CN108823673A - A kind of conduction flame-resistant terylene and its preparation and application - Google Patents
A kind of conduction flame-resistant terylene and its preparation and application Download PDFInfo
- Publication number
- CN108823673A CN108823673A CN201810706306.7A CN201810706306A CN108823673A CN 108823673 A CN108823673 A CN 108823673A CN 201810706306 A CN201810706306 A CN 201810706306A CN 108823673 A CN108823673 A CN 108823673A
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- CN
- China
- Prior art keywords
- parts
- tetrathiafulvalene
- flame
- resistant terylene
- acid
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
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Classifications
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- D—TEXTILES; PAPER
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- 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
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- 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
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- 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
- D01F1/09—Addition of substances to the spinning solution or to the melt for making electroconductive or anti-static filaments
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- 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
- D01F1/10—Other agents for modifying properties
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- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/36—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
- D06M11/38—Oxides or hydroxides of elements of Groups 1 or 11 of the Periodic Table
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/80—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with boron or compounds thereof, e.g. borides
- D06M11/82—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with boron or compounds thereof, e.g. borides with boron oxides; with boric, meta- or perboric acids or their salts, e.g. with borax
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- D06M14/00—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials
- D06M14/08—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of synthetic origin
- D06M14/12—Graft polymerisation of monomers containing carbon-to-carbon unsaturated bonds on to fibres, threads, yarns, fabrics, or fibrous goods made from such materials on to materials of synthetic origin of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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- D06M2101/00—Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
- D06M2101/16—Synthetic fibres, other than mineral fibres
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Abstract
The invention proposes a kind of conductive flame-resistant terylenes, are prepared by following raw material：120-150 parts of tetrathiafulvalene modified polyester fibre, 20-40 parts of nitrogen phosphorus boron fire retardant preservative, 10-15 parts of dispersing agent, 1-5 parts of p-methyl benzenesulfonic acid, 20-30 parts of oxidant.Conduction flame-resistant terylene prepared by the present invention, while with the excellent properties such as polyester material intensity inherently is high, elasticity is good, shape-retaining ability is good, dimensional stability is high, antistatic property and flame retardant property are had both, therefore, it can be applied in the fields such as togs, have broad application prospects.
Description
Technical field
The present invention relates to textile fiber technology fields, and in particular to a kind of conduction flame-resistant terylene and preparation method thereof.
Background technique
Conventional fibre especially synthetic fibers easily generate electrostatic because of good electrical insulating property in processing, use, make it
Application field is very limited.The conducting of fiber can reduce even is eliminated electrostatic hazard, can also further expansion fiber
Application field.As a kind of important functional material, conductive fiber will be increasingly valued by people.Common conductive fiber
Mainly it is made using inorganic conductive material as conductive component using modes such as co-blended spinning or final finishings.Organic macromolecule conducting material
After especially polyaniline and its in-situ polymerization phenomenon are found, a kind of new material and method for preparing conductive fiber are provided.
Preparing Conductive Polyaniline Fibers using situ aggregation method has simple process, conducts electricity very well, the holding of matrix fiber mechanical property
The advantages that, attract the concern of numerous studies personnel rapidly.In the past 30 years, the various conductive fiber layers prepared with situ aggregation method
It is not poor out：The polyaniline composite conducting fibre that fiber is prepared as substrate is mainly such as conventionally synthesized using polyamide fibre, polypropylene fibre, polyurethane in early days
Dimension；In recent years with some new chemical fibers and natural fiber-such as polyimide fiber, polymethylmethacrylate fibers, sheep
Hair, silk, cotton fiber, cellulose fibre, kenaf, mango fiber, coir fibre, sugarcane fibre etc. are that substrate prepares polyphenyl
Amine composite conducting fiber has also obtained the attention of researcher.These conductive fibers are applied to anti-static material, electromagnetic shielding material
The fields such as material, pH value switch, gas sensor.
