CN104278349B - Antistatic-fire retardation copolyester fiber of one kind and preparation method thereof - Google Patents
Antistatic-fire retardation copolyester fiber of one kind and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to technical field of polymer materials, it is related to a kind of anti-electrostatic fire retardant copolyester fiber and preparation method thereof.The copolyester fiber is made of the component comprising following parts by weight：Poly terephthalic acid/100 parts of adipic acid fourth diester, 15 parts of polyethylene glycol, 0.2 1.3 parts of antistatic agent, 2 10 parts of phosphorus flame retardant, 0.1 4 parts of inorganic nanometer powder.The anti-electrostatic fire retardant copolyester fiber that the present invention obtains, intensity >=2.58cN/dtex, degree of stretching is and soft 30% or so, has good antistatic property, flame retardant property and mechanical property, is with a wide range of applications.
Description
Technical field
The invention belongs to technical field of polymer materials, it is related to a kind of polyester fiber and preparation method thereof.
Background technology
Polyester fiber is the current maximum synthetic fibers of yield in the world, has excellent comprehensive performance and wide application
Foreground, but polyester fiber is a kind of hydrophobic fiber, the volume resistivity under the status of criterion reaches 1013Ω cm or more,
Electrostatic is easy tod produce, and belongs to Flammable fibers, these reasons limit the application field of polyester fiber.
Japan Patent JP47-36459, which is related to a kind of use in aliphatic alcohol polyethenoxy phosphate, to be added in polyester resin
Obtained fiber, though antistatic property has persistent form, effect bad.Chinese patent 20110071051.X discloses one kind
Inorganic clay is dispersed into after the lamella of nano-scale and is copolymerized again by the preparation method of flame-retardant anti-dripping copolyester fibers in water.
This method has the defect for being difficult to overcome, and is unfavorable for large-scale industrial production.Chinese patent CN200410072375.5 is disclosed
A kind of manufacturing method of multi-functional PET staple fibers, by adding phosphorus flame retardant and inorganic anti-quiet in polyester polymerization process
Electric agent copolymerization has fire retardant-antistatic composite multifunction PET slices, then is spun into composite multifunction by this kind slice
Polyester staple fiber, but the bad control of its building-up process.
The fiber with complex function is made in polyester and phosphorus flame retardant, antistatic agent co-blended spinning by the present invention, to
Expand the purposes of the fibrous material.Simultaneously by lengthening cooling distance during the melt spinning of the present invention, to effective
It improves Direct-spinning of PET Fiber to be not easy to cool down in the process, is easy the problem of bonding, while also improving the comprehensive performance of material.
Invention content
It is an object of the invention to provide being total to for a kind of anti-flammability and antistatic property to overcome the deficiencies of existing technologies
Polyester fiber and preparation method thereof.
The present invention is modified for poly terephthalic acid/adipic acid fourth diester polyester fiber, is made it have good comprehensive
Performance is closed, its application field is widened, and method is simple, easy to operate, common terylene spinning equipment can be used, be not required to particular purchased
And transformation.
To achieve the goals above, the present invention uses following technical scheme：
A kind of copolyester fiber is made of the component comprising following parts by weight：
The structural formula of the poly terephthalic acid/adipic acid fourth diester is：
Polyadipate/the butylene terephthalate is random copolymerization, is made of above-mentioned two repetitive unit,
In, 1≤x≤50,1≤y≤50.
The molecular weight polyethylene glycol is 5000-20000.
The antistatic agent is anionic antistatic agents, the preferably antistatic agent containing organic sulfonic acid salt, general formula
For (R-SO3)nM, wherein R are C8-C18Straight chained alkyl or alkyl phenyl, M is alkali or alkaline earth metal ion, preferably Na,
K or Mg etc., n are 1 or 2.
The antistatic agent be neopelex, pentadecyl sulfonic acid sodium or sodium stearyl sulfonate, preferably
Neopelex.
