CN106811820B - A kind of preparation method of fire-retardant anti-molten droplet fiber - Google Patents
A kind of preparation method of fire-retardant anti-molten droplet fiber Download PDFInfo
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- CN106811820B CN106811820B CN201610204307.2A CN201610204307A CN106811820B CN 106811820 B CN106811820 B CN 106811820B CN 201610204307 A CN201610204307 A CN 201610204307A CN 106811820 B CN106811820 B CN 106811820B
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 55
- 239000000835 fiber Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 24
- 239000004594 Masterbatch (MB) Substances 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 12
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000000843 powder Substances 0.000 claims abstract description 8
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 14
- 229910021389 graphene Inorganic materials 0.000 claims description 11
- 239000004952 Polyamide Substances 0.000 claims description 6
- 229920002647 polyamide Polymers 0.000 claims description 6
- ZQKXQUJXLSSJCH-UHFFFAOYSA-N melamine cyanurate Chemical compound NC1=NC(N)=NC(N)=N1.O=C1NC(=O)NC(=O)N1 ZQKXQUJXLSSJCH-UHFFFAOYSA-N 0.000 claims description 4
- 238000010035 extrusion spinning Methods 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- XZMCDFZZKTWFGF-UHFFFAOYSA-N Cyanamide Chemical compound NC#N XZMCDFZZKTWFGF-UHFFFAOYSA-N 0.000 claims 1
- 150000001408 amides Chemical class 0.000 claims 1
- ZFSLODLOARCGLH-UHFFFAOYSA-N isocyanuric acid Chemical compound OC1=NC(O)=NC(O)=N1 ZFSLODLOARCGLH-UHFFFAOYSA-N 0.000 claims 1
- 238000009987 spinning Methods 0.000 abstract description 16
- 239000003795 chemical substances by application Substances 0.000 abstract description 13
- 239000011159 matrix material Substances 0.000 abstract description 11
- 229920005989 resin Polymers 0.000 abstract description 11
- 239000011347 resin Substances 0.000 abstract description 11
- 238000002844 melting Methods 0.000 abstract description 6
- 230000008018 melting Effects 0.000 abstract description 6
- 239000004744 fabric Substances 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 239000000155 melt Substances 0.000 abstract description 3
- 239000004753 textile Substances 0.000 abstract description 2
- 239000004743 Polypropylene Substances 0.000 description 12
- 229920002292 Nylon 6 Polymers 0.000 description 10
- 229920000139 polyethylene terephthalate Polymers 0.000 description 9
- -1 polypropylene Polymers 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 8
- 229920000728 polyester Polymers 0.000 description 8
- 229920001155 polypropylene Polymers 0.000 description 7
- JDSHMPZPIAZGSV-UHFFFAOYSA-N melamine Chemical compound NC1=NC(N)=NC(N)=N1 JDSHMPZPIAZGSV-UHFFFAOYSA-N 0.000 description 5
- 229920000877 Melamine resin Polymers 0.000 description 4
- 229910002804 graphite Inorganic materials 0.000 description 4
- 239000010439 graphite Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 229920001169 thermoplastic Polymers 0.000 description 4
- 239000004416 thermosoftening plastic Substances 0.000 description 4
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 229920001707 polybutylene terephthalate Polymers 0.000 description 3
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 2
- 229920002302 Nylon 6,6 Polymers 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 229920007019 PC/ABS Polymers 0.000 description 1
- 206010053615 Thermal burn Diseases 0.000 description 1
- 229920000122 acrylonitrile butadiene styrene Polymers 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 229920005669 high impact polystyrene Polymers 0.000 description 1
- 239000004797 high-impact polystyrene Substances 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- XFZRQAZGUOTJCS-UHFFFAOYSA-N phosphoric acid;1,3,5-triazine-2,4,6-triamine Chemical compound OP(O)(O)=O.NC1=NC(N)=NC(N)=N1 XFZRQAZGUOTJCS-UHFFFAOYSA-N 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 229920006149 polyester-amide block copolymer Polymers 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001902 propagating effect Effects 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 238000009941 weaving Methods 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/07—Addition of substances to the spinning solution or to the melt for making fire- or flame-proof filaments
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/44—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds
- D01F6/46—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polymers obtained by reactions only involving carbon-to-carbon unsaturated bonds as major constituent with other polymers or low-molecular-weight compounds of polyolefins
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/90—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyamides
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention belongs to the modified neck technology domains of textile fabric, it is related to a kind of preparation method of fire-retardant anti-molten droplet fiber, first by matrix resin chip drying, add anti-dripping agent powder and fire retardant thereto again, it is further blended, squeezes out, cools down, is granulated through double screw extruder after being sufficiently mixed, to which fire-retardant anti-molten droplet master batch be made, then by another matrix resin chip drying, it is mixed with injector conveying fire-retardant anti-molten droplet master batch with matrix resin slice, through the abundant melting mixing of spinning screw, and spinning is carried out, so that fire-retardant anti-molten droplet fiber be made；Directly anti-dripping agent and fire retardant are added in matrix resin slice, without melting drip phenomenon when resulting fire-retardant anti-molten droplet fiber burns, and the melt blending spinning process used will not influence the existing spinning technique of the fiber, and process flow is simple, is conducive to industrialized production.