Fiber by limit oxygen index greater than 27% is commonly referred to as fire resistance fibre.Flame retardant property is by reducing material in fire
Combustibility in flame, slows down the rate of propagation of flame, and material leaves after flame can soon self-extinguishment.Using chemical fibre as raw material
Textile often becomes kindling and lures combustion things, discharges toxic and harmful gas, directly ignites and be detrimental to health.Especially high residential building and
Hotel is higher and higher to the flame-retardancy requirements of indoor article and adornment, and developed country has formulated the flame retardant regulation of textile already
And flame-retardant standard, concern of the development and application of fire resistance fibre and textile more by society.
Terylene has the excellent properties such as intensity is high, elasticity is good, shape-retaining ability is good, dimensional stability is high, the clothing being made by it
Prolonged endurable, electrical insulating property is good, quick-drying washable, the laudatory title with " wash and wear ", thus is widely used in clothes, decoration, production
The fields such as industry.But terylene is since interior molecules arrangement is close, it is intermolecular to lack hydrophilic-structure, therefore regain very little, moisture absorption
Performance is poor, and antistatic property is bad.That even if fire retardant is not added or joined fire retardant in common terylene preparation method, greatly
Part is also halogenated flame retardant, although halogenated flame retardant has preferable flame retardant effect, its hydrogen chloride etc. generated when burning
Toxic gas seriously endangers people's health.Therefore, it under the pressure of the demand of practical application, needs to develop a antistatic effect good same
When the high polyester fiber of flame retardant property, preparation and corresponding Material Field for togs.
Summary of the invention
In order to solve the above technical problems, the present invention provides a kind of conductive flame-resistant terylene and preparation method thereof, purpose
It is, a kind of conductive flame-resistant terylene is provided, by greatly strengthening leading for polyester fiber for tetrathiafulvalene modified polyester fibre
Electrical property, compare has better conductive effect, has it with polyaniline/polyester fiber, conductive fiber prepared by the present invention
Good antistatic property；By the nitrogen phosphorus boron fire retardant preservative of addition preparation, flame retardant effect and halogenated flame retardant effect are quite even
More excellent, more environmentally friendly, performance is more excellent.
The present invention provides a kind of conductive flame-resistant terylene, which is characterized in that is prepared by following raw material：Four sulphur are rich
Watt 120-150 parts of alkene modified polyester fibre, 20-40 parts of nitrogen phosphorus boron fire retardant preservative, 10-15 parts of dispersing agent, 1-5 parts of p-methyl benzenesulfonic acid,
20-30 parts of oxidant；
The dispersing agent is selected from fatty acid, aliphatic amide type, esters, paraffin class, metal soap and low molecule wax class
One or more of dispersing agent；
The oxidant be alkaline oxidiser, one in sodium hypochlorite, SODIUM PERCARBONATE, sodium perborate, potassium perborate
Kind is several.
As further improvement of the invention, it is prepared by following raw material：Tetrathiafulvalene modified dacron is fine
Tie up 130-140 parts, 25-35 parts of nitrogen phosphorus boron fire retardant preservative, 12-14 parts of dispersing agent, 2-4 parts of p-methyl benzenesulfonic acid, 22-27 parts of oxidant.
As further improvement of the invention, it is prepared by following raw material：Tetrathiafulvalene modified dacron is fine
Tie up 137 parts, 29 parts of nitrogen phosphorus boron fire retardant preservative, 13 parts of dispersing agent, 3 parts of p-methyl benzenesulfonic acid, 25 parts of oxidant.
As further improvement of the invention, dispersing agent is selected from hexenyl bis-stearamides, glyceryl monostearate, three firmly
Glycerol, atoleine/stearic acid, microcrystalline wax/calcium stearate, microcrystalline wax/stearic acid, atoleine // stearic acid
Calcium, barium stearate, zinc stearate, calcium stearate, cadmium stearate, magnesium stearate, copper stearate, ethylene-acrylic acid copolymer,
One of ethylene-vinyl acetate copolymer is several.
