CN104120505A - Inflaming retarding modified PBT (Polybutylene Terephthalate) fiber and preparation method thereof - Google Patents
Inflaming retarding modified PBT (Polybutylene Terephthalate) fiber and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the field of fiber preparation and relates to an inflaming retarding PBT (Polybutylene Terephthalate) fiber and a preparation method thereof. The inflaming retarding PBT fiber is prepared from the following components in parts by mass: 42-65 parts of terephthalic acid, 35-58 parts of butanediol, 0.008-1.3 parts of a catalyst, 0-0.5 part of a stabilizing agent, 5-10 parts of a phosphorus based flame retardant and 0.1-10 parts of an inorganic nano material. Compared with the prior art, the preparation method is simple and is easy to operate; a textile processed by the fiber has the advantages of good fire resistance, heat resistance, washing durability and the like; meanwhile, the phosphorus based flame retardant and the inorganic nano material are added to achieve a synergic inflaming retarding effect; the inorganic nano material is added so that polyester is good in spinnability, fiber forming property and heat stability.
Description
Invention field
The invention belongs to fiber preparation field, relate to a kind of modified PBT (polybutylene terephthalate (PBT)) fiber and preparation method thereof.
Technical background
Polyester fiber has that intensity is high, good springiness, wrinkle resistance is strong, ABRASION RESISTANCE is good and excellent features such as heat resistance.Therefore, no matter civilian and industrial being widely used, be, a kind of comparatively desirable textile material.Polyester fiber is the kind that in synthetic fiber, output is maximum, purposes is the widest at present, due to its good mechanical performance and tensile property, is widely used in fields such as dress ornament, industry, good logical transportation, ornament materials.But, polyester fiber belongs to flammable fiber, along with the expansion of its Application Areas, in the use occasion of some special dimension, such as the ornament materials of military affairs, aviation, communications and transportation, public place of entertainment, hospital etc., fire fighting device etc., need the fire-retardant requirement that reaches certain.The fire that the whole world causes because fibrous material is inflammable has every year caused huge economic loss.
In recent years, along with a large amount of uses of polyester fiber, people conduct in-depth research the flame retardant type of polyester fiber.Multiple fire retardant and flame treatment way have been developed.At present, the fire retardant having utilized has halogen contained compound, metal oxide mixture, nitrogen-containing compound, phosphorus-containing compound and analog etc.But the fire-retardant polyester fibre of halogen-containing flame retardant easily discharges irritant and corrosive toxic hydrogen halide and cigarette when burning, harm environment, thereby restriction has been received in its use; And this based flame retardant of metal oxide is mainly used in plastics flame retardant polyester; When using phosphorus flame retardant, also exist some heat endurances to reduce, the color and luster variation of polyester fiber, the problems such as product flavescence, affect the quality of final products.
Chinese patent 200780047558.3 discloses a kind of fire-retardant polyester fibre and preparation method thereof, by warping in independent drawing device, do not draw the fiber of heat treatment for drawing in fiber, make the fiber making show low thermal stress and heat is had to good shape stability.But the method more complicated is higher to equipment requirement, is unfavorable for suitability for industrialized production.Chinese patent 20110071051.X discloses a kind of preparation method of flame-retardant anti-dripping copolyester fibers, inorganic clay is dispersed in water to copolymerization again after the lamella of nano-scale.The method has the defect that is difficult to overcome, and is unfavorable for large-scale industrial production.
Polyester fiber of the present invention, due to the introducing of phosphorus flame retardant, gives polyester fiber good lasting fire resistance; Add inorganic nano material simultaneously, can effectively improve resistance to melt-dropping property and the spinning property of material.Phosphorus flame retardant and inorganic nano material are used in conjunction with, make material in the situation that using less additive, effectively improve the fire resistance of material, the Application Areas of having widened polyester fiber.
Summary of the invention
The object of the present invention is to provide a kind of good spinnability, Product Safety high, excellent performance and prepare easy flame-retardant modified PBT fiber and preparation method thereof.
To achieve these goals, the present invention is by the following technical solutions:
A modified PBT fiber, by the component that comprises following parts by mass, made:
Terephthalic acid (TPA) 42-65 part,
Butanediol 35-58 part,
Catalyst 0.008-1.3 part,
Stabilizing agent 0-0.5 part,
Phosphorus flame retardant 5-10 part,
Inorganic nano material 0.1-10 part.
