CN110158189A - A kind of preparation method of high mode and low mode type flame-resistant terylene industrial yarn - Google Patents
A kind of preparation method of high mode and low mode type flame-resistant terylene industrial yarn Download PDFInfo
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- CN110158189A CN110158189A CN201910447241.3A CN201910447241A CN110158189A CN 110158189 A CN110158189 A CN 110158189A CN 201910447241 A CN201910447241 A CN 201910447241A CN 110158189 A CN110158189 A CN 110158189A
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- phosphonic acid
- methylene phosphonic
- industrial yarn
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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
-
- 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
- D01F11/00—Chemical after-treatment of artificial filaments or the like during manufacture
- D01F11/04—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers
- D01F11/08—Chemical after-treatment of artificial filaments or the like during manufacture of synthetic polymers of macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
-
- 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
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- 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)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The present invention relates to macromolecular fibre production technical fields, more particularly to a kind of preparation method of high mode and low mode type flame-resistant terylene industrial yarn.The present invention, which mainly passes through, chooses specific material, macromolecule phosphorus flame retardant, high viscous PET slice are mixed, and control the important parameters such as the viscosity of mixture, phosphorus content, then actual parameter control is carried out in each spinning link, including temperature, winding speed etc., high-strength flame-resistant terylene industrial yarn is finally obtained.It is an advantage of the invention that the spinning oil used has good rub resistance, coherent in production terylene industrial yarn spinning oil agent, the generation stretched with lousiness in rear weaving process can be greatly reduced, intensity is high, halogen-free environmental, the features such as flame retardant property is good, and spinning lousiness is few.
Description
Technical field
The invention belongs to macromolecular fibre production technical fields, more particularly to a kind of high mode and low mode type flame-resistant terylene industry
The preparation method of silk.
Background technique
High mode and low mode type flame-resistant terylene industrial yarn is mainly used in tyre cord, mine conveying belt, and automobile-used sebific duct etc. is wanted
Ask intensity high, good stability of the dimension, wearability is good, excellent fireproof performance.
The limit oxygen index LOI of terylene is generally 20%-22%, belongs to combustible material, occurs to dive brought by fire
It also becomes increasingly conspicuous in danger.Current terylene both domestic and external is flame-retardant modified mainly (main using the fire retardant of phosphorus system as modifying agent
It is based on copolymerization addition CEPPA), a large amount of combustion heat is generated in combustion using the phosphorus-containing groups of phosphorus flame retardant, is made
Polyester melt reduces kinematic viscosity and generates melting drippage, takes away heat, and put out using the effect of the radical-scavenging of phosphonium flame retardant
It puts out a fire flame, reaches fire-retardant purpose, it is fire-retardant that fire retardant mechanism is that molten drop takes away heat.Generally have before spinning winding dip-coating fire retardant and
Modified method is sliced to prepare flame-resistant terylene industrial yarn, using the method for yarn dip-coating fire retardant before winding, since it only exists
Yam surface contains fire retardant, in rear weaving, due to by high temperature, solvent, the influence of the processes such as friction, fire retardant during arrangement
Easily by damage sledge, the flame retardant property of fabric is affected, and flame retardant property reduces as time goes by.
Using the modified production CEPPA phosphorous flame-retardant slice of PET, fire retardant belongs to low-molecular material, although slice IV value is logical
The method for crossing solid-phase tack producing reaches 1.0~1.2dl/g, but is sliced crystallization temperature and fusing point and is intended to low, spinning than pure PET slice
Molecule thermal degradation is serious in journey, to affect spinnability and tensile property.The method oxygen index (OI) (LOI) of current application CEPPA
32% flame-resistant terylene industrial yarn maximum intensity generally in 6.5cN/dtex or so, hence it is evident that be lower than existing high-strength non-flame resistant terylene
Industrial yarn, and lousiness, broken end are also apparently higher than the non-flame resistant polyester industrial yarn of similar product.Due to the low and lousiness of intensity
It is more, the cost and difficulty of rear road application are increased, to limit the development of industry.
