fiber cloth, fire resistant viscose acetal fibre cloth, flame-resistant terylene cloth etc., this fiber have melting drippage, make skin when meeting fire
Skin is scalded, it is impossible to reach the effect of fire safety.Durable fire retardant THPC when fiber is post-processed, in length
There is the problem of separating out in the phase, it is difficult to reach persistently fire-retardant effect in existing, and be generally small molecule due to what is used in Final finishing
, there is the problem of reduction fire resistance is difficult to persistently fire-retardant through repeatedly washing in long-term use in fire retardant.
Du pont company is to utilize copolymerization method earliest, passes through the closeness and cohesion of the macromolecular chain in fiber-forming polymer
Power, so as to improve its heat endurance, successfully have developed the aromatic polyamide fibre of entitled " Nomex ", its heat resistance is non-
Chang Hao, limited oxygen index is up to 29, with permanent safeguard function, does not dissolve not combustion-supporting, leaves after burning things which may cause a fire disaster, can self-extinguish and not
Molten drop is produced, with certain comfortableness, gas permeability." Kevlar " studies for another aromatic polyamide fibre of E.I.Du Pont Company
Achievement, it is in addition to good fire resistance, also with high limited oxygen index and extremely strong friction resistant, Resisting fractre energy
Power.Japanese Di Ren companies also successfully have developed trade name " Apyil " aromatic polyamide fibre, its pole using the above method
Limited oxygen index is up to 29%~32%；Amoco Corp. of the U.S. disclosed a patent of invention in 1999, and the patent is provided
A kind of daiamid composition, said composition can reach flame retardant effect and non-condensing with good anti-drop performance；Suo Luodi
Sub- company discloses the flame-retardant polymer of a non-halogen on polymer-bound for 1998, prepared fiber, fabric or
Product all has anti-flammability or fire line.
But, above-mentioned fiber cost is high, it is difficult to widespread adoption is obtained in a short time, even if widely used virtue
Synthetic fibre fiber, there is also on the high side, poor air permeability, the low problem of snugness of fit.
The key for developing fire-retardant fireproof cloth is fire-retardant, fire proofing firbre preparation, develops a kind of good flame retardation effect, dress
Comfortableness height and cost low fire-retardant, fire proofing firbre, it is extremely urgent.
The content of the invention
The invention aims to solve that existing conventional fire resistance fibre is present it is inefficient, rheological temperature is low, melting
Drippage the problem of cause secondary burn, dyeing and finishing difficulty, poor, the price height of feel etc. there is provided a kind of poly- phosphamide fiber and its melt
Melt preparation method.
The purpose of the present invention is achieved through the following technical solutions.
A kind of poly- phosphamide fiber, fiber composition is poly- phosphamide macromolecule, and its structural formula is：
Wherein, n is the integer between 2~2000.
A kind of poly- phosphamide fibers melt method preparation method, is comprised the following steps that：
Step 1: under nitrogen protection, by dimethyl methyl phosphonate and 4,4 '-diamino phenyl phosphine oxide is well mixed,
It is dried in vacuo under catalyst action after heating response, produces poly- phosphinylidyne polyimide resin；
Catalyst is the one or more in ferric trichloride, anhydrous magnesium chloride, triphenyl phosphate, triethylamine, ethylenediamine；
Step 2: after the poly- phosphinylidyne polyimide resin of step one gained is cut into slices, vacuum drying, control moisture content is less than
80ppm；
Step 3: poly- phosphamide resin slicer will be dried obtained by step 2, melt spinnings are carried out at 340 DEG C -390 DEG C, just
Stretching, obtains the poly- phosphamide fiber filament of the denier of 0.0243 denier -2.2；
Step 4: poly- phosphamide fibre semi-finished products obtained by step 3, by boundling, stretching, thermal finalization, oil, crimp, cut
Into 70mm-160mm, drying, packing, poly- phosphamide semi-finished product chopped fiber is obtained.
Beneficial effect
1st, a kind of poly- phosphamide fiber of the invention, intensity is high, safety non-toxic, is suitable for that yarn weaved fabric etc. is fire-retardant to knit
Thing, good flame retardation effect, raw materials used source is wide, and cost is low；
2nd, a kind of poly- phosphamide fibers melt method preparation method of the invention, preparation technology is simple, easily operation, production effect
Rate is high, adapts to existing industrialized production appointed condition, can realize industrialized production, production process is safe and reliable.