Described catalyst is selected from one or more in acetate or titanium compound, is further selected from calcium acetate, zinc acetate, tetraethyl titanate, metatitanic acid four n-propyls or tetra-n-butyl titanate, preferably tetra-n-butyl titanate.
Described stabilizing agent is selected from one or more in triphenyl phosphite, Trimethyl phosphite, tricresyl phosphite certain herbaceous plants with big flowers ester, trimethyl phosphate or triphenyl phosphate, preferably phosphoric acid trimethyl or triphenyl phosphate.
Described phosphorus flame retardant is one or more in 2-hydroxyethylbenzene phosphoric acid, 2-ethoxy methyl phosphorodithioate or 2-ethoxy methyl acid phosphate, and its corresponding structural formula is:
2-hydroxyethylbenzene phosphoric acid 2-ethoxy methyl phosphorodithioate
2-ethoxy methyl acid phosphate
Described inorganic nano material is one or more in silica, magnesium hydroxide, aluminium hydroxide or zirconium hydroxide, is individual particle dispersity, and particle diameter is less than 100nm.
A preparation method for above-mentioned modified PBT fiber, comprises the following steps:
(1) 42-65 part terephthalic acid (TPA), 35-58 part butanediol and 0.008-1.3 part catalyst are joined to reactor and react, then insulation;
(2) add 0-0.5 part stabilizing agent, 5-10 part phosphorus flame retardant and 0.1-10 part inorganic nano material, then vacuumize polycondensation, obtain PBT polyester;
(3) flame retardant polyester that step (1) obtained carries out melt spinning through screw type spinning machine, cooling after, oil, preliminary draft, coiling, drawing-off process, and obtains even structure, the controlled fire-retardant polyester fibre of fiber number.
In described step (1), reaction temperature is 190-240 ℃, until cut goes out the total amount of water, reaches the more than 90% of theoretical value, is then incubated half an hour.
In described step (2), the temperature of polycondensation reaction is 240-270 ℃, and the reaction time is 2-5h; When the viscosity of polymer is 0.6-0.95 scope, finish reaction.
The spinning temperature of described step (3) is 240-270 ℃, and spinning speed is 800-2000m/min.
The multiplying power that the traction of described step (3) is processed is 1.5-3, and processing temperature is 60-90 ℃.
The fire resistance fibre of producing with additive method (post treatment method, blending modification method etc.) by copolymerization flame retardant products is compared, and low molecule is inorganic or organic matter is few, and fire resistance is more excellent.
Flame retardant polyester and fiber are mainly to adopt addition type or reactive flame retardant at present, and obtain good flame retardant effect needs the addition of fire retardant larger, can cause like this problem of some environment.Organic fire-resisting polyester has good flame retardant effect, but when burning there will be more serious melting drip phenomenon, polyester to have fire-retardant and refractory simultaneously, drips the focus that function is research in world wide.
The present invention improves the fire resistance of polyester by adding phosphorus flame retardant and inorganic nano material, large usage quantity when using separately, by several while using simultaneously, can make fire resistance separately give full play of, can integrate the flame retardant efficiency of different materials again, make that it is had complementary advantages, cooperative flame retardant, only can also play under the addition of lower fire retardant, just promote significantly the effect of the fire resistance of polyester material.In the production process of polyester, add nano inorganic material, make polyester there is good spinnability performance, and there is good fibre-forming performance and heat endurance simultaneously.
Compared with prior art, the present invention has following beneficial effect:
The fire-retardant polyester fibre obtaining in the present invention, has good bulkiness, feel is good, has overcome stiff, the stiff sensation of general inflaming retarding fabric, obtains better application weaving in the safety article such as old young dress ornament.Production method is simple, easy to operate simultaneously, and the fabric processing has the advantages such as good anti-flammability, heat resistance, washing resistance.The fiber that this method obtains can be widely used in products such as producing high-grade bunting, nonwoven fabric, frock cloth, carpet, ornament materials, has the features such as nontoxic, anti-flammability is lasting.
The present invention is directed to PBT polyester fiber and carry out modification, make it have good fire resistance, widen its Application Areas, and method is simple, easy to operate, can use conventional Direct-spinning of PET Fiber equipment, do not need particular purchased and transformation.
The specific embodiment
Below in conjunction with specific embodiment, further illustrate the present invention.