Phosphorus flame retardant is the most effective environment friendly flame retardant of terylene, and the processing method that fire retardant introduces can be divided mainly into altogether
Poly- modification and blending and modifying process route.Modification by copolymerization is to utilize small molecule fire retardant and polyester monocase with reactive functional groups
Copolyreaction is carried out, introduces fire-retardant group in polyester molecule chain.This method is more stable with product quality, adds fire retardant
Less, the more durable advantage of flame retardant effect.But the introducing of reactive phosphorus flame retardant can destroy the rule of polyester macromolecule chain structure
Integer, to influence crystal property and anti-hydrolytic performance of polyester fiber etc., eventually lead to product heat resistance, mechanical property and
The significant decrease of the performances such as resistance to ag(e)ing.
Blending and modifying is fire retardant and polyester slice or melt to be carried out melt blending, then obtain fire resistance fibre through spinning.
This method has better flexibility and diversity, but be easily precipitated with fire retardant bad dispersibility in the polyester, fire retardant,
The disadvantages such as poor, the spinnability difference of durability of fire-retardant, to limit its application in polyester fiber.
Polyphosphate polymer masterbatch selected by this patent has the characteristics that phosphorus content is high, good with polyester compatibility, overcomes
Blending modification method fire retardant bad dispersibility is easily precipitated, the disadvantages of durability is poor, spinnability is poor, prepared flame-resistant terylene work
Industry long filament has the characteristics that intensity is high, flame retardant property is good, ageing-resistant.
Summary of the invention
The invention proposes a kind of slices being blended using supra polymer phosphorus flame retardant with PET, obtain through melting spinning
A kind of high mode and low mode type flame-resistant terylene industrial yarn, it includes the characteristics of have；Intensity is high, and halogen-free environmental, flame retardant property is good, spinning
The features such as lousiness is few.
A kind of high mode and low mode type flame-resistant terylene industrial yarn Denier range of the present invention include: 840dtex~
3000dtex, thickness (fiber number/hole count) DPF range of individual thread include 2~10 polyester industrial yarn.Its breaking strength range:
6.0~7.5cN/dtex, extension at break range: 10.0~20.0%, intermediate elongation (@4.0cN/dtex): 4.5~6.5%；It is dry
Percent thermal shrinkage (177 DEG C of * 10min*0.05cN/dtex): 2.0~4.0%, limit oxygen index (LOI) >=32.0%.
The present invention is achieved by following technical proposals:
A kind of preparation method of high mode and low mode type flame-resistant terylene industrial yarn, which is characterized in that include the following steps:
(1) raw material is selected
Component A: macromolecule phosphorus flame retardant, design parameter are as follows: molecular weight 40000~100000, phosphorus content: 8~12%,
Tg；100~105 DEG C；The macromolecule phosphorus flame retardant is a kind of containing polyphosphonate carbonates altogether, and polyphosphonates are copolymerized phosphine
Acid esters it is one or more, be formed by scion grafting to PET strand；The control of its middle-molecular-weihydroxyethyl is 60000~70000 for most
It is good；
Component B: the viscous PET slice of height, design parameter are as follows: special industry viscosity is 1.10~1.20dl/g, and the viscous PET slice of height includes
There are light and/or micro- delustring slice TiO greatly2≤ 0.5%；
(2) mixed process: component A is mixed with component B, component A account for mixing after raw material mass ratio be 5~10%,
Its viscosity is 1.0~1.20dl/g, 5000~9000PPM of phosphorus content；Wherein 6000~8000PPM of phosphorus content is preferable；Component A
Account for the mass ratio of raw material after mixing are as follows: effect when 7~10% is more preferable；
(3) drying process: mixed raw material in step (2) is dried；
(4) melting process: by step (3) through dry feedstock in N2Under protection, to original within the scope of 265 DEG C~310 DEG C
Material carries out heating melting, enters back into spinning manifold, and the temperature of spinning manifold is controlled at 265 DEG C~310 DEG C；
(5) measure spinning process: the melt through abundant melting carries out spinning by metering pump；Melt warp through abundant melting
It crosses metering pump and requires accurate measurement according to the fiber number of setting, metering pump speed is calculated according to institute's textile product fiber number and spinning speed；
(6) be cooled and shaped: the spinning sprayed through spinneret orifice carries out being cooled to tow, cooling wind control temperature through ring blowing cooling wind
Degree is 40~65 DEG C；；
(7) drawing process: carrying out stretching and thermal finalization for tow after cooling, stretches total multiplying power 1.5~3.0, sizing temperature
235 DEG C~260 DEG C of degree；To reach desired strength, elongation is xeothermic every object then data such as to shrink.