3rd, the present invention is crimped at 370 DEG C, can voluntarily be carbonized under hot conditions, does not cause melting to be dripped.
Embodiment
Present disclosure is further described with reference to embodiment.
Embodiment 1
A kind of poly- phosphamide fiber, fiber composition is poly- phosphamide macromolecule, and its structural formula is：
Wherein, n is the integer between 2~2000.
Embodiment 2
By 105mol dimethyl methyl phosphonates, 100mol 4,4 '-diamino phenyl phosphine oxide, 1mol triethylamines, input
It is well mixed in polymeric kettle, 12h is reacted at 378 DEG C, 80 DEG C of vacuum extraction 2.5h after reaction terminates, extracting is cooled to room after terminating
Temperature, obtains light yellow solid, and as poly- phosphamide resin polymerization degree is 1865.After poly- phosphinylidyne polyimide resin is cut into slices, 80 DEG C
Rotary-drum vacuum is dried after 1.5h, and 150 DEG C of rotary-drum vacuums dry 6h, and control moisture content is less than 40ppm；Poly- phosphinylidyne polyimide resin will be dried
Section, carries out spinning, it is 360 DEG C to control screw extruder temperature, and spinning speed is 1200m/ through screw extruder, spinneret
Min, obtains the poly- phosphamide fiber filament semi-finished product of 0.37 denier, continues through boundling, stretching, thermal finalization, oils, crimps, being cut into
75mm semi-finished product, after drying, packing, obtain 37.91 kilograms of poly- phosphamide chopped fibers；
The poly- phosphamide chopped fiber of preparation is discongested in the reciprocating breaker beater of HXF-1 types and mixes equal in machine through confusing
It is even；Through spinning, machine is woven into yarn, controls the fabric of preparation using computer on WF-II type looms.The fabric of preparation hangs down
Straight combustion testing, test result is as shown in table 1.
The vertical burn test result of the fire- resistance cloth of table 1
Embodiment 3
By 100mol dimethyl methyl phosphonates, 100mol 4,4 '-diamino phenyl phosphine oxide, 1.5mol triphenyl phosphates are thrown
Enter in polymeric kettle and be well mixed, 10h is reacted at 380 DEG C, 80 DEG C of vacuum extraction 2h after reaction terminates, extracting is cooled to room after terminating
Temperature, obtains light yellow solid, and as poly- phosphamide resin polymerization degree is 1970.After poly- phosphinylidyne polyimide resin is cut into slices, 85 DEG C
Rotary-drum vacuum is dried after 1h, and 180 DEG C of rotary-drum vacuums dry 5h, and control moisture content is less than 40ppm；Poly- phosphinylidyne polyimide resin will be dried to cut
Piece, carries out spinning, it is 365 DEG C to control screw extruder temperature, and spinning speed is 1500m/min through screw extruder, spinneret,
The poly- phosphamide fiber filament of 0.82 denier is obtained, boundling, stretching is continued through, thermal finalization, oils, crimps, being cut into 96mm semi-finished product,
After drying, packing, 38.13 kilograms of poly- phosphamide chopped fibers are obtained.
The short silk of poly- phosphamide of preparation is discongested in the reciprocating breaker beater of HXF-1 types and is well mixed through confusing in machine；
Through spinning, machine is woven into yarn, controls the fabric of preparation using computer on WF-II type looms.The fabric of preparation vertically fires
Test is burnt, test result is as shown in table 2.
The vertical burn test result of the fire- resistance cloth of table 2
Embodiment 4
By 125mol dimethyl methyl phosphonates, 100mol 4,4 '-diamino phenyl phosphine oxide, 1.5mol ferric trichlorides,
Put into polymeric kettle and be well mixed, 8h, 80 DEG C of vacuum extraction 1.5h after reaction terminates are reacted at 386 DEG C, extracting is cooled down after terminating
To room temperature, light yellow solid is obtained, as poly- phosphamide resin polymerization degree is 730.After poly- phosphinylidyne polyimide resin is cut into slices, 70
DEG C rotary-drum vacuum is dried after 2h, and 220 DEG C of rotary-drum vacuums dry 5h, and control moisture content is less than 40ppm；Poly- phosphinylidyne polyimide resin will be dried
Section, carries out spinning, it is 360 DEG C to control screw extruder temperature, and spinning speed is 1000m/ through screw extruder, spinneret
Min, obtains the poly- phosphamide fiber filament semi-finished product of 1.73 denier, continue through boundling, stretching, thermal finalization, oil, crimp, drying,
After packing process, 37.99 kilograms of poly- phosphamide filament fibers are obtained.