The present invention's terephthalic acid (TPA) used, butanediol are all purchased from Shanghai Cao Shi chemical science and technology Development Co., Ltd, technical grade.If no special instructions, the raw material in following each embodiment is in parts by mass.
Embodiment 1
(1) 55 parts of terephthalic acid (TPA)s, 45 parts of butanediols and 0.4 part of tetraethyl titanate of catalyst are joined in 2L reactor and reacted with 230 ℃, until cut goes out the total amount of water, reach the more than 90% of theoretical value, insulation half an hour;
(2) (filler is individual particle dispersity to add 2 parts, 0.1 part of stabilizing agent triphenyl phosphate, 5 parts of 2-hydroxyethylbenzene phosphoric acid, 1 part of magnesium hydroxide and aluminium hydroxide, particle diameter is less than 100nm), then vacuumize polycondensation, the temperature of polycondensation reaction is controlled at 260 ℃, and the time is 2h; When the viscosity of polymer is 0.6-0.95 scope, can finish reaction, obtain flame retardant polyester.
(3) flame retardant polyester that step (2) obtained carries out melt spinning through screw type spinning machine, cooling after, oil, preliminary draft, coiling, drawing-off process, and obtains even structure, the controlled fire-retardant polyester fibre of fiber number.Wherein, spinning temperature is 250 ℃, and spinning speed is 800m/min; The processing multiplying power of drawing-off is 2.1, and processing temperature is 70 ℃.
The fire-retardant polyester fibre good spinnability that the present embodiment obtains, intensity is 3.25cN/dtex, limited oxygen index is 29.
Embodiment 2
(1) 42 parts of terephthalic acid (TPA)s, 57 parts of butanediols and 0.008 part of zinc acetate of catalyst are joined in 2L reactor in 190 ℃ and react, until cut goes out the total amount of water, reach the more than 90% of theoretical value, insulation half an hour;
(2) add 6 parts of 2-ethoxy methyl phosphorodithioates, 2 parts of silica, 2 parts of magnesium hydroxides, 1 part of zirconium hydroxide, then vacuumize polycondensation, the temperature of polycondensation reaction is controlled at 240 ℃, and the time is 5h.When the viscosity of polymer is 0.6-0.95 scope, can finish reaction, obtain flame retardant polyester.
(3) flame retardant polyester that step (2) obtained carries out melt spinning through screw type spinning machine, cooling after, oil, preliminary draft, coiling, drawing-off process, and obtains even structure, the controlled fire-retardant polyester fibre of fiber number.Wherein, spinning temperature is 240 ℃, and spinning speed is 1000m/min; The processing multiplying power of drawing-off is 1.5, and processing temperature is 60 ℃.
The fire-retardant polyester fibre good spinnability that the present embodiment obtains, intensity is 2.89cN/dtex, limited oxygen index is 30.5.
Embodiment 3
(1) 60 parts of terephthalic acid (TPA)s, 40 parts of butanediols and 0.8 part of calcium acetate of catalyst are joined in 2L reactor and reacted with 240 ℃, until cut goes out the total amount of water, reach the more than 90% of theoretical value, insulation half an hour;
(2) add 0.2 part of stabilizing agent trimethyl phosphate, 2-hydroxyethylbenzene phosphatase 24 part, 4 parts of 2-ethoxy methyl phosphorodithioates, 0.1 part of silica, then vacuumize polycondensation, the temperature of polycondensation reaction is controlled at 270 ℃, and the time is 3h.When the viscosity of polymer is 0.6-0.95 scope, can finish reaction, obtain flame retardant polyester.
(3) flame retardant polyester that step (2) obtained carries out melt spinning through screw type spinning machine, cooling after, oil, preliminary draft, coiling, drawing-off process, and obtains even structure, the controlled fire-retardant polyester fibre of fiber number.Wherein, spinning temperature is 270 ℃, and spinning speed is 1200m/min; The processing multiplying power of drawing-off is 1.8, and processing temperature is 80 ℃.
The fire-retardant polyester fibre good spinnability that the present embodiment obtains, intensity is 2.98cN/dtex, limited oxygen index is 27.
