CN105350109A - Polyphosphamide fiber and melting-process preparation method thereof - Google Patents
Polyphosphamide fiber and melting-process preparation method thereof Download PDFInfo
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- CN105350109A CN105350109A CN201510770454.1A CN201510770454A CN105350109A CN 105350109 A CN105350109 A CN 105350109A CN 201510770454 A CN201510770454 A CN 201510770454A CN 105350109 A CN105350109 A CN 105350109A
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Abstract
The invention relates to a polyphosphamide fiber and a melting preparation method thereof, and belongs to the technical field of chemical fiber forming processing. The fiber is composed of polyphosphamide macromolecules and has the structural formula described in the description, wherein n is an integer of 2-2000. The polyphosphamide fiber melting preparation method comprises the steps: firstly, under nitrogen gas protection, mixing dimethyl methylphosphonate and 4,4'-diaminophenyl phosphine oxide evenly, and under the action of a catalyst, carrying out a reaction to obtain polyphosphamide resin; secondly, slicing the polyphosphamide resin obtained in the step one, carrying out vacuum drying, and controlling the moisture content to be less than 30-80 ppm; and thirdly, drying the polyphosphamide resin slices, carrying out melt spinning by a melt spinning machine, carrying out processes of initial drawing, clustering, stretching, heat setting, oiling, curling, cutting, drying and packaging, and thus obtaining the polyphosphamide fiber.
Description
Technical field
The present invention relates to a kind of poly-phosphamide fiber and fusion method preparation method thereof, belong to chemical fibre forming processing technology field.
Background technology
The multiple industry such as petrochemical industry, natural gas, public security, fire-fighting all requires to possess the cloth with fire-retardant fireproof performance.Flame-retarding blended fiber manufactures processing method and mainly contains two kinds: one is that cotton/terylene/nylon cloth prepares flame retardant fabric through Final finishing; Another kind uses aramid fiber blending to prepare flame-retardant textile.
Fire-retardant, fireproof cloth is various in style at present.Conventional some have the cloth of fire resistance as spandex fibre cloth, polyacrylic and polyester fiber cloth, fire resistant viscose acetal fibre cloth, flame-resistant terylene cloth etc., and this fibrid all also exists melting drippage, makes skin scald, can not reach the effect of fire safety when meeting fire.Durable fire retardant Tetrakis hydroxymethyl phosphonium chloride during fiber post processing, the problem of precipitation is there is in long-term existence, be difficult to reach effect fire-retardant lastingly, and mostly be Small molecular fire retardant due to what use in Final finishing, be difficult to problem fire-retardant lastingly through repeatedly washing existence reduction fire resistance in Long-Time Service.
Du pont company utilizes copolymerization method the earliest, by closeness and the cohesive force of the macromolecular chain at fiber-forming polymer, thus improve its heat endurance, successfully have developed the aromatic polyamide fibre of " Nomex " by name, its heat resistance is very good, limited oxygen index reaches 29, has permanent safeguard function, does not dissolve not combustion-supporting, after leaving burning things which may cause a fire disaster, can self-extinguish and do not produce molten drop, there is certain comfortableness, gas permeability.Another aromatic polyamide fibre achievement in research that " Kevlar " is E.I.Du Pont Company, it is except having good fire resistance, also has high limited oxygen index and extremely strong friction resistant, Resisting fractre ability.Di Ren company of Japan also adopts said method successfully to have developed the aromatic polyamide fibre of commodity " Apyil " by name, and its limited oxygen index can reach 29% ~ 32%; Amoco Corp. of the U.S. disclosed a patent of invention in 1999, and this patent provides a kind of daiamid composition, and said composition can reach flame retardant effect and have the good anti-performance and noncondensing of dripping; Solutia Corp discloses the flame-retardant polymer of a non-halogen about polymer-bound for 1998, and prepared fiber, fabric or goods all have anti-flammability or fire line.
But above-mentioned fiber cost is high, be difficult to obtain widespread adoption at short notice, even if widely used aramid fiber, also there is the problems such as on the high side, poor air permeability, snugness of fit are low.
The key of development fire-retardant fireproof cloth is preparation that is fire-retardant, Flame Retardant Fibers, develops a kind of good flame retardation effect, snugness of fit high and fire-retardant, Flame Retardant Fibers that cost is low, extremely urgent.