As further improvement of the invention, tetrathiafulvalene modified polyester fibre is prepared by following methods：It is to mix with HCl
Heteroacid, by tetrathiafulvalene and HCl with the ratio of the amount of substance for 1:It is molten that 1 ratio is hybridly prepared into the mixing of HCl/ tetrathiafulvalene
Liquid adds initiator, obtains mixed solution；Polyester fiber is padded in mixed solution during continuous operation, yarn quilt
It deflects from and is statically placed under room temperature environment after padding area, make the oxidation polymerization under non-liquid environment of the mixing liquid of yam surface, 5-6h
Conductive tetrathiafulvalene modified polyester fibre is obtained afterwards.
As further improvement of the invention, initiator is selected from benzoyl peroxide, lauroyl peroxide, benzoyl peroxide first
Tert-butyl acrylate, peroxidating trimethylacetic acid tertiary butyl ester, di-isopropyl peroxydicarbonate, sodium peroxydisulfate, ammonium persulfate, azo two are different
One or more of butyronitrile, azobisisoheptonitrile.
As further improvement of the invention, nitrogen phosphorus boron fire retardant preservative is prepared by following methods：Phosphoric acid is added in a kettle
Ammonium when agitating and heating temperature reaches 90 DEG C, is added catalyst, boric acid or borax, continues to stir；Persistently overheating is to 135 DEG C, heat preservation
Stop heating after reacting 10min, obtains nitrogen phosphorus boron fire retardant preservative.
As further improvement of the invention, catalyst is by stannic chloride, copper sulphate, potassium chloride in mass ratio 1：(0.5-1)：
(2-5) ratio is uniformly mixed and forms.
The present invention further protects a kind of preparation method of above-mentioned conductive flame-resistant terylene, is prepared according to the following steps：
Step 1: alkali decrement treatment：It is 200g/L's that tetrathiafulvalene modified polyester fibre monofilament, which is put into mass concentration,
In NaOH solution, it is placed on roughening treatment 60-90min in 70 DEG C of thermostat water bath, is sufficiently cleaned after taking-up with deionized water,
Then it dries at 60 DEG C to constant-quality；
Step 2: being sent into after being heated to 150 DEG C by nitrogen phosphorus boron fire retardant preservative, p-methyl benzenesulfonic acid and oxidant, dry 6-10h
Screw extruder is pumped into batch mixer in screw extruder heating melting；Again by the tetrathiafulvalene Modified Polyester after alkali decrement treatment
After synthetic fibre fibre single thread and dispersing agent dry 10h under conditions of 150-170 DEG C, batch mixer is added, with nitrogen phosphorus boron fire retardant preservative, to first
Benzene sulfonic acid and oxidant carry out melt spinning after mixing, obtain conductive flame-resistant terylene.
As further improvement of the invention, the process conditions of spinning are that the area screw extruder I-V set temperature is respectively
280 DEG C, 284 DEG C, 290 DEG C, 293 DEG C, 285 DEG C, melt pipe temperature are 293 DEG C；Prefilter temperature is 285 DEG C, manifold
Temperature is 285 DEG C；Metering pump speed is 30-40r/min, specification 10mL/r, and pump is 4200-4400g/min for amount；Spinning speed
Degree is 800-820m/min；Upper oil mass is 0.7-0.8%.
The present invention has the advantages that：
1. tetrathiafulvalene modified polyester fibre prepared by the present invention, as the good organism structure of electric conductivity ---
Tetrathiafulvalene polymerize in PET fiber surface and generates tetrathiafulvalene, greatly strengthens the electric conductivity of polyester fiber, compare
With polyaniline/polyester fiber, conductive fiber prepared by the present invention has better conductive effect, has it antistatic well
Performance；
2. the bittern-free flame-proof material that the present invention adds in raw material, the terylene being prepared by the method for the invention is fine
Dimension, flame retardant effect is quite even more excellent with halogenated flame retardant effect, and perfection is instead of halogenated flame retardant, and more environmentally friendly, performance is more excellent
It is different；
To sum up, polyester fiber prepared by the present invention, not only with the intensity of polyester material inherently is high, elasticity is good, protects
The excellent properties such as type is good, dimensional stability is high, meanwhile, antistatic effect is good, and flame retardant property is good, therefore, can be applied to spy
In the fields such as different clothes, have broad application prospects.