Neopelex is white or pale yellow powder or graininess, molecular structural formula are：
The fire retardant be selected from 2- hydroxyethylbenzenes phosphoric acid, 2- hydroxyethyl methyls phosphate, 2- hydroxyethyl methyls phosphoric acid or
Bis- (p- carboxy phenyl) phenyl phosphine oxides（BCPPO）In one or more, corresponding structural formula is：
The inorganic nanometer powder be nano level silica, calcium carbonate or magnesium carbonate or one kind in barium sulfate or
More than one.
A kind of preparation method of above-mentioned copolyester fiber, includes the following steps：
（1）Poly terephthalic acid/adipic acid fourth diester, polyethylene glycol are dried in vacuo respectively, keep its moisture content small
In 200ppm；
（2）100 parts of poly terephthalic acids/adipic acid fourth diester, 1-5 parts of polyethylene glycol, 0.2-1.3 parts of anion are resisted quiet
Electric agent 2-10 parts of phosphorus flame retardants, 0.1-4 parts of inorganic nanometer powders carry out blending 3-10min, are carried out by screw type spinning-drawing machine
Melt spinning after cooling, is oiled, the processing of preliminary draft, winding, obtains the copolyester fiber that structure is uniform, fiber number is controllable；
（3）By step（2）In obtained copolyester fiber carry out drawing-off processing, obtain antistatic-fire retardation copolyester fiber.
The step（2）Spinning temperature be 250-290 DEG C, spinning speed 800-1200m/min.
The step（3）The processing multiplying power of middle traction processing is 1.5-3.5, and volume speed is 300-800m/min, processing temperature
Degree is 60-90 DEG C, wherein processing multiplying power refers to draft ratio.
A kind of preparation method of above-mentioned copolyester fiber, comprises the steps of：
（a）By 50 parts of poly terephthalic acids/adipic acid fourth diester, 1-5 parts of polyethylene glycol, 2-10 parts of phosphorus flame retardants and
0.1-4 parts of inorganic nanometer powders are squeezed out through double screw extruder, are granulated, and obtain polyethylene glycol/poly terephthalic acid adipic acid fourth
Two ester blends；
（b）By poly terephthalic acid/adipic acid fourth diester, step（1）Obtained polyethylene glycol/poly terephthalic acid oneself two
Two ester blend of sour fourth is dried in vacuo, and moisture is less than 200ppm after drying；
Take dry poly terephthalic acid/50 parts of adipic acid fourth diester, polyethylene glycol/poly terephthalic acid/adipic acid fourth
Two ester blends, 0.2-1.3 parts of anionic antistatic agents carry out blending 3-10min, and melting spinning is carried out by screw type spinning-drawing machine
Silk after cooling, is oiled, the processing of preliminary draft, winding, obtains the copolyester fiber that structure is uniform, fiber number is controllable；
（c）By step（b）In obtained fiber carry out drawing-off processing, obtain antistatic-fire retardation copolyester fiber.
The step（a）The extrusion temperature of middle double screw extruder is 120-170 DEG C.
The step（b）Spinning temperature be 250-290 DEG C, spinning speed 800-1200m/min.
The step（c）The multiplying power of middle traction processing is 1.5-3.5, and volume speed is 300-800m/min, drawing-off processing temperature
Degree is 60-90 DEG C.
Compared with prior art, the present invention has the following advantages：
There is the antistatic property fire-retardant polyester fibre obtained in the present invention elasticity, the fabric processed to have good anti-
It is the advantages that antistatic property, anti-flammability, heat resistance, washing fastness, soft, can be blended with cotton, wool fibre, and with good
Biological degradability.The preparation method is pollution-free, flow is short, efficient, high-quality, method is simple, is easy to industrialized production；Pass through
Cooling distance is lengthened, the problem that strand bonds in spinning process is effectively improved, obtains fibrous material of good performance；Polyester simultaneously
In nano material and fire retardant generate synergistic effect, reduce polyester fiber and injured caused by molten drop in burning.
Description of the drawings
Fig. 1 is the structural schematic diagram for implementing the spinning-drawing machine of the present invention
Attached drawing marks：
1 hopper, 2 screw rods,
3 babinets, 4 metering pumps,
5 spinnerets, 6 lengthen distance cooling,
7 boundling oiling devices, 8 take-up rolls.