Summary of the invention
The object of the invention is the problem that efficiency is not high, rheological temperature is low, melting drippage causes secondary burn, dyeing and finishing is difficult, feel is poor, price is high existed to solve existing conventional fire resistance fibre, the one provided gathers phosphamide fiber and fusion preparation method thereof.
The object of the invention is to be achieved through the following technical solutions.
A kind of poly-phosphamide fiber, fibrous 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, concrete steps are as follows:
Step one, under nitrogen protection, by dimethyl methyl phosphonate and 4,4 '-diamino phenyl phosphine oxide mixes, and adds thermal response final vacuum dry, obtain poly-phosphamide resin under catalyst action;
Catalyst is one or more in ferric trichloride, anhydrous magnesium chloride, triphenyl phosphate, triethylamine, ethylenediamine;
Step 2, to be gathered by step one gained after phosphamide resin cuts into slices, vacuumize, controls moisture content and is less than 80ppm;
Step 3, by the poly-phosphamide resin slicer of step 2 gained drying, carry out melt spinning, just stretch at 340 DEG C-390 DEG C, obtaining for 0.0243 dawn at dawn-2.2 gathers phosphamide fiber filament;
Step 4, step 3 gained gather phosphamide fibre semi-finished products, through boundling, stretching, HEAT SETTING, oil, curling, be cut into 70mm-160mm, oven dry, packing, obtain poly-phosphamide semi-finished product staple fibre.
Beneficial effect
1, one of the present invention gathers phosphamide fiber, and intensity is high, safety non-toxic, is suitable for the flame-retardant textiles such as blending cloth, good flame retardation effect, and raw materials used source is wide, and cost is low;
2, one of the present invention gathers phosphamide fibers melt method preparation method, and preparation technology is simple, and easily operate, production efficiency is high, and adapt to existing suitability for industrialized production appointed condition, can realize suitability for industrialized production, production process is safe and reliable.
3, the present invention is curling 370 DEG C of generations, can carbonize voluntarily, do not cause melting to drip under hot conditions.
Detailed description of the invention
Below in conjunction with embodiment, content of the present invention is further described.
Embodiment 1
A kind of poly-phosphamide fiber, fibrous is poly-phosphamide macromolecule, and its structural formula is:
Wherein, n is the integer between 2 ~ 2000.
Embodiment 2
By 105mol dimethyl methyl phosphonate, 100mol4,4 '-diamino phenyl phosphine oxide, 1mol triethylamine, drop in polymeric kettle and mix, at 378 DEG C of reaction 12h, reaction terminates rear 80 DEG C of vacuum extraction 2.5h, be cooled to room temperature after extracting terminates, obtain light yellow solid, being poly-phosphamide resin polymerization degree is 1865.After being cut into slices by poly-phosphamide resin, after 80 DEG C of dry 1.5h of rotary-drum vacuum, 150 DEG C of dry 6h of rotary-drum vacuum, control moisture content and are less than 40ppm; Drying is gathered phosphamide resin slicer, spinning is carried out through screw extruder, spinnerets, controlling screw extruder temperature is 360 DEG C, spinning speed is 1200m/min, obtaining for 0.37 dawn gathers phosphamide fiber filament semi-finished product, continue through boundling, stretching, HEAT SETTING, oil, curling, be cut into 75mm semi-finished product, dry, packing after, obtain 37.91 kilograms of poly-phosphamide staple fibres;
The poly-phosphamide staple fibre of preparation is discongested and mixed through confusing in machine in the reciprocating breaker beater of HXF-1 type; Yarn is woven into, the fabric that WF-II type loom adopts conputer controlled to prepare through spinning machine.The fabric vertical combustion test of preparation, test result is as shown in table 1.
The vertical combustion test result of table 1 fire-resistance cloth
Embodiment 3
By 100mol dimethyl methyl phosphonate, 100mol4,4 '-diamino phenyl phosphine oxide, 1.5mol triphenyl phosphate, drop in polymeric kettle and mix, at 380 DEG C of reaction 10h, reaction terminates rear 80 DEG C of vacuum extraction 2h, be cooled to room temperature after extracting terminates, obtain light yellow solid, being poly-phosphamide resin polymerization degree is 1970.After being cut into slices by poly-phosphamide resin, after 85 DEG C of dry 1h of rotary-drum vacuum, 180 DEG C of dry 5h of rotary-drum vacuum, control moisture content and are less than 40ppm; Drying is gathered phosphamide resin slicer, spinning is carried out through screw extruder, spinnerets, controlling screw extruder temperature is 365 DEG C, spinning speed is 1500m/min, obtaining for 0.82 dawn gathers phosphamide fiber filament, continue through boundling, stretching, HEAT SETTING, oil, curling, be cut into 96mm semi-finished product, dry, packing after, obtain 38.13 kilograms of poly-phosphamide staple fibres.