Detailed description of the invention
Fig. 1 is the preparation technology figure of conductive flame-resistant terylene.
Specific embodiment
Below in conjunction with the embodiment of the present invention, the technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, the embodiment described is the embodiment of part of representative of the invention, rather than whole embodiments, this field are general
Other all embodiments obtained belong to protection of the invention to logical technical staff without making creative work
Range.
The preparation of the conductive flame-resistant terylene of embodiment 1
Raw material composition：120 parts of tetrathiafulvalene modified polyester fibre, 20 parts of nitrogen phosphorus boron fire retardant preservative, hexenyl stearic bicine diester
10 parts of amine, 1 part of p-methyl benzenesulfonic acid, 20 parts of sodium hypochlorite；
Tetrathiafulvalene modified polyester fibre is prepared by following methods：Using HCl as dopant acid, by tetrathiafulvalene and HCl
With the ratio of the amount of substance for 1:1 ratio is hybridly prepared into HCl/ tetrathiafulvalene mixed solution, adds lauroyl peroxide, obtains
Mixed solution；Polyester fiber is padded in mixed solution during continuous operation, yarn is deflected from pad area after be statically placed in
Under room temperature environment, make the oxidation polymerization under non-liquid environment of the mixing liquid of yam surface, rich watt of four conductive sulphur is obtained after 5h
Alkene modified polyester fibre.
Nitrogen phosphorus boron fire retardant preservative is prepared by following methods：Ammonium phosphate is added in a kettle, agitating and heating temperature reaches 90 DEG C
When, catalyst is added (by stannic chloride, copper sulphate, potassium chloride in mass ratio 1：0.7：3.5 ratios be uniformly mixed forms), boric acid or
Borax continues to stir；Persistently overheating stops heating, obtains nitrogen phosphorus boron fire retardant preservative to 135 DEG C after insulation reaction 10min.
Conductive flame-resistant terylene following methods preparation：
Step 1: alkali decrement treatment：It is 200g/L's that tetrathiafulvalene modified polyester fibre monofilament, which is put into mass concentration,
In NaOH solution, it is placed on roughening treatment 60min in 70 DEG C of thermostat water bath, is sufficiently cleaned after taking-up with deionized water, so
It dries at 60 DEG C to constant-quality afterwards；
Step 2: being sent into spiral shell after being heated to 150 DEG C by nitrogen phosphorus boron fire retardant preservative, p-methyl benzenesulfonic acid and sodium hypochlorite, dry 6h
Bar extruder is pumped into batch mixer in screw extruder heating melting；Again by the tetrathiafulvalene modified dacron after alkali decrement treatment
After fibre single thread and hexenyl bis-stearamides dry 10h under conditions of 150 DEG C, be added batch mixer, with nitrogen phosphorus boron fire retardant preservative,
P-methyl benzenesulfonic acid and oxidant carry out melt spinning after mixing, obtain conductive flame-resistant terylene；
The process conditions of spinning be the area screw extruder I-V set temperature be respectively 280 DEG C, 284 DEG C, 290 DEG C, 293 DEG C,
285 DEG C, melt pipe temperature is 293 DEG C；Prefilter temperature is 285 DEG C, and condition of spinning manifold temperature is 285 DEG C；Metering pump speed is
30r/min, specification 10mL/r, pump are 4200g/min for amount；Spinning speed is 800m/min；Upper oil mass is 0.7%.