Specific implementation method
With reference to specific embodiment, further illustrate the present invention.Poly terephthalic acid/adipic acid in the following example
The structural formula of fourth diester is：Gather oneself two
Acid/butylene terephthalate is random copolymerization, is made of above-mentioned two repetitive unit, wherein 1≤x≤50,1≤y≤50；
Molecular weight polyethylene glycol is 5000-20000.
Embodiment 1
（1）By poly terephthalic acid/adipic acid fourth diester, polyethylene glycol（Molecular weight is 5000）It is dry that vacuum is carried out respectively
Dry, moisture is less than 200ppm；
（2）By step（1）100 parts of poly terephthalic acids/adipic acid fourth diester, 1 part of polyethylene glycol after drying process,
0.2 part of neopelex, 2 parts of 2- hydroxyethylbenzenes phosphoric acid, 0.1 part of silica carry out blending 3min, pass sequentially through material
Bucket 1 enters double screw extruder, enters the babinet 3 of filament spinning component after melting extrusion through melt pipe under the action of screw rod 2, leads to
The metering of metering pump 4 is crossed, is squeezed out successively by spinneret 5, the cooling of cooling zone 6, boundling oiling device 7 is oiled, take-up roll 8 carries out
Preliminary draft and winding processing, obtain the copolyester fiber that structure is uniform, fiber number is controllable.Wherein, spinning temperature is 250 DEG C, spinning
Speed is 800m/min；Its fibre strength is 1.53cN/dtex, and degree of stretching is 140.6%, soft；
（3）By step（2）In obtained fiber carry out drawing-off processing, obtain antistatic-fire retardation copolyester fiber.Wherein,
It is 1.5 to process multiplying power, and volume speed is 300m/min, and drawing-off processing temperature is 60 DEG C.
Copolyester fiber good spinnability made from the present embodiment, the volume resistivity of fiber about 10 after drawing-off9Ω cm, pole
Limited oxygen index is 27.5, intensity 2.62cN/dtex, and feel is relatively soft.
Embodiment 2
（1）By poly terephthalic acid/adipic acid fourth diester, polyethylene glycol（Molecular weight is 10000）It is dried in vacuo, water
Divide and is less than 200ppm；
（2）By step（1）100 parts of poly terephthalic acids/adipic acid fourth diester, 2 parts of polyethylene glycol after drying process,
0.8 part of pentadecyl sulfonic acid sodium, 5 parts of 2- hydroxyethyl methyls phosphates, 1 part of calcium carbonate carry out blending 5min, pass sequentially through hopper 1
Into double screw extruder, enters the babinet 3 of filament spinning component after melting extrusion through melt pipe under the action of screw rod 2, pass through
Metering pump 4 measure, successively by spinneret 5 squeeze out, cooling zone 6 cooling, boundling oiling device 7 oiled, take-up roll 8 carry out it is pre-
Drawing-off and winding processing, obtain the biodegradable polyester fiber that structure is uniform, fiber number is controllable.Wherein, spinning temperature is 260 DEG C, is spun
Silk speed is 1000m/min.Its fibre strength is 1.41cN/dtex, and degree of stretching is 152.3%, soft.
（3）By step（2）In obtained fiber carry out drawing-off processing, obtain antistatic-fire retardation copolyester fiber.Wherein plus
Work multiplying power is 1.8, and volume speed is 400m/min, and drawing-off processing temperature is 75 DEG C.
Copolyester fiber good spinnability made from the present embodiment, the volume resistivity of fiber about 10 after drawing-off9Ω cm, pole
Limited oxygen index is 29, intensity 2.84cN/dtex, and feel is relatively soft.
