CN102277653A - Preparation method of inflame-retardant anti-dripping polyester composite fibers - Google Patents
Preparation method of inflame-retardant anti-dripping polyester composite fibers Download PDFInfo
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Abstract
The invention relates to a preparation method of inflame-retardant anti-dripping polyester composite fibers. The method provided by the invention comprises the following steps of: (1) mixing aromatic dicarboxylic acid, dihydric alcohol and phosphorus-containing fire retardant and adding catalyst and heat stability; reacting to obtain an inflame-retardant copolyester; (2) pre-mixing SNF2, SnO, NH4H2PO4 or P2O5 for 30-60 min and melting at a temperature in a range of 400-500 DEG C for 60-90 min; cooling and carrying out a heat treatment at a temperature in a range of 70-100 DEG C for 90-120 min to obtain phosphate glass; and (3) blending the inflame-retardant copolyester with the phosphate glass and melting and spinning to obtain the inflame-retardant anti-dripping polyester composite fibers. The method provided by the invention has the advantages of simple process and easiness of being implemented; the prepared copolyester and fibers thereof have good inflame-retardant and anti-dripping performances; the limit oxygen index of the textiles is 29.8-33.2% and no melted drops are formed when the product is combusted so that the method provided by the invention has a good application prospect.
Description
Technical field
The invention belongs to the preparation field of polyester complex fiber, particularly a kind of preparation method of flame-retardant and anti-dripping polyester complex fiber.
Background technology
Most of fibers and textiles belong to inflammable or combustible material, because of the not fire-retardant fire that causes of textiles accounts for the fire incident sum more than 20%.Polyester fiber has become the kind that purposes is the widest in the textiles, output is maximum because of its excellent physical and mechanical performance and excellent comprehensive performances.But fiber is a kind of combustible fibre, and when burning produce serious fusion drippage, its application in a lot of fields is restricted.Therefore, the research of fiber flame-retarded technology becomes the problem that academia and industrial quarters are extremely paid close attention to, and various fire-retardant polyester fibre products and patent are constantly come out since last century the seventies.
Polyester fiber or fabric are carried out fire-retardant method to be had a variety ofly, can reduce fire-retardant post processing, modification by copolymerization method and blending modification method by the introducing mode of production process and fire retardant.The advantage of fire-retardant post treatment method is that technology is simple, and is with low cost, but that shortcoming is a persistence is poor, bigger to physical and mechanical properties influences such as the brute force of fiber and fabric, feels; Blending modification method has characteristics such as production is easy, and variety renovation is flexible, and shortcoming is that additive flame retardant is prone to migration or osmotic phenomena; The modification by copolymerization method is because fire-retardant monomer solid fixes on the polyester macromolecule chain, and fire resistance is lasting, is a kind of permanent fire resistance fibre.Aspect fire retardant, there is not the phosphorus flame retardant that has excitant and corrosive gas to discharge when high-efficiency environment friendly, burning, become the research direction of fire-retardant polyester fibre.
Can just the limited oxygen index (LOI) of polyester can be brought up to more than 28% in lower use amount although studies show that phosphonium flame retardant, but still have serious molten drop problem.Polyester fiber can produce the fusion dropping in combustion process, the personnel that cause scald or burn; The fusion dropping that has flame simultaneously also very easily causes electrical short-circuit or other article that ignite, and forms new ignition point, causes secondary disaster.With regard to present studies show that, still there is not real successful melt-drip resistant inflaming retarding polyester fiber both at home and abroad, this also becomes unsolved always international technical barrier.
The inorganic nano flame-retarded technology is noticeable in the achievement of improving the fusion drippage.By adding the inorganic combustion inhibitor powder of a large amount of (greater than 40wt%), can solve the fusion drippage problem of plastic product fully as magnesium hydroxide or aluminium hydroxide etc.But this method can't obtain to use in fiber, and its reason is that the inorganic combustion inhibitor powder can fusion in the fiberizing process, but exists with particle aggregate form, the rheological property of polymer and spinnability is brought have a strong impact on.Therefore, can't obtain melt-drip resistant inflaming retarding polyester fiber by adding a large amount of inorganic fire-retarded powders.