The preparation of the conductive flame-resistant terylene of embodiment 2
Raw material composition：150 parts of tetrathiafulvalene modified polyester fibre, 40 parts of nitrogen phosphorus boron fire retardant preservative, atoleine // tristearin
15 parts of sour calcium, 5 parts of p-methyl benzenesulfonic acid, 30 parts of SODIUM PERCARBONATE；
Tetrathiafulvalene modified polyester fibre is prepared by following methods：Using HCl as dopant acid, by tetrathiafulvalene and HCl
With the ratio of the amount of substance for 1:1 ratio is hybridly prepared into HCl/ tetrathiafulvalene mixed solution, adds azodiisobutyronitrile, obtains
Mixed solution；Polyester fiber is padded in mixed solution during continuous operation, yarn is deflected from pad area after be statically placed in
Under room temperature environment, make the oxidation polymerization under non-liquid environment of the mixing liquid of yam surface, it is rich that four conductive sulphur are obtained after 5-6h
Watt alkene modified polyester fibre.
Nitrogen phosphorus boron fire retardant preservative is prepared by following methods：Ammonium phosphate is added in a kettle, agitating and heating temperature reaches 90 DEG C
When, catalyst is added (by stannic chloride, copper sulphate, potassium chloride in mass ratio 1：0.5：2 ratios are uniformly mixed and form), boric acid or boron
Sand continues to stir；Persistently overheating stops heating, obtains nitrogen phosphorus boron fire retardant preservative to 135 DEG C after insulation reaction 10min.
Conductive flame-resistant terylene following methods preparation：
Step 1: alkali decrement treatment：It is 200g/L's that tetrathiafulvalene modified polyester fibre monofilament, which is put into mass concentration,
In NaOH solution, it is placed on roughening treatment 90min in 70 DEG C of thermostat water bath, is sufficiently cleaned after taking-up with deionized water, so
It dries at 60 DEG C to constant-quality afterwards；
Step 2: being sent into after being heated to 150 DEG C by nitrogen phosphorus boron fire retardant preservative, p-methyl benzenesulfonic acid and SODIUM PERCARBONATE, dry 10h
Screw extruder is pumped into batch mixer in screw extruder heating melting；Again by the tetrathiafulvalene Modified Polyester after alkali decrement treatment
After synthetic fibre fibre single thread and atoleine // calcium stearate dry 10h under conditions of 170 DEG C, batch mixer is added, is hindered with nitrogen phosphorus boron
Combustion agent, p-methyl benzenesulfonic acid and oxidant carry out melt spinning after mixing, obtain conductive flame-resistant terylene；
The process conditions of spinning be the area screw extruder I-V set temperature be respectively 280 DEG C, 284 DEG C, 290 DEG C, 293 DEG C,
285 DEG C, melt pipe temperature is 293 DEG C；Prefilter temperature is 285 DEG C, and condition of spinning manifold temperature is 285 DEG C；Metering pump speed is
40r/min, specification 10mL/r, pump are 4400g/min for amount；Spinning speed is 820m/min；Upper oil mass is 0.8%.
The preparation of the conductive flame-resistant terylene of embodiment 3
Raw material composition：It is 137 parts of tetrathiafulvalene modified polyester fibre, 29 parts of nitrogen phosphorus boron fire retardant preservative, 13 parts of cadmium stearate, right
3 parts of toluenesulfonic acid, 25 parts of potassium perborate；
Tetrathiafulvalene modified polyester fibre is prepared by following methods：Using HCl as dopant acid, by tetrathiafulvalene and HCl
With the ratio of the amount of substance for 1:1 ratio is hybridly prepared into HCl/ tetrathiafulvalene mixed solution, adds the tertiary fourth of perbenzoic acid
Ester obtains mixed solution；Polyester fiber is padded in mixed solution during continuous operation, yarn is deflected from pad area after
It is statically placed under room temperature environment, makes the oxidation polymerization under non-liquid environment of the mixing liquid of yam surface, conduction is obtained after 5-6h
Tetrathiafulvalene modified polyester fibre.