The poly- phosphamide long filament of preparation is woven into yarn through the machine that spins, computer control is used on WF-II type looms
The fabric prepared.The fabric vertical burn test of preparation, test result is as shown in table 3.
The vertical burn test result of the fire- resistance cloth of table 3
Embodiment 5
By 150mol dimethyl methyl phosphonates, 100mol 4,4 '-diamino phenyl phosphine oxide, 0.5mol ferric trichlorides,
Put into polymeric kettle and be well mixed, 8h, 80 DEG C of vacuum extraction 1.5h after reaction terminates are reacted at 384 DEG C, extracting is cooled down after terminating
To room temperature, light yellow solid is obtained, as poly- phosphamide resin polymerization degree is 1780.After poly- phosphinylidyne polyimide resin is cut into slices,
70 DEG C of rotary-drum vacuums are dried after 2h, and 220 DEG C of rotary-drum vacuums dry 5h, and control moisture content is less than 40ppm；Poly- phosphamide tree will be dried
Fat is cut into slices, and carries out spinning through screw extruder, spinneret, it is 360 DEG C to control screw extruder temperature, and spinning speed is 1000m/
Min, obtains the poly- phosphamide fiber filament semi-finished product of 1.82 denier, continue through boundling, stretching, thermal finalization, oil, crimp, drying,
After packing, 39.22 kilograms of poly- phosphamide filament fibers are obtained.
Embodiment 6
By 50mol dimethyl methyl phosphonates, 100mol 4,4 '-diamino phenyl phosphine oxide, 0.8mol ferric trichlorides,
It is well mixed in 0.3mol triethylamines, input polymeric kettle, 13h, 80 DEG C of vacuum extraction 3.5h after reaction terminates is reacted at 367 DEG C,
Extracting is cooled to room temperature after terminating, and obtains light yellow solid, and as poly- phosphamide resin polymerization degree is 1688.By poly- phosphamide tree
After fat is cut into slices, 90 DEG C of rotary-drum vacuums are dried after 2h, and 250 DEG C of rotary-drum vacuums dry 5h, and control moisture content is less than 30ppm；Will
Poly- phosphamide resin slicer is dried, spinning is carried out through screw extruder, spinneret, it is 300 DEG C to control screw extruder temperature, is spun
Silk speed be 800m/min, obtain the poly- phosphamide fiber filament semi-finished product of 2.1 denier, continue through boundling, stretching, thermal finalization, on
After oil, curling, drying, packing, 38.67 kilograms of poly- phosphamide filament fibers are obtained.
Claims (2)
1. a kind of preparation method of poly- phosphamide fibers melt, its feature is as follows, comprise the following steps that：
Step 1: under nitrogen protection, by dimethyl methyl phosphonate and 4,4 '-diamino phenyl phosphine oxide is well mixed, in catalysis
It is dried in vacuo after the lower heating response of agent effect, produces poly- phosphinylidyne polyimide resin；
Step 2: after the poly- phosphinylidyne polyimide resin of step one gained is cut into slices, vacuum drying, control moisture content is less than 80ppm；
Step 3: poly- phosphamide resin slicer will be dried obtained by step 2, in 340 DEG C of -390 DEG C of progress melt spinnings, just stretch,
Obtain the poly- phosphamide fiber filament of the denier of 0.0243 denier -2.2；
Step 4: poly- phosphamide fibre semi-finished products obtained by step 3, by boundling, stretching, thermal finalization, oil, crimp, be cut into
70mm-160mm, drying, packing, obtain poly- phosphamide semi-finished product chopped fiber.
2. a kind of preparation method of poly- phosphamide fibers melt according to claim 1, its feature is as follows, institute in step one
The catalyst stated includes the one or more in ferric trichloride, anhydrous magnesium chloride, triphenyl phosphate, triethylamine, ethylenediamine.
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