Embodiment 3
（1）By 50 parts of poly terephthalic acids/adipic acid fourth diester, 3 parts of polyethylene glycol（Molecular weight is 15000）, 4 parts of 2- hydroxyls
Ethyl-methyl phosphoric acid and 2 parts of barium sulfate are squeezed out through double screw extruder, are granulated, obtain polyethylene glycol/poly terephthalic acid/oneself two
Two ester blend of sour fourth, processing temperature are 140 DEG C；
（2）By 50 parts of poly terephthalic acids/adipic acid fourth diester, step（1）Obtained polyethylene glycol/poly- terephthaldehyde
Acid/two ester blend of adipic acid fourth is dried in vacuo, and moisture is less than 200ppm.Take it is dry after 50 parts of poly terephthalic acids/
Adipic acid fourth diester and polyethylene glycol/two ester blend of poly terephthalic acid adipic acid fourth, 1.0 parts of neopelexes into
8min is blended in row, passes sequentially through hopper 1 and enters double screw extruder, through melt pipe after melting extrusion under the action of screw rod 2
It into the babinet 3 of filament spinning component, is measured, is squeezed out successively by spinneret 5, the cooling of cooling zone 6, boundling oil dress by metering pump 4
Set 7 oiled, take-up roll 8 carries out preliminary draft and winding processing, obtain the copolyester fiber that structure is uniform, fiber number is controllable.Its
In, spinning temperature is 270 DEG C, spinning speed 1200m/min.Its fibre strength is 1.48cN/dtex, and degree of stretching is 161.5%,
It is soft.
（3）By step（2）In obtained fiber carry out drawing-off processing, obtain antistatic-fire retardation copolyester fiber.Wherein,
It is 2.0 to process multiplying power, and volume speed is 600m/min, and drawing-off processing temperature is 70 DEG C.
Copolyester fiber good spinnability made from the present embodiment, the volume resistivity of fiber about 10 after drawing-off9Ω cm, pole
Limited oxygen index is 30.5, intensity 3.10cN/dtex, and feel is relatively soft.
Embodiment 4
（1）By 50 parts of poly terephthalic acids/adipic acid fourth diester, 5 parts of polyethylene glycol（Molecular weight is 20000）, 7 parts it is double
(p- carboxy phenyl) phenyl phosphine oxide and 2 parts of calcium carbonate, 2 parts of magnesium carbonate are squeezed out through double screw extruder, are granulated, and obtain poly- second two
Alcohol/two ester blend of poly terephthalic acid adipic acid fourth, processing temperature are 120 DEG C；
（2）By 50 parts of poly terephthalic acids/adipic acid fourth diester, step（1）Obtained polyethylene glycol/poly- terephthaldehyde
Acid/two ester blend of adipic acid fourth is dried in vacuo respectively, and moisture is less than 200ppm；Take 50 parts of poly- terephthaldehydes after drying
Acid/adipic acid fourth diester and polyethylene glycol/poly terephthalic acid/two ester blend of adipic acid fourth, 0.6 part of detergent alkylate sulphur
Sour sodium carries out blending 10min, passes sequentially through hopper 1 and enters double screw extruder, through molten after melting extrusion under the action of screw rod 2
Body pipeline enters the babinet 3 of filament spinning component, is measured by metering pump 4, is squeezed out successively by spinneret 5, cooling zone 6 cools down, boundling
Oiling device 7 is oiled, take-up roll 8 carries out preliminary draft and winding processing, and it is fine to obtain the copolyesters that structure is uniform, fiber number is controllable
Dimension.Wherein, spinning temperature is 280 DEG C, spinning speed 1100m/min.Its fibre strength is 1.85cN/dtex, and degree of stretching is
146.4%, it is soft.
（3）By step（2）In obtained fiber carry out drawing-off processing, obtain antistatic-fire retardation copolyester fiber.Wherein,
It is 2.2 to process multiplying power, and volume speed is 700m/min, and drawing-off processing temperature is 80 DEG C.
Copolyester fiber good spinnability made from the present embodiment, the volume resistivity of fiber about 10 after drawing-off9Ω cm, pole
Limited oxygen index is 31, intensity 3.49cN/dtex, and feel is relatively soft.