The short silk of poly-phosphamide of preparation is discongested and mixed through confusing in machine in the reciprocating breaker beater of HXF-1 type; Yarn is woven into, the fabric that WF-II type loom adopts conputer controlled to prepare through spinning machine.The fabric vertical combustion test of preparation, test result is as shown in table 2.
The vertical combustion test result of table 2 fire-resistance cloth
Embodiment 4
By 125mol dimethyl methyl phosphonate, 100mol4,4 '-diamino phenyl phosphine oxide, 1.5mol ferric trichloride, drop in polymeric kettle and mix, at 386 DEG C of reaction 8h, reaction terminates rear 80 DEG C of vacuum extraction 1.5h, be cooled to room temperature after extracting terminates, obtain light yellow solid, being poly-phosphamide resin polymerization degree is 730.After being cut into slices by poly-phosphamide resin, after 70 DEG C of dry 2h of rotary-drum vacuum, 220 DEG C of dry 5h of rotary-drum vacuum, control moisture content and are less than 40ppm; Drying is gathered phosphamide resin slicer, spinning is carried out through screw extruder, spinnerets, controlling screw extruder temperature is 360 DEG C, spinning speed is 1000m/min, obtaining for 1.73 dawn gathers phosphamide fiber filament semi-finished product, continue through boundling, stretching, HEAT SETTING, oil, curling, dry, after packing process, obtain 37.99 kilograms of poly-phosphamide filament fibers.
The poly-phosphamide long filament of preparation is woven into yarn, the fabric that WF-II type loom adopts conputer controlled to prepare through spinning machine.The fabric vertical combustion test of preparation, test result is as shown in table 3.
The vertical combustion test result of table 3 fire-resistance cloth
Embodiment 5
By 150mol dimethyl methyl phosphonate, 100mol4,4 '-diamino phenyl phosphine oxide, 0.5mol ferric trichloride, drop in polymeric kettle and mix, at 384 DEG C of reaction 8h, reaction terminates rear 80 DEG C of vacuum extraction 1.5h, be cooled to room temperature after extracting terminates, obtain light yellow solid, being poly-phosphamide resin polymerization degree is 1780.After being cut into slices by poly-phosphamide resin, after 70 DEG C of dry 2h of rotary-drum vacuum, 220 DEG C of dry 5h of rotary-drum vacuum, control moisture content and are less than 40ppm; Drying is gathered phosphamide resin slicer, spinning is carried out through screw extruder, spinnerets, controlling screw extruder temperature is 360 DEG C, spinning speed is 1000m/min, obtaining for 1.82 dawn gathers phosphamide fiber filament semi-finished product, continue through boundling, stretching, HEAT SETTING, oil, curling, dry, packing after, obtain 39.22 kilograms of poly-phosphamide filament fibers.
Embodiment 6
By 50mol dimethyl methyl phosphonate, 100mol4,4 '-diamino phenyl phosphine oxide, 0.8mol ferric trichloride, 0.3mol triethylamine, drop in polymeric kettle and mix, at 367 DEG C of reaction 13h, reaction terminates rear 80 DEG C of vacuum extraction 3.5h, be cooled to room temperature after extracting terminates, obtain light yellow solid, being poly-phosphamide resin polymerization degree is 1688.After being cut into slices by poly-phosphamide resin, after 90 DEG C of dry 2h of rotary-drum vacuum, 250 DEG C of dry 5h of rotary-drum vacuum, control moisture content and are less than 30ppm; Drying is gathered phosphamide resin slicer, spinning is carried out through screw extruder, spinnerets, controlling screw extruder temperature is 300 DEG C, spinning speed is 800m/min, obtaining for 2.1 dawn gathers phosphamide fiber filament semi-finished product, continue through boundling, stretching, HEAT SETTING, oil, curling, dry, packing after, obtain 38.67 kilograms of poly-phosphamide filament fibers.