Polymer/inorganic phyllosilicate nano composite flame-proof material caused extensive concern in recent years.What inorganic laminated silicate utilized mainly that nature exists if you would take off clay minerals such as soil, kaolin, diatomite.CN101768342, CN 02133602.4, CN101805444A disclose adopting montmorillonite and Meccah stone has phosphorous copolyester/laminated nm-silicate composite material that flame resistance anti-thawing drips effect by the preparation of intercalation copolycondensation.Because the silicate lamella has iris action, the migration of the fused mass that produces in the time of can stopping burning delays the speed of extraneous oxygen to the combustion boundary internal migration simultaneously, therefore plays fire-retardant and slow down to melt the effect of dripping.But studies show that to have only the inorganic silicate lamella in matrix, to realize effectively peeling off evenly disperseing in a large number, could guarantee that material has good flame retardancy with nano-scale.Yet because huge surface area and relatively poor with the polymer phase capacitive, inorganic silicate is very easily reunited in matrix, forms the structural form that is separated, and not only flame retardant effect can not be given full play to, and also may the mechanical property of material be impacted.
(Phosphate glass, Pglass) hybrid material is the novel hybrid inorganic-organic materials of a class to polymer/phosphate glass.Pglass is formed by connecting by the oxo bridge key by some asymmetric phosphorus oxygen tetrahedrons, can make it have lower vitrification point (Tg) by structural design, makes it be fluid state in the processing temperature scope of many polymer.Therefore, can it be mixed in the high-molecular organic material, avoid inorganic object height addition and the processing problems brought with the processing method of traditional melt blending.Simultaneously, because polymer and phosphate glass work in-process all are fluids, in process, realize microscopic pattern regulation and control easily, thereby give the macro property of composite excellence Pglass.Some studies show that Pglass is uniformly dispersed in polymeric matrix, along with the addition raising of inorganic component, its microscopic pattern becomes strip shape from drop, and last and polymer forms inierpeneirating network structure.And make Pglass in PP, be orientated to sheet to the biaxial tension of discovering of PP/Pglass hybrid material, can increase substantially the barrier properties for gases of material.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of flame-retardant and anti-dripping polyester complex fiber, this method technology is simple, easily implement, copolyesters that makes and fiber thereof have good flame and anti-molten drop effect, the limited oxygen index of fabric is 29.8%～33.2%, do not have the fusion drippage during burning, have a good application prospect.
The preparation method of a kind of flame-retardant and anti-dripping polyester complex fiber of the present invention comprises:
(1) aromatic binary carboxylic acid, dihydroxylic alcohols and phosphonium flame retardant are mixed, add catalyst and heat stabilizer simultaneously, under 240～270 ℃, pressure 0～0.5MPa, reacted 2～5 hours, again reaction system was reacted 1.5～5 hours under 270～300 ℃ of vacuum, promptly get flame-proof copolyester; Wherein, the mol ratio of aromatic binary carboxylic acid and dihydroxylic alcohols is 1: 1.1-3.0, phosphonium flame retardant is the 3%-20% of aromatic binary carboxylic acid and dihydroxylic alcohols gross mass, catalyst is the 0.02%-0.1% of aromatic binary carboxylic acid quality, and heat stabilizer is the 0.02%-0.06% of aromatic binary carboxylic acid quality;
(2) be 40～65: 10～30 with mol ratio: 20～40 SnF
2, SnO, NH
4H
2PO
4Or P
2O
5At 400～500 ℃ of following fusion 60～90min, the cooling back promptly gets phosphate glass at 70-100 ℃ of following heat treatment 90～120min behind premixed 30～60min;
(3) above-mentioned flame-proof copolyester and phosphate glass 90: 10 by mass percentage～20: 80 are got flame-proof copolyester/phosphate glass 220～270 ℃ of following blend, be sandwich layer then with the flame-proof copolyester, be cortex, promptly get the flame-retardant and anti-dripping polyester complex fiber through melt spinning with flame-proof copolyester/phosphate glass.
Aromatic binary carboxylic acid in the described step (1) is terephthalic acid (TPA), M-phthalic acid or 2, the 6-naphthalenedicarboxylic acid.
Dihydroxylic alcohols in the described step (1) is ethylene glycol, butanediol or 1, ammediol.
Phosphonium flame retardant in the described step (1) is 9, the 10-dihydro-9-oxy is assorted-and the assorted luxuriant and rich with fragrance succinic acid of 10-phosphorus phthalein, 2-carboxyethyl phenyl phosphinic acid, two (4-carboxy phenyl) phenyl phosphine oxide, 2-carboxyethyl methylphosphinate phosphate or 2-carboxyethyl methylphosphinate phosphoric acid.
Catalyst in the described step (1) is Sb, Ti, Sn or Co compound.