Embodiment 5
（1）By 50 parts of poly terephthalic acids/adipic acid fourth diester, 4 parts of polyethylene glycol（Molecular weight is 18000）, 4 parts of 2- hydroxyls
Ethyl benzenephosphonic acid, 6 parts of 2- hydroxyethyl methyls phosphates and 2.5 parts of silica are squeezed out through double screw extruder, are granulated, and are gathered
Ethylene glycol/poly terephthalic acid/two ester blend of adipic acid fourth, processing temperature are 170 DEG C；
（2）By 50 parts of poly terephthalic acids/adipic acid fourth diester, step（1）Obtained polyethylene glycol/poly- terephthaldehyde
Acid/two ester blend of adipic acid fourth is dried in vacuo respectively, and moisture is less than 200ppm；Take 50 parts of poly- terephthaldehydes after drying
Acid/adipic acid fourth diester and polyethylene glycol/poly terephthalic acid/two ester blend of adipic acid fourth, 1.3 parts of sodium stearyl sulfonates
Blending 6min is carried out, hopper 1 is passed sequentially through and enters double screw extruder, through melt pipe after melting extrusion under the action of screw rod 2
Road enters the babinet 3 of filament spinning component, is measured by metering pump 4, is squeezed out successively by spinneret 5, cooling zone 6 cools down, boundling oils
Device 7 is oiled, take-up roll 8 carries out preliminary draft and winding processing, and it is fine to obtain the degradable polyester that structure is uniform, fiber number is controllable
Dimension.Wherein, spinning temperature is 290 DEG C, spinning speed 900m/min.Its fibre strength is 1.50cN/dtex, and degree of stretching is
155.2%, it is soft.
（3）By step（2）In obtained fiber carry out drawing-off processing, obtain antistatic-fire retardation copolyester fiber.Wherein,
It is 3.5 to process multiplying power, and volume speed is 800m/min, and drawing-off processing temperature is 90 DEG C.
Copolyester fiber good spinnability made from the present embodiment, the volume resistivity of fiber about 10 after drawing-off9Ω cm, pole
Limited oxygen index is 32, intensity 3.35cN/dtex, and feel is relatively soft.
By above example result it is found that antistatic-fire retardation copolyester fiber that the present invention obtains, volume resistivity
109Ω cm or so, limit oxygen index is 27 or more, intensity >=2.58cN/dtex, and soft, has good
Antistatic property, flame retardant property and mechanical property, be with a wide range of applications.
This hair can be understood and applied the above description of the embodiments is intended to facilitate those skilled in the art
It is bright.Person skilled in the art obviously easily can make various modifications to these embodiments, and described herein
General Principle is applied in other embodiment without having to go through creative labor.Therefore, the present invention is not limited to implementations here
Example, those skilled in the art's announcement according to the present invention, improvement and modification made without departing from the scope of the present invention all should be
Within protection scope of the present invention.
Claims (8)
1. a kind of copolyester fiber, it is characterised in that：It is made of the component of following parts by weight：
The structural formula of the poly terephthalic acid/adipic acid fourth diester is：
The poly terephthalic acid/adipic acid fourth diester is random copolymerization, is made of above-mentioned two repetitive unit, wherein 1≤
X≤50,1≤y≤50；
The molecular weight polyethylene glycol is 5000-20000；
The antistatic agent is neopelex, pentadecyl sulfonic acid sodium or sodium stearyl sulfonate；
The fire retardant is selected from 2- hydroxyethylbenzenes phosphoric acid, 2- hydroxyethyl methyls phosphate, 2- hydroxyethyl methyls phosphoric acid or double
One or more of (p- carboxy phenyl) phenyl phosphine oxide；
The inorganic nanometer powder is nano level silica, calcium carbonate or one or more of magnesium carbonate or barium sulfate.
2. a kind of preparation method of copolyester fiber described in claim 1, it is characterised in that：Include the following steps：
(1) poly terephthalic acid/adipic acid fourth diester, polyethylene glycol are dried in vacuo respectively, its moisture content is made to be less than
200ppm；
(2) by 100 parts of poly terephthalic acids/adipic acid fourth diester, 1-5 parts of polyethylene glycol, 0.2-1.3 parts of 2-10 parts of antistatic agents
Phosphorus flame retardant, 0.1-4 part inorganic nanometer powder carry out blending 3-10min, and melt spinning is carried out by screw type spinning-drawing machine, cold
But it after, is oiled, the processing of preliminary draft, winding, obtains the copolyester fiber that structure is uniform, fiber number is controllable；
(3) copolyester fiber obtained in step (2) is subjected to drawing-off processing, obtains antistatic-fire retardation copolyester fiber；
The antistatic agent is neopelex, pentadecyl sulfonic acid sodium or sodium stearyl sulfonate.