Description
Technical field:
The invention belongs to the modified neck technology domains of textile fabric, are related to a kind of preparation method of fire-retardant anti-molten droplet fiber.
Background technique:
Thermoplastic fibre, such as polyester, Fypro, endurance life and breaking strength height, appearance good with wearability
Outstanding properties such as easy dyeing, thus be widely used in the fields such as clothes, daily necessity and industrial goods, but they are in burning
Melting drippage can be with propagating flame, other materials of igniting；It is viscous then to make skin scald on the skin, which greatly limits its
The application of garment material, drapery and fabrics for industrial use etc., although flame-retarded processing can be carried out to this fiber,
But the problem of molten drop not no good solution, therefore, fire-retardant anti-molten droplet are asking of constantly exploring all the time of researchers
Topic.
Currently, the method for fire-retardant anti-molten droplet has blending method, copolymerization method, post treatment method and graft crosslinking method etc..Blending method
Add anti-dripping agent powder etc. mainly to increase melt viscosity to reduce molten drop phenomenon.This method does not change production work used
Skill, simple and easy, applicable surface is wider, has been widely used for improving the flame retardant of plastics anti-dripping melts such as PC, ABS, PC/ABS, HIPS
Property.But since the partial size of existing powder is thicker, dosage is larger, can not be used for fibre spinning by melt blending.Therefore, it seeks
The preparation method for seeking a kind of fire-retardant anti-molten droplet fiber resists graphene, graphene oxide, graphite of the partial size between 0.5-5um
After dripping agent powder, fire retardant and matrix resin are pre-mixed, double screw extruder is recycled to be blended, squeezed out, is granulated, spun
Silk is applied in the co-blended spinning of the fiber using the flame-retardant anti-dropping agent of preparation as anti-dripping agent, and resulting fiber solves
The melting drippage problem of thermoplastic fibre.
Summary of the invention:
It is an object of the invention to overcome disadvantage of the existing technology, asked for the melting drippage of current thermoplastic fibre
Topic, design provide a kind of preparation method of fire-retardant anti-molten droplet fiber, the fire-retardant anti-molten droplet fiber of preparation can be applied to garment material,
Protective garment, drapery and fabrics for industrial use.
To achieve the goals above, the present invention prepares the detailed process of fire-retardant anti-molten droplet fiber are as follows:
(1) by matrix resin be sliced 95-135 DEG C at a temperature of it is dry reach 300ppm to moisture content, add thereto
Anti-dripping agent powder and fire retardant after being sufficiently mixed, then are further blended through double screw extruder, squeeze out, cool down, being granulated, from
And fire-retardant anti-molten droplet master batch is made, fire-retardant anti-molten droplet master batch is with the matrix resin that its poidometer includes 70-79.5%, 10-20%
Fire retardant and 20-0.5% anti-dripping agent；
(2) matrix resin slice is dry at a temperature of 95 DEG C -135 DEG C, until moisture content reaches 300ppm, use injector
The fire-retardant anti-molten droplet master batch of supplying step (1) preparation is mixed with matrix resin slice, through the abundant melting mixing of spinning screw, and
Spinning is carried out, so that fire-retardant anti-molten droplet fiber be made, anti-dripping agent weight percentage is 0.5%- in fire-retardant anti-molten droplet fiber
5%.
Anti-dripping agent of the present invention is graphene, graphene oxide or the graphite that partial size is 0.5-5um.
Fire-retardant anti-molten droplet fiber prepared by the present invention can long filament or staple fiber form, wherein the fineness of long filament is 50D-
300D, hole count 12F-144F；The fineness of staple fiber is 1.4D-20D, length 32mm-152mm.
Matrix resin of the present invention is polyester or polyamide or polypropylene.
Polyester of the present invention is polyethylene terephtalate, polybutylene terephthalate (PBT) PBT or poly- pairs
Benzene dicarboxylic acid trimethylene glycol ester PTT；The polyamide is polycaprolactam PA6 or polyhexamethylene adipamide PA66；The polypropylene
For polypropylene PP.
Fire retardant of the present invention is nitrogenated flame retardant melamine, melamine phosphate or melamine cyanurate
Salt.
Fire-retardant anti-molten droplet fiber prepared by the present invention can be used for garment material, protective garment, drapery and industry weaving
Product.
Compared with prior art, the present invention directly anti-dripping agent and fire retardant are added in matrix resin slice, use
Fire-retardant anti-molten droplet fiber has been obtained after the conventional spinning processes of thermoplastic fibre, when resulting fire-retardant anti-molten droplet fiber burns without
Drip phenomenon is melted, and the melt blending spinning process used will not influence the existing spinning technique of the fiber, technique stream
Journey is simple, is conducive to industrialized production.
Specific embodiment:
Technical solution of the present invention is further described in detail below by specific embodiment.
Embodiment 1:
The present embodiment prepares the detailed process of fire-retardant anti-molten droplet fiber are as follows:
(1) by PET be sliced 120 DEG C at a temperature of it is dry reach 300ppm to moisture content, add thereto graphene and
Melamine powder is squeezed out in double screw extruder with 280 DEG C or so of temperature mixing, so that fire-retardant anti-molten droplet polyester be made
Master batch, the fire-retardant anti-molten droplet polyester master particle include 10% graphene powder of the partial size at 0.5 μm with its poidometer, 20%
Melamine and 70% PET；
(2) by PET be sliced 120 DEG C at a temperature of it is pre-crystallized, and 140 DEG C at a temperature of it is dry, until moisture content reaches
To 300ppm；The fire-retardant anti-molten droplet polyester master particle of step (1) preparation is reached in 140 DEG C of at a temperature of drying to moisture content
300ppm；The fire-retardant anti-molten droplet polyester master particle after drying is added in the PET slice with the injector of volume metering mode,
Make content 1% of the graphene in PET, using conventional polyester spinning equipment and technique, spins the short fibre of PET of 1.4D, 38mm.
Embodiment 2:
The present embodiment prepares the detailed process of fire-retardant anti-molten droplet fiber are as follows:
(1) PA6 is sliced and is lower than 0.08% in 105 DEG C or so of at a temperature of drying to moisture content, addition oxidation thereto
Graphene and melamine cyanurate powder are squeezed out in double screw extruder with 230 DEG C or so of temperature mixing, to make
Fire-retardant anti-molten droplet polyamide master batch, the fire-retardant anti-molten droplet polyamide master batch with its poidometer include 5% partial size at 0.5 μm
Graphene oxide powder, 10% melamine cyanurate and 85% PA6；
(2) by PA6 slice, drying makes moisture content lower than 0.08% at 105 DEG C；Fire-retardant anti-molten droplet master batch is done at 105 DEG C
It is dry to be lower than 0.08% to moisture content, fire-retardant anti-molten droplet master batch after drying is quantitatively added with the injector of volume metering mode
Into PA6 slice, make content 1% of the graphene oxide in PA6, using conventional extrusion spinning equipment and technique, spinning
The PA6 fully drawn yarn of 150d/24f.
Embodiment 3:
The present embodiment prepares the detailed process of fire-retardant anti-molten droplet fiber are as follows:
(1) after being pre-mixed PP slice, nano-graphite and melamine, with 180 DEG C or so in double screw extruder
Temperature mixing squeezes out, so that fire-retardant anti-molten droplet polypropylene agglomerate be made, the fire-retardant anti-molten droplet polypropylene agglomerate is with its poidometer
Comprising 10% powdered graphite of the partial size at 1 μm, 10% melamine and 80% PP；
(2) above-mentioned fire-retardant anti-molten droplet master batch is drawn entirely using conventional polypropylene spinning equipment and technique, the PP for spinning 75d/42f
Stretch silk.
Comparative example 1:
PET is sliced by this comparative example makes moisture content reach 300ppm in 140 DEG C of at a temperature of drying, is spun using conventional polyester
Silk equipment and technique spin the short fibre of PET of 1.4D, 38mm.
Comparative example 2:
PA6 is sliced by this comparative example makes moisture content lower than 0.08% in 105 DEG C of at a temperature of drying, is spun using conventional polyamide fibre
Silk equipment and technique, spin the PA6 fully drawn yarn of 150d/24f.
Comparative example 3:
This comparative example spins the PP fully drawn yarn of 75d/42f using conventional polypropylene spinning equipment and technique.
Embodiment 4:
Short fine and long filament obtained in embodiment 1-3 and comparative example 1-3 is carried out fire-retardant anti-molten droplet performance by the present embodiment
It tests and compares, short fine and long filament obtained in embodiment 1-3 and comparative example 1-3 is first weighed into certain quality, is organized into
Effective length is the twisted fiber yarn of 10cm, and the twist is 14 twirls/10cm.Clamping sample opening one end with tweezers makes samples vertical,
With identical flame ignition, total molten drop number in burning time is recorded, evaluation result is as shown in the table, it can be seen that is not added with
The fiber burning time of fire retardant and anti-dripping agent is long, and drippage is obvious, and is added to the fiber afterflame of fire retardant and anti-dripping agent
Time is short, and drips without molten drop.
Claims (1)
1. a kind of preparation method of fire-retardant anti-molten droplet fiber, it is characterised in that detailed process are as follows:
(1) PA6 is sliced and is lower than 0.08% in 105 DEG C of at a temperature of drying to moisture content, add graphene oxide and three thereto
Poly cyanamid cyanurate powder is squeezed out in double screw extruder with 230 DEG C of temperature mixing, so that it is poly- that fire-retardant anti-molten droplet is made
Amide master batch, the fire-retardant anti-molten droplet polyamide master batch with its poidometer include 5% partial size 0.5mm graphene oxide powder
End, 10% melamine cyanurate and 85% PA6；
(2) by PA6 slice, drying makes moisture content lower than 0.08% at 105 DEG C；Fire-retardant anti-molten droplet master batch is dried extremely at 105 DEG C
Moisture content is lower than 0.08%, and fire-retardant anti-molten droplet master batch after drying is quantitatively added to PA6 with the injector of volume metering mode
In slice, make content 1% of the graphene oxide in PA6, using conventional extrusion spinning equipment and technique, spins 150d/24f
PA6 fully drawn yarn.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610204307.2A CN106811820B (en) | 2016-04-01 | 2016-04-01 | A kind of preparation method of fire-retardant anti-molten droplet fiber |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610204307.2A CN106811820B (en) | 2016-04-01 | 2016-04-01 | A kind of preparation method of fire-retardant anti-molten droplet fiber |
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| Publication Number | Publication Date |
|---|---|
| CN106811820A CN106811820A (en) | 2017-06-09 |
| CN106811820B true CN106811820B (en) | 2019-04-26 |
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| CN201610204307.2A Expired - Fee Related CN106811820B (en) | 2016-04-01 | 2016-04-01 | A kind of preparation method of fire-retardant anti-molten droplet fiber |
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107557901A (en) * | 2017-09-06 | 2018-01-09 | 广东大红马纺织新材料有限公司 | A kind of flame-retardant and anti-dripping polyester fiber and preparation method thereof |
| CN107936372A (en) * | 2017-12-01 | 2018-04-20 | 天津市恒宇磁塑制品有限公司 | Formula preparation method for the high resistant combustible material of window screening |
| CN108149337A (en) * | 2017-12-05 | 2018-06-12 | 上海帕吉索纳米技术有限公司 | A kind of graphene Jinlun-6 fireproof fiber and preparation method thereof |
| CN108360143B (en) * | 2017-12-25 | 2019-06-18 | 江苏美翔体育用品有限公司 | A kind of processing method of compound trampoline net |
| CN108048929B (en) * | 2017-12-29 | 2020-04-03 | 福建华彩新材料有限公司 | Nylon 6 fiber and preparation method thereof |
| CN110512336A (en) * | 2019-07-12 | 2019-11-29 | 浙江蓝天海纺织服饰科技有限公司 | Fast-drying type is without molten drop fabric |
| CN111471283A (en) * | 2020-04-23 | 2020-07-31 | 安徽大学 | Antistatic anti-dripping flame-retardant polymer master batch for spinning and preparation method thereof |
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| CN103741250A (en) * | 2013-12-04 | 2014-04-23 | 太仓荣文合成纤维有限公司 | Inorganic/organic hybrid composite fire retardation agent and application of the same in PET fibers |
| CN103923348A (en) * | 2014-04-02 | 2014-07-16 | 合肥杰事杰新材料股份有限公司 | Application of graphene as composition flame-retardant anti-dripping agent |
| CN104294398B (en) * | 2014-09-12 | 2016-10-05 | 浙江金彩新材料有限公司 | Method for preparing anti-dripping polyester fiber |
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