Nitrogen phosphorus boron fire retardant preservative is prepared by following methods：Ammonium phosphate is added in a kettle, agitating and heating temperature reaches 90 DEG C
When, catalyst is added (by stannic chloride, copper sulphate, potassium chloride in mass ratio 1：1：5 ratios are uniformly mixed and form), boric acid or boron
Sand continues to stir；Persistently overheating stops heating, obtains nitrogen phosphorus boron fire retardant preservative to 135 DEG C after insulation reaction 10min.
Conductive flame-resistant terylene following methods preparation：
Step 1: alkali decrement treatment：It is 200g/L's that tetrathiafulvalene modified polyester fibre monofilament, which is put into mass concentration,
In NaOH solution, it is placed on roughening treatment 75min in 70 DEG C of thermostat water bath, is sufficiently cleaned after taking-up with deionized water, so
It dries at 60 DEG C to constant-quality afterwards；
Step 2: being sent into spiral shell after being heated to 150 DEG C by nitrogen phosphorus boron fire retardant preservative, p-methyl benzenesulfonic acid and potassium perborate, dry 8h
Bar extruder is pumped into batch mixer in screw extruder heating melting；Again by the tetrathiafulvalene modified dacron after alkali decrement treatment
After fibre single thread and cadmium stearate dry 10h under conditions of 160 DEG C, batch mixer is added, with nitrogen phosphorus boron fire retardant preservative, to toluene sulphur
Acid and oxidant carry out melt spinning after mixing, obtain conductive flame-resistant terylene；
The process conditions of spinning be the area screw extruder I-V set temperature be respectively 280 DEG C, 284 DEG C, 290 DEG C, 293 DEG C,
285 DEG C, melt pipe temperature is 293 DEG C；Prefilter temperature is 285 DEG C, and condition of spinning manifold temperature is 285 DEG C；Metering pump speed is
35r/min, specification 10mL/r, pump are 4300g/min for amount；Spinning speed is 810m/min；Upper oil mass is 0.75%.
Reference examples 1 are prepared according to " production method of inflaming retarding hollow polyster fiber " method of patent ZL 201210053402.9
Polyester raw material terephthalic acid (TPA) and ethylene glycol are pressed 1.12：1 molar ratio after evenly mixing, in urging for antimony glycol
Under change effect, polyethylene terephthalate melt successively is obtained through esterification and polycondensation reaction, polyester fondant booster pump will gather
Ethylene glycol terephthalate melt is pumped into first road static mixer；After phosphorus flame retardant is heated to 150 DEG C, drying 5 hours,
It is sent into screw extruder, point six temperature-controlled areas in screw extruder, the heating temperature of each temperature-controlled area is 275 DEG C,
277 DEG C, 280 DEG C, 280 DEG C, 277 DEG C, 275 DEG C, the fire retardant melt of screw extruder heating melting is also pumped into through metering pump
First road static mixer；Polyethylene terephthalate melt and fire retardant melt are formed after the mixing of first road static mixer
Blend melt again through blend melt booster pump, successively pumped through fondant filter, two static mixers and be sent into spinning head,
Blend melt is extruded into hollow Filamentous thread from the micropore of " C " type of spinning head spinneret, and hollow filiform thread is through circular blow
Wind apparatus quenching is solidified into hollow fibre filament, 17 DEG C of the wind-warm syndrome of circular blow wind apparatus, wind speed 4m/s；The poly terephthalic acid second two
The mass ratio 97 of alcohol ester melt and fire-retardant melt：4；The phosphorus flame retardant is polyphenyl phosphonic acids diphenyl sulphone (DPS) ester；The blend melt
Into the pressure 10Mpa of spinning head.
Reference examples 2 are according to a kind of " the preparation side of copper sulfide/terylene composite conducting fiber patent ZL 201610209912.9
The preparation of method " method
20 grams of polyester fibers are immersed in ethylenediamine/normal propyl alcohol solution that 1000 gram mass concentration are 5%, is reacted at 60 DEG C
It 1 hour, after completion of the reaction, is sufficiently rinsed with water to remove unreacted ethylenediamine, the terylene of amination will be obtained after fiber drying
Fiber.