Heat stabilizer in the described step (1) is trimethyl phosphate or triphenyl phosphate.
Melt-spinning technology parameter in the described step (3) is 260 ℃-300 ℃ of spinning temperatures, spinning speed 400-3200m/min, and 70 ℃-160 ℃ of drawing temperatures, drafting multiple 1-5 times, core-skin is than 10: 90-60: 40.
Novelty of the present invention is the phosphate glass that has different phosphate, fluorine content and vitrification point by MOLECULE DESIGN preparation, obtains the flame-proof copolyester/Pglass hybrid inorganic-organic materials of high content of phosphorus with the flame-proof copolyester blend; Be that sandwich layer, flame-proof copolyester/Pglass hybrid material are the fire resistance fibre of cortex by the composite spinning technology spinning with the flame-proof copolyester then.Utilize in the uniaxial tension process of fiber surface high content of phosphorus and fiberizing Pglass to form and have the laminated structure of iris action, flowing and migration of barrier polymers strand molten melt drop is accelerated into the charcoal process, plays the effect that fire-retardant and anti-fusion is dripped.
Beneficial effect
Technology of the present invention is simple, easily implements, and copolyesters that makes and fiber thereof have good flame and anti-molten drop effect, and the limited oxygen index of fabric is 29.8%～33.2%, does not have the fusion drippage during burning, has a good application prospect.
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.
Embodiment 1
250 gram terephthalic acid (TPA)s, 150 milliliters of ethylene glycol (99vol%) and 32 gram 2-carboxyethyl phenyl phosphinic acids are mixed, and the antimony glycol that adds 0.1 gram is a heat stabilizer as catalyst, 0.1 gram triphenyl phosphate.At 230 ℃, pressure is to carry out esterification under the 0.4MPa condition, carries out polycondensation reaction then under 260 ℃ of vacuum conditions, can obtain flame-proof copolyester.
With 100 gram SnF
2, 40 the gram SnO and 60 the gram P
2O
5Premixed 30min at 450 ℃ of following fusion 70min, is poured on the corrosion resistant plate subsequently and cools off then, at 90 ℃ of following heat treatment 90min, obtains phosphate glass at last.
Melt blending in twin-screw prepares flame-proof copolyester/phosphate glass hybrid material with 55% flame-proof copolyester and 45% phosphate glass (percentage by weight), and blending temperature is 230 ℃.
Flame-proof copolyester and phosphate glass are sandwich layer with the flame-proof copolyester after drying, are cortex with flame-proof copolyester/phosphate glass hybrid material, carry out melt spinning.Spinning temperature is 260 ℃, spinning speed 800m/min, and 70 ℃ of drawing temperatures, 3.3 times of drafting multiples, the core-skin ratio is 50: 50.System has good spinning properties, and the fracture strength of fiber is 3.04cN/dtex, and the limited oxygen index that is woven into fabric is 31.4%, does not have the fusion drippage during burning.
Embodiment 2
With 250 gram terephthalic acid (TPA)s, 170 milliliters of ethylene glycol (99vol%) and 40 grams 9, the 10-dihydro-9-oxy is assorted-the assorted luxuriant and rich with fragrance succinic acid of 10-phosphorus phthalein mixes, and it is heat stabilizer that the antimony glycol that adds 0.1 gram restrains triphenyl phosphate as catalyst, 0.1.At 280 ℃, pressure is to carry out esterification under the 0.1MPa condition, carries out polycondensation reaction then under 290 ℃ of high vacuum conditions, can obtain flame-proof copolyester.
With 90 gram SnF
2, 50 the gram SnO and 60 the gram P
2O
5Premixed 30min at 450 ℃ of following fusion 70min, is poured on the corrosion resistant plate subsequently and cools off then, at 90 ℃ of following heat treatment 90min, obtains phosphate glass at last.
Melt blending in twin-screw prepares flame-proof copolyester/phosphate glass hybrid material with 40% flame-proof copolyester and 60% phosphate glass (percentage by weight), and blending temperature is 270 ℃.
Flame-proof copolyester and phosphate glass are sandwich layer with the flame-proof copolyester after drying, are cortex with flame-proof copolyester/phosphate glass hybrid material, carry out melt spinning.Spinning temperature is 300 ℃, spinning speed 1200m/min, and 160 ℃ of drawing temperatures, 2.5 times of drafting multiples, the core-skin ratio is 20: 80.System has good spinning properties, and the fracture strength of fiber is 2.86cN/dtex, and the limited oxygen index that is woven into fabric is 33.2%, does not have the fusion drippage during burning.