Claims (3)
1. a poly-phosphamide fiber, its feature is as follows, and fibrous is poly-phosphamide macromolecule, and its structural formula is:
Wherein, n is the integer between 2 ~ 2000.
2. a preparation method for poly-phosphamide fibers melt, its feature is as follows, and concrete steps are as follows:
Step one, under nitrogen protection, by dimethyl methyl phosphonate and 4,4 '-diamino phenyl phosphine oxide mixes, and adds thermal response final vacuum dry, obtain poly-phosphamide resin under catalyst action;
Step 2, to be gathered by step one gained after phosphamide resin cuts into slices, vacuumize, controls moisture content and is less than 80ppm;
Step 3, by the poly-phosphamide resin slicer of step 2 gained drying, carry out melt spinning, just stretch at 340 DEG C-390 DEG C, obtaining for 0.0243 dawn at dawn-2.2 gathers phosphamide fiber filament;
Step 4, step 3 gained gather phosphamide fibre semi-finished products, through boundling, stretching, HEAT SETTING, oil, curling, be cut into 70mm-160mm, oven dry, packing, obtain poly-phosphamide semi-finished product staple fibre.
3. the preparation method of a kind of poly-phosphamide fibers melt according to claim 2, its feature is as follows, and the catalyst described in step one comprises one or more in ferric trichloride, anhydrous magnesium chloride, triphenyl phosphate, triethylamine, ethylenediamine.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105239189A (en) * | 2015-11-13 | 2016-01-13 | 深圳市名仕度服饰有限公司 | Phosphamide fiber and preparation method thereof through solution method |
| CN109251602A (en) * | 2018-07-28 | 2019-01-22 | 南京艾利克斯电子科技有限公司 | A kind of anti-static coatings and preparation method thereof of electronic component high adhesion force |
| CN115449906A (en) * | 2022-08-30 | 2022-12-09 | 福建成东新材料科技有限公司 | Preparation method of polymethylpentene spun monofilament |
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| CN101497741A (en) * | 2009-02-27 | 2009-08-05 | 中北大学 | Phosphine copolyamide / nano montmorillonite flame-retardant composite material and preparation thereof |
| CN103732815A (en) * | 2011-05-27 | 2014-04-16 | 东丽奥培隆特士有限公司 | Elastic fabric |
| CN104278349A (en) * | 2013-07-02 | 2015-01-14 | 上海杰事杰新材料(集团)股份有限公司 | Antistatic and flame retardant copolyester fiber and preparation method thereof |
| CN105037715A (en) * | 2014-12-02 | 2015-11-11 | 淮安市欣佳尼龙有限公司 | Preparation method of flame-retarding nylon 610 and toothbrush hair produced therefrom |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101497741A (en) * | 2009-02-27 | 2009-08-05 | 中北大学 | Phosphine copolyamide / nano montmorillonite flame-retardant composite material and preparation thereof |
| CN103732815A (en) * | 2011-05-27 | 2014-04-16 | 东丽奥培隆特士有限公司 | Elastic fabric |
| CN104278349A (en) * | 2013-07-02 | 2015-01-14 | 上海杰事杰新材料(集团)股份有限公司 | Antistatic and flame retardant copolyester fiber and preparation method thereof |
| CN105037715A (en) * | 2014-12-02 | 2015-11-11 | 淮安市欣佳尼龙有限公司 | Preparation method of flame-retarding nylon 610 and toothbrush hair produced therefrom |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105239189A (en) * | 2015-11-13 | 2016-01-13 | 深圳市名仕度服饰有限公司 | Phosphamide fiber and preparation method thereof through solution method |
| CN105239189B (en) * | 2015-11-13 | 2017-07-07 | 深圳市名仕度服饰有限公司 | A kind of poly- phosphamide fiber and its solwution method preparation method |
| CN109251602A (en) * | 2018-07-28 | 2019-01-22 | 南京艾利克斯电子科技有限公司 | A kind of anti-static coatings and preparation method thereof of electronic component high adhesion force |
| CN115449906A (en) * | 2022-08-30 | 2022-12-09 | 福建成东新材料科技有限公司 | Preparation method of polymethylpentene spun monofilament |
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