Embodiment 4
(1) 65 parts of terephthalic acid (TPA)s, 35 parts of butanediols and 1.3 parts of tetra-n-butyl titanates of catalyst are joined in 2L reactor and reacted with 210 ℃, until cut goes out the total amount of water, reach the more than 90% of theoretical value, insulation half an hour;
(2) add 0.3 part of stabilizing agent tricresyl phosphite certain herbaceous plants with big flowers ester, 7 parts of 2-ethoxy methyl acid phosphates, 4 parts of magnesium hydroxides, 6 parts, aluminium hydroxide, then vacuumize polycondensation, the temperature of polycondensation reaction is controlled at 250 ℃, and the time is 4h; When the viscosity of polymer is 0.6-0.95 scope, can finish reaction, obtain flame retardant polyester.
(3) flame retardant polyester that step (2) obtained carries out melt spinning through screw type spinning machine, cooling after, oil, preliminary draft, coiling, drawing-off process, and obtains even structure, the controlled fire-retardant polyester fibre of fiber number.Wherein, spinning temperature is 250 ℃, and spinning speed is 2000m/min; The processing multiplying power of drawing-off is 2.5, and processing temperature is 90 ℃.
The fire-retardant polyester fibre good spinnability that the present embodiment obtains, intensity is 3.89cN/dtex, limited oxygen index is 31.
Embodiment 5
(1) 48 parts of terephthalic acid (TPA)s, 52 parts of butanediols and 0.2 part of metatitanic acid four n-propyl of catalyst are joined in 2L reactor and reacted with 220 ℃, until cut goes out the total amount of water, reach the more than 90% of theoretical value, insulation half an hour;
(2) add 4 parts, 0.5 part of stabilizing agent triphenyl phosphite, 10 parts of 2-ethoxy methyl acid phosphates, 3 parts of magnesium hydroxides and aluminium hydroxide, then vacuumize polycondensation, the temperature of polycondensation reaction is controlled at 265 ℃, and the time is 3.5h; When the viscosity of polymer is 0.6-0.95 scope, can finish reaction, obtain flame retardant polyester;
(3) flame retardant polyester that step (2) obtained carries out melt spinning through screw type spinning machine, cooling after, oil, preliminary draft, coiling, drawing-off process, and obtains even structure, the controlled fire-retardant polyester fibre of fiber number.Wherein, spinning temperature is 265 ℃, and spinning speed is 1600m/min.The processing multiplying power of drawing-off is 3, and processing temperature is 75 ℃.
The fire-retardant polyester fibre good spinnability that the present embodiment obtains, intensity is 3.91cN/dtex, limited oxygen index is 33.
Known by above embodiment result, the fire-retardant polyester fibre that the present invention obtains, its fire resistance is good, its limited oxygen index is all more than 27, and intensity >=2.5cN/dtex is soft, there is good fire resistance and mechanical property, be with a wide range of applications.
The above-mentioned description to embodiment is can understand and apply the invention for ease of those skilled in the art.Person skilled in the art obviously can easily make various modifications to these embodiment, and General Principle described herein is applied in other embodiment and needn't passes through performing creative labour.Therefore, the invention is not restricted to the embodiment here, those skilled in the art are according to announcement of the present invention, and not departing from the improvement that category of the present invention makes and revise all should be within protection scope of the present invention.
Claims (10)
1. a polybutylene terephthalate (PBT) fiber, is characterized in that: by the component that comprises following parts by mass, made:
Terephthalic acid (TPA) 42-65 part,
Butanediol 35-58 part,
Catalyst 0.008-1.3 part,
Stabilizing agent 0-0.5 part,
Phosphorus flame retardant 5-10 part,
Inorganic nano material 0.1-10 part.
2. polybutylene terephthalate (PBT) fiber according to claim 1, it is characterized in that: described catalyst is selected from one or more in acetate or titanium compound, further be selected from calcium acetate, zinc acetate, tetraethyl titanate, metatitanic acid four n-propyls or tetra-n-butyl titanate, preferably tetra-n-butyl titanate.
3. polybutylene terephthalate (PBT) fiber according to claim 1, it is characterized in that: described stabilizing agent is selected from one or more in triphenyl phosphite, Trimethyl phosphite, tricresyl phosphite certain herbaceous plants with big flowers ester, trimethyl phosphate or triphenyl phosphate, preferably phosphoric acid trimethyl or triphenyl phosphate.
4. polybutylene terephthalate (PBT) fiber according to claim 1, is characterized in that: described phosphorus flame retardant is one or more in 2-hydroxyethylbenzene phosphoric acid, 2-ethoxy methyl phosphorodithioate or 2-ethoxy methyl acid phosphate.