Embodiment 3
250 gram terephthalic acid (TPA)s, 150 milliliters of ethylene glycol (99vol%) and 25 gram 2-carboxyethyl phenyl phosphinic acids are mixed, and the antimony glycol that adds 0.1 gram is a heat stabilizer as catalyst, 0.1 gram triphenyl phosphate.At 240 ℃, pressure is to carry out esterification under the 0.2MPa condition, carries out polycondensation reaction then under 280 ℃ of high vacuum conditions, can obtain flame-proof copolyester.
With 100 gram SnF
2, 40 the gram SnO and 95 the gram NH
4H
2PO
4Premixed 30min at 450 ℃ of following fusion 70min, is poured on the corrosion resistant plate subsequently and cools off then, at 90 ℃ of following heat treatment 90min, obtains phosphate glass at last.
Melt blending in twin-screw prepares flame-proof copolyester/phosphate glass hybrid material with 35% flame-proof copolyester and 65% phosphate glass (percentage by weight), and blending temperature is 260 ℃.
Flame-proof copolyester and phosphate glass are sandwich layer with the flame-proof copolyester after drying, are cortex with flame-proof copolyester/phosphate glass hybrid material, carry out melt spinning.Spinning temperature is 280 ℃, spinning speed 400m/min, and 100 ℃ of drawing temperatures, 3.3 times of drafting multiples, the core-skin ratio is 30: 70.System has good spinning properties, and the fracture strength of fiber is 2.78cN/dtex, and the limited oxygen index that is woven into fabric is 29.8%, does not have the fusion drippage during burning.
Embodiment 4
With 250 gram M-phthalic acids, 170 milliliters of butanediols (99vol%) and 30 grams 9, the 10-dihydro-9-oxy is assorted-the assorted luxuriant and rich with fragrance succinic acid of 10-phosphorus phthalein mixes, and it is heat stabilizer that the antimony glycol that adds 0.1 gram restrains triphenyl phosphate as catalyst, 0.1.At 270 ℃, pressure is to carry out esterification under the 0.4MPa condition, carries out polycondensation reaction then under 280 ℃ of high vacuum conditions, can obtain flame-proof copolyester.
With 105 gram SnF
2, 35 the gram SnO and 90 the gram NH
4H
2PO
4Premixed 50min at 400 ℃ of following fusion 70min, is poured on the corrosion resistant plate subsequently and cools off then, at 70 ℃ of following heat treatment 100min, obtains phosphate glass at last.
Melt blending in twin-screw prepares flame-proof copolyester/phosphate glass hybrid material with 70% flame-proof copolyester and 30% phosphate glass, and blending temperature is 260 ℃.
Flame-proof copolyester and phosphate glass are sandwich layer with the flame-proof copolyester after drying, are cortex with flame-proof copolyester/phosphate glass hybrid material, carry out melt spinning.Spinning temperature is 300 ℃, spinning speed 2500m/min, and 120 ℃ of drawing temperatures, 1.6 times of drafting multiples, the core-skin ratio is 30: 70.System has good spinning properties, and the fracture strength of fiber is 3.25cN/dtex, and the limited oxygen index that is woven into fabric is 30.1%, does not have the fusion drippage during burning.
Embodiment 5
250 gram terephthalic acid (TPA)s, 170 milliliters of ethylene glycol (99vol%) and two (4-carboxy phenyl) phenyl phosphine oxides of 40 grams are mixed, and the antimony glycol that adds 0.1 gram is a heat stabilizer as catalyst, 0.1 gram triphenyl phosphate.At 250 ℃, pressure is to carry out esterification under the 0.2MPa condition, carries out polycondensation reaction then under 290 ℃ of high vacuum conditions, can obtain flame-proof copolyester.
With 80 gram SnF
2, 40 the gram SnO and 110 the gram NH
4H
2PO
4Premixed 60min at 500 ℃ of following fusion 70min, is poured on the corrosion resistant plate subsequently and cools off then, at 100 ℃ of following heat treatment 120min, obtains phosphate glass at last.
Melt blending in twin-screw prepares flame-proof copolyester/phosphate glass hybrid material with 80% flame-proof copolyester and 20% phosphate glass, and blending temperature is 270 ℃.