(8) winding process: control winding speed 4000m/min~6500m/min.Using the high-speed winding of TMT fork type
The characteristics of tow after stretching directly on paper tube, is had package beautiful by aspect, even tension.
Preferably, adding in Part A components in a kind of preparation method of above-mentioned high mode and low mode type flame-resistant terylene industrial yarn
Enter polyester slice and carry out heating melting, fire-retardant master granule is made in slice；Wherein, matter of the macromolecule phosphorus flame retardant in fire-retardant master granule
Amount ratio 20~50%；Wherein polyester slice is that (a kind of polyesters are new by PET, PBT (polybutylene terephthalate (PBT)) or PTT
One or more of fiber type, it is the fiber as made of terephthalic acid (TPA) and 1,3- propylene glycol polycondensation).
Preferably, the drying of the step of preparation method of above-mentioned high mode and low mode type flame-resistant terylene industrial yarn (3) a kind of
In the process, by raw material in rotary drum vacuum drying, vacuum degree≤30Pa, 90~120 DEG C of drying temperature.
Preferably, the melting of the step of preparation method of above-mentioned high mode and low mode type flame-resistant terylene industrial yarn (4) a kind of
In the process, spinning manifold is heated with biphenyl.
Preferably, the stretching of the step of preparation method of above-mentioned high mode and low mode type flame-resistant terylene industrial yarn (7) a kind of
Cheng Qian is crossed, is oiled to tow, the finish is by monohydric alcohol fatty acid, polyol fatty acid, organic phosphate, dimethyl-silicon
Oxygen alkane or polysiloxanes, potassium oleate, fatty acid composition, the mass ratio of each component are as follows:
Organic phosphate therein are as follows: methylene phosphonic acid potassium, methylene phosphonic acid sodium, methylene phosphonic acid magnesium, di 2 ethylhexyl phosphonic acid potassium, three
Phosphonic acids potassium, tetra methylene phosphonic acid potassium, penta methylene phosphonic acid potassium, di 2 ethylhexyl phosphonic acid sodium, tri methylene phosphonic acid sodium, tetra methylene phosphonic acid sodium, penta methylene phosphonic acid sodium, di 2 ethylhexyl phosphonic acid magnesium, tri methylene phosphonic acid
One or more of magnesium, tetra methylene phosphonic acid magnesium, penta methylene phosphonic acid magnesium.
As more preferably selecting, the composition of finish and the mass ratio of each component are as follows:
Organic phosphate therein are as follows: one of methylene phosphonic acid potassium, di 2 ethylhexyl phosphonic acid potassium, penta methylene phosphonic acid potassium.
Preferably, the step of preparation method of above-mentioned a kind of high mode and low mode type flame-resistant terylene industrial yarn (7), stretched
Cheng Hou makes tow generate network node on tow by network nozzle under the action of level pressure sky.
High molecular weight flame retardant described in the fire-retardant slice that the present invention uses is a kind of macromolecule containing P elements, it is high
Can react with molten originally crosslink of PET when temperature melting, graft it completely in PET molecule, fusing point has reached 255 DEG C, and
The fusing point of existing CEPPA fire-retardant slice is only 238 DEG C.The thermal degradation rate of PET at high temperature can be made to decline to a great extent, it is resulting
Melt has excellent tension property and heat resistance.
The utility model has the advantages that the spinning oil that the present invention uses be with foreign vendor cooperative development it is special in production terylene industrial
Yarn spinning oil agent, has good rub resistance, and coherent can greatly reduce the production stretched with lousiness in rear weaving process
It is raw.