3. preparation method according to claim 2, it is characterised in that：The spinning temperature of the step (2) is 250-290
DEG C, spinning speed 800-1200m/min.
4. preparation method according to claim 2, it is characterised in that：The processing times of traction processing in the step (3)
Rate is 1.5-3.5, and volume speed is 300-800m/min, and processing temperature is 60-90 DEG C, wherein processing multiplying power refers to draft ratio.
5. a kind of preparation method of copolyester fiber described in claim 1, it is characterised in that：It comprises the steps of：
(a) by 50 parts of poly terephthalic acids/adipic acid fourth diester, 1-5 parts of polyethylene glycol, 2-10 parts of phosphorus flame retardants and 0.1-4
Part inorganic nanometer powder is squeezed out through double screw extruder, is granulated, and it is total to obtain polyethylene glycol/poly terephthalic acid adipic acid fourth diester
Mixed object；
(b) polyethylene glycol for obtaining poly terephthalic acid/adipic acid fourth diester, step (a)/poly terephthalic acid adipic acid fourth
Two ester blends are dried in vacuo, and moisture is less than 200ppm after drying；
Take dry poly terephthalic acid/50 parts of adipic acid fourth diester, polyethylene glycol/poly terephthalic acid/adipic acid fourth diester
Blend, 0.2-1.3 parts of antistatic agent carry out blending 3-10min, and melt spinning is carried out by screw type spinning-drawing machine, after cooling,
It is oiled, the processing of preliminary draft, winding, obtains the copolyester fiber that structure is uniform, fiber number is controllable；
(c) fiber obtained in step (b) is subjected to drawing-off processing, obtains antistatic-fire retardation copolyester fiber；
The antistatic agent is neopelex, pentadecyl sulfonic acid sodium or sodium stearyl sulfonate.
6. preparation method according to claim 5, it is characterised in that：Double screw extruder squeezes in the step (a)
It is 120-170 DEG C to go out temperature.
7. preparation method according to claim 5, it is characterised in that：The spinning temperature of the step (b) is 250-290
DEG C, spinning speed 800-1200m/min.
8. preparation method according to claim 5, it is characterised in that：The multiplying power of traction processing is in the step (c)
1.5-3.5, volume speed are 300-800m/min, and drawing-off processing temperature is 60-90 DEG C.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105350109B (en) * | 2015-11-13 | 2017-08-22 | 深圳市名仕度服饰有限公司 | A kind of poly- phosphamide fiber and its fusion method preparation 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 |
| WO2017176604A1 (en) * | 2016-04-06 | 2017-10-12 | Ascend Performance Materials Operations Llc | Light color /low resistance anti-static fiber and textiles incorporating the fiber |
| CN105780260B (en) * | 2016-04-29 | 2018-11-13 | 绍兴思安阻燃科技有限公司 | PSA fiber flame-retardant blended fabric |
| 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 |
| CN106521691B (en) * | 2016-11-16 | 2018-09-25 | 汕头市东华铖织造有限公司 | Polyester fiber with flame-proof antibiotic characteristic and its application |
| CN107119341A (en) * | 2017-04-21 | 2017-09-01 | 常熟涤纶有限公司 | A kind of fire-retardant Biodegradable fibers |
| CN112127005A (en) * | 2020-10-10 | 2020-12-25 | 杭州成江纺织有限公司 | Polyester filament yarn and preparation process thereof |
| CN112760982A (en) * | 2020-12-28 | 2021-05-07 | 安徽省天助纺织科技集团股份有限公司 | High-flame-retardant antistatic yarn and processing method thereof |
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Denomination of invention: Antistatic and flame retardant copolyester fiber and preparation method thereof Effective date of registration: 20191202 Granted publication date: 20180918 Pledgee: Chuzhou economic and Technological Development Corporation Pledgor: Shanghai Jieshijie New Materials (Group) Co., Ltd. Registration number: Y2019980000815 |