The amination polyester fiber for taking 10 grams of above-mentioned steps to obtain immerses the cupric sulfate pentahydrate water that 50 gram mass concentration are 5%
It in solution, is impregnated at 60 DEG C after twenty minutes, the sodium thiosulfate solution that 50 gram mass concentration are 5% is added, is warming up to 95 DEG C
It reacts 0.3 hour, is rinsed after taking-up fiber with water, obtains copper sulfide/terylene composite conducting fiber after drying.
1 performance test of test case
1. electric conductivity：By polyester fiber made from 1-3 of the embodiment of the present invention and reference examples 2 temperature be 20 DEG C, humidity
After being balanced for 24 hours under conditions of being 65%, using the resistance of high insulation resistance instrument measurement certain length yarn section.
2. mechanical property：Using universal testing machine, according to GB/T 3916-2013《Yarn single yarn is wrapped in textile
The measurement of ultimate strength and elongation at break》Test yarn ultimate strength and elongation at break.Sample holder length is 250mm,
The collet speed of service is 250mm/min；100 times of calculating of stress when initial modulus presses yarn elongation 1%.
3. dry heat resistance energy：DHL7-9097A type electric heating constant-temperature blowing drying box is used under tension-free state, to this hair
Polyester material prepared by bright embodiment 1-3 and reference examples 1 handles 1h at 220 DEG C.Will treated sample in constant temperature and humidity shape
It is stood under state for 24 hours, later in this case with X L-1 type Yarn Strength instrument test strength.
10 groups of data of each sample test.
Test result is shown in Table 1.
The performance test results of 1 each group polyester material of table
As seen from the above table, conductive flame-resistant terylene prepared by the present invention, has higher conductivity, and dry heat resistance can be more excellent,
And mechanical property is preferable, is comprehensively compared, the performance of the conductive flame-resistant terylene of preparation of the embodiment of the present invention is more preferably comprehensive, more suitable for
The preparation of togs.
Those skilled in the art is not under conditions of departing from the spirit and scope of the present invention that claims determine, also
Various modifications can be carried out to the above content.Therefore the scope of the present invention is not limited in above explanation, but by
The range of claims determines.
Claims (10)
1. a kind of conduction flame-resistant terylene, which is characterized in that be prepared by following raw material：Tetrathiafulvalene modified dacron
120-150 parts of fiber, 20-40 parts of nitrogen phosphorus boron fire retardant preservative, 10-15 parts of dispersing agent, 1-5 parts of p-methyl benzenesulfonic acid, oxidant 20-30
Part；
The dispersing agent is selected from fatty acid, aliphatic amide type, esters, paraffin class, metal soap and the dispersion of low molecule wax class
One or more of agent；
The oxidant is alkaline oxidiser, selected from one of sodium hypochlorite, SODIUM PERCARBONATE, sodium perborate, potassium perborate or
It is several.
2. a kind of conductive flame-resistant terylene according to claim 1, which is characterized in that be prepared by following raw material：
130-140 parts of tetrathiafulvalene modified polyester fibre, 25-35 parts of nitrogen phosphorus boron fire retardant preservative, 12-14 parts of dispersing agent, p-methyl benzenesulfonic acid
2-4 parts, 22-27 parts of oxidant.
3. a kind of conductive flame-resistant terylene according to claim 1, which is characterized in that be prepared by following raw material：
137 parts of tetrathiafulvalene modified polyester fibre, 29 parts of nitrogen phosphorus boron fire retardant preservative, 13 parts of dispersing agent, 3 parts of p-methyl benzenesulfonic acid, oxidant
25 parts.