Specific embodiment
Implementation of the invention is illustrated below:
Embodiment 1
Raw material is determined first:
Component A: macromolecule phosphorus flame retardant, design parameter are as follows: molecular weight 40000~100000, phosphorus content: 8~12%,
Tg；100~105 DEG C；The macromolecule phosphorus flame retardant is a kind of containing polyphosphonate carbonates altogether, and polyphosphonates are copolymerized phosphine
Acid esters it is one or more, be formed by scion grafting to PET strand；
Component B: the viscous PET slice of height, design parameter are as follows: special industry viscosity is 1.10~1.20dl/g, and the viscous PET slice of height includes
There are light and/or micro- delustring slice TiO greatly2≤ 0.5%；
(2) mixed process: component A is mixed with component B, component A account for mixing after raw material mass ratio be 7~10%,
Its viscosity is 1.0~1.20dl/g, 5000~9000PPM of phosphorus content；
(3) drying process: mixed raw material in step (2) is dried；
(4) melting process: by step (3) through dry feedstock in N2Under protection, to original within the scope of 265 DEG C~310 DEG C
Material carries out heating melting, enters back into spinning manifold, and the temperature of spinning manifold is controlled at 265~310 DEG C；
(5) measure spinning process: the melt through abundant melting carries out spinning by metering pump；
(6) be cooled and shaped: the spinning sprayed through spinneret orifice carries out being cooled to tow, cooling wind control temperature through ring blowing cooling wind
Degree is 40~65 DEG C；
(7) drawing process: carrying out stretching and thermal finalization for tow after cooling, stretches total multiplying power 1.5~3.0, sizing temperature
235 DEG C~260 DEG C of degree；
(8) winding process: control winding speed 4000m/min~6500m/min.Speed control in winding process is direct
The last performance of product is influenced, although this speed may be implemented, to the causality between the speed and properties of product
The prior understanding of technical staff is needed, can just go to realize the speed consciously.
By product obtained by this method, the result through detecting is as follows:
This it appears that its intensity of flame-resistant terylene industrial yarn produced by the invention is apparently higher than and is hindered using CEPPA from table
The polyester industrial yarn of combustion slice spinning.
Embodiment 2
On the basis of embodiment 1, PET slice is added in component A and carries out heating melting, fire-retardant master granule is made in slice；Its
In, the mass ratio being added in PET slice, PBT or the PTT of component A is the characteristic that 30%~40%, PET of component A is sliced
Viscosity are as follows: 0.66~0.68dl/g；Then component A is mixed with component B, component A account for mixing after raw material mass ratio be 7~
10%, viscosity is 1.0~1.20dl/g, 6000~8000PPM of phosphorus content；In the drying process of step (3), raw material is being turned
Vacuum drying in drum, vacuum degree≤30Pa, 105 DEG C of drying temperature；During the melting of step (4), spinning manifold biphenyl
Heating.
Example products obtained therefrom is after tested, it may have good performance advantage, all aspects of the parameters are similar to table in embodiment 1.
Embodiment 3-7
In embodiment, it before the drawing process of step (7), oiling to tow, the finish is sour by monohydric alcohol fatty,
Polyol fatty acid, organic phosphate, dimethyl siloxane or polysiloxanes, potassium oleate, fatty acid composition, the quality of each component
Ratio is as follows:
Above-described embodiment 3 --- 7 through testing acquired results, compared with existing product, has better performance.Wherein implement
The comprehensive performance of example 7 is best.
Organic phosphate therein are as follows: methylene phosphonic acid potassium, methylene phosphonic acid sodium, methylene phosphonic acid magnesium, di 2 ethylhexyl phosphonic acid potassium, three
Phosphonic acids potassium, tetra methylene phosphonic acid potassium, penta methylene phosphonic acid potassium, di 2 ethylhexyl phosphonic acid sodium, tri methylene phosphonic acid sodium, tetra methylene phosphonic acid sodium, penta methylene phosphonic acid sodium, di 2 ethylhexyl phosphonic acid magnesium, tri methylene phosphonic acid
One or more of magnesium, tetra methylene phosphonic