Flame-proof copolyester and phosphate glass are sandwich layer with the flame-proof copolyester after drying, are cortex with flame-proof copolyester/phosphate glass hybrid material, carry out melt spinning.Spinning temperature is 260 ℃, spinning speed 1200m/min, and 110 ℃ of drawing temperatures, 2.5 times of drafting multiples, the core-skin ratio is 60: 40.System has good spinning properties, and the fracture strength of fiber is 2.65cN/dtex, and the limited oxygen index that is woven into fabric is 31.0%, does not have the fusion drippage during burning.
Claims (7)
1. the preparation method of a flame-retardant and anti-dripping polyester complex fiber comprises:
(1) aromatic binary carboxylic acid, dihydroxylic alcohols and phosphonium flame retardant are mixed, add catalyst and heat stabilizer simultaneously, under 240～270 ℃, pressure 0～0.5MPa, reacted 2～5 hours, again reaction system was reacted 1.5～5 hours under 270～300 ℃ of vacuum, promptly get flame-proof copolyester; Wherein, the mol ratio of aromatic binary carboxylic acid and dihydroxylic alcohols is 1: 1.1-3.0, phosphonium flame retardant is the 3%-20% of aromatic binary carboxylic acid and dihydroxylic alcohols gross mass, catalyst is the 0.02%-0.1% of aromatic binary carboxylic acid quality, and heat stabilizer is the 0.02%-0.06% of aromatic binary carboxylic acid quality;
(2) be 40～65: 10～30 with mol ratio: 20～40 SnF2, SnO, NH
4H
2PO
4Or P
2O
5At 400～500 ℃ of following fusion 60～90min, the cooling back promptly gets phosphate glass at 70-100 ℃ of following heat treatment 90～120min behind premixed 30～60min;
(3) above-mentioned flame-proof copolyester and phosphate glass 90: 10 by mass percentage～20: 80 are got flame-proof copolyester/phosphate glass 220～270 ℃ of following blend, be sandwich layer then with the flame-proof copolyester, be cortex, promptly get the flame-retardant and anti-dripping polyester complex fiber through melt spinning with flame-proof copolyester/phosphate glass.
2. the preparation method of a kind of flame-retardant and anti-dripping polyester complex fiber according to claim 1 is characterized in that: the aromatic binary carboxylic acid in the described step (1) is terephthalic acid (TPA), M-phthalic acid or 2, the 6-naphthalenedicarboxylic acid.
3. the preparation method of a kind of flame-retardant and anti-dripping polyester complex fiber according to claim 1 is characterized in that: the dihydroxylic alcohols in the described step (1) is ethylene glycol, butanediol or 1, ammediol.
4. the preparation method of a kind of flame-retardant and anti-dripping polyester complex fiber according to claim 1, it is characterized in that: the phosphonium flame retardant in the described step (1) is 9, the 10-dihydro-9-oxy is assorted-and the assorted luxuriant and rich with fragrance succinic acid of 10-phosphorus phthalein, 2-carboxyethyl phenyl phosphinic acid, two (4-carboxy phenyl) phenyl phosphine oxide, 2-carboxyethyl methylphosphinate phosphate or 2-carboxyethyl methylphosphinate phosphoric acid.
5. the preparation method of a kind of flame-retardant and anti-dripping polyester complex fiber according to claim 1 is characterized in that: the catalyst in the described step (1) is Sb, Ti, Sn or Co compound.
6. the preparation method of a kind of flame-retardant and anti-dripping polyester complex fiber according to claim 1 is characterized in that: the heat stabilizer in the described step (1) is trimethyl phosphate or triphenyl phosphate.
7. the preparation method of a kind of flame-retardant and anti-dripping polyester complex fiber according to claim 1, it is characterized in that: the melt-spinning technology parameter in the described step (3) is 260 ℃-300 ℃ of spinning temperatures, spinning speed 400-3200m/min, 70 ℃-160 ℃ of drawing temperatures, drafting multiple 1-5 times, core-skin is than 10: 90-60: 40.
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| CN112608461B (en) * | 2020-12-17 | 2021-08-17 | 上海思涛新材料科技有限公司 | Thermotropic flame-retardant anti-dripping aromatic liquid crystal copolyester and preparation method thereof |
| CN113445154A (en) * | 2021-07-19 | 2021-09-28 | 宁波华星科技有限公司 | Flame-retardant low-melting-point polyester fiber and preparation method thereof |
| CN113445154B (en) * | 2021-07-19 | 2023-03-14 | 宁波华星科技有限公司 | Flame-retardant low-melting-point polyester fiber and preparation method thereof |
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