5. polybutylene terephthalate (PBT) fiber according to claim 1, it is characterized in that: described inorganic nano material is one or more in silica, magnesium hydroxide, aluminium hydroxide or zirconium hydroxide, be individual particle dispersity, particle diameter is less than 100nm.
6. a preparation method for arbitrary described polybutylene terephthalate (PBT) fiber in claim 1-5, is characterized in that: comprise the following steps:
(1) 42-65 part terephthalic acid (TPA), 35-58 part butanediol and 0.008-1.3 part catalyst are joined to reactor and react, then insulation;
(2) add 0-0.5 part stabilizing agent, 5-10 part phosphorus flame retardant and 0.1-10 part inorganic nano material, then vacuumize polycondensation, obtain PBT polyester;
(3) flame retardant polyester that step (1) obtained carries out melt spinning through screw type spinning machine, cooling after, oil, preliminary draft, coiling, drawing-off process, and obtains even structure, the controlled fire-retardant polyester fibre of fiber number.
7. preparation method according to claim 6, is characterized in that: in described step (1), reaction temperature is 190-240 ℃, until cut goes out the total amount of water, reaches the more than 90% of theoretical value, is then incubated half an hour.
8. preparation method according to claim 6, is characterized in that: in described step (2), the temperature of polycondensation reaction is 240-270 ℃, and the reaction time is 2-5h; When the viscosity of polymer is 0.6-0.95 scope, finish reaction.
9. preparation method according to claim 6, is characterized in that: the spinning temperature of described step (3) is 240-270 ℃, and spinning speed is 800-2000m/min.
10. preparation method according to claim 6, is characterized in that: the multiplying power that the traction of described step (3) is processed is 1.5-3, and processing temperature is 60-90 ℃.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105088383A (en) * | 2015-09-02 | 2015-11-25 | 太仓市宏亿化纤有限公司 | PBT (polybutylene terephthalate) fiber production technology |
| CN105113046A (en) * | 2015-09-02 | 2015-12-02 | 太仓市宏亿化纤有限公司 | Production process of modified halogen-free flame retardant PBT |
| CN105624825A (en) * | 2016-03-15 | 2016-06-01 | 张家港骏马无纺布有限公司 | Flame-retardant melt-blowing nonwoven material and preparation method thereof |
| CN105908284A (en) * | 2016-06-13 | 2016-08-31 | 常熟市欧西依织造有限公司 | Environment-friendly flame-retardant polyester fiber |
| CN105951206A (en) * | 2016-06-27 | 2016-09-21 | 仪征盛大纺织新材料有限公司 | Anti-electrostatic modified PBT fiber |
| CN105970340A (en) * | 2016-06-27 | 2016-09-28 | 仪征盛大纺织新材料有限公司 | Preparation method of antistatic modified PBT fiber |
| CN106087101A (en) * | 2016-06-13 | 2016-11-09 | 常熟市欧西依织造有限公司 | A kind of fire-resistant antistatic polyester fiber |
| CN106835339A (en) * | 2017-01-11 | 2017-06-13 | 福建百宏聚纤科技实业有限公司 | Flame retardant polyester polyester filament |
| CN108085779A (en) * | 2017-12-12 | 2018-05-29 | 马鞍山市鑫程纳米新材料科技有限公司 | A kind of preparation method of heat resistant type non-woven fabrics |
| CN117551338A (en) * | 2024-01-12 | 2024-02-13 | 北京慕湖新材料技术有限公司 | Flame-retardant cold-resistant and damp-heat-resistant polyester composition and preparation method thereof |
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| CN106835339A (en) * | 2017-01-11 | 2017-06-13 | 福建百宏聚纤科技实业有限公司 | Flame retardant polyester polyester filament |
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| CN108085779A (en) * | 2017-12-12 | 2018-05-29 | 马鞍山市鑫程纳米新材料科技有限公司 | A kind of preparation method of heat resistant type non-woven fabrics |
| CN117551338A (en) * | 2024-01-12 | 2024-02-13 | 北京慕湖新材料技术有限公司 | Flame-retardant cold-resistant and damp-heat-resistant polyester composition and preparation method thereof |
| CN117551338B (en) * | 2024-01-12 | 2024-03-26 | 北京慕湖新材料技术有限公司 | Flame-retardant cold-resistant and damp-heat-resistant polyester composition and preparation method thereof |
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Application publication date: 20141029 |