4. a kind of conductive flame-resistant terylene according to claim 1, which is characterized in that it is double stearic that the dispersing agent is selected from hexenyl
Amide, glyceryl monostearate, glyceryl tristearate, atoleine/stearic acid, microcrystalline wax/calcium stearate, microlite
It is wax/stearic acid, atoleine // calcium stearate, barium stearate, zinc stearate, calcium stearate, cadmium stearate, magnesium stearate, hard
One of resin acid copper, ethylene-acrylic acid copolymer, ethylene-vinyl acetate copolymer are several.
5. a kind of conductive flame-resistant terylene according to claim 1, which is characterized in that the tetrathiafulvalene modified polyester fibre
It is prepared by following methods：Using HCl as dopant acid, by tetrathiafulvalene and HCl with the ratio of the amount of substance for 1:1 ratio mixed preparing
At HCl/ tetrathiafulvalene mixed solution, initiator is added, mixed solution is obtained；Polyester fiber is soaked during continuous operation
Roll in mixed solution, yarn is deflected from pad area after be statically placed under room temperature environment, make the mixing liquid of yam surface in non-liquid
Oxidation polymerization under phase environment obtains conductive tetrathiafulvalene modified polyester fibre after 5-6h.
6. a kind of conductive flame-resistant terylene according to claim 5, which is characterized in that the initiator is selected from benzoyl peroxide first
Acyl, lauroyl peroxide, peroxidized t-butyl perbenzoate, peroxidating trimethylacetic acid tertiary butyl ester, di-isopropyl peroxydicarbonate,
One or more of sodium peroxydisulfate, ammonium persulfate, azodiisobutyronitrile, azobisisoheptonitrile.
7. a kind of conductive flame-resistant terylene according to claim 1, which is characterized in that the nitrogen phosphorus boron fire retardant preservative is by following methods
Preparation：Ammonium phosphate is added in a kettle, when agitating and heating temperature reaches 90 DEG C, catalyst, boric acid or borax is added, continues to stir
It mixes；Persistently overheating stops heating, obtains nitrogen phosphorus boron fire retardant preservative to 135 DEG C after insulation reaction 10min.
8. a kind of conductive flame-resistant terylene according to claim 7, which is characterized in that the catalyst by stannic chloride, copper sulphate,
Potassium chloride in mass ratio 1：(0.5-1)：(2-5) ratio is uniformly mixed and forms.
9. a kind of preparation method of conduction flame-resistant terylene described in -8 any claims according to claim 1, which is characterized in that press
It is prepared according to following steps：
Step 1: alkali decrement treatment：Tetrathiafulvalene modified polyester fibre monofilament is put into the NaOH that mass concentration is 200g/L
In solution, it is placed on roughening treatment 60-90min in 70 DEG C of thermostat water bath, is sufficiently cleaned after taking-up with deionized water, then
It dries at 60 DEG C to constant-quality；
Step 2: being sent into screw rod after being heated to 150 DEG C by nitrogen phosphorus boron fire retardant preservative, p-methyl benzenesulfonic acid and oxidant, dry 6-10h
Extruder is pumped into batch mixer in screw extruder heating melting；It is again that the tetrathiafulvalene modified dacron after alkali decrement treatment is fine
After dimension monofilament and dispersing agent dry 10h under conditions of 150-170 DEG C, batch mixer is added, with nitrogen phosphorus boron fire retardant preservative, to toluene sulphur
Acid and oxidant carry out melt spinning after mixing, obtain conductive flame-resistant terylene.
10. a kind of preparation method of conductive flame-resistant terylene according to claim 9, which is characterized in that the technique of the spinning
Condition is that the area screw extruder I-V set temperature is respectively 280 DEG C, 284 DEG C, 290 DEG C, 293 DEG C, 285 DEG C, melt pipe temperature
It is 293 DEG C；Prefilter temperature is 285 DEG C, and condition of spinning manifold temperature is 285 DEG C；Metering pump speed is 30-40r/min, and specification is
10mL/r, pump are 4200-4400g/min for amount；Spinning speed is 800-820m/min；Upper oil mass is 0.7-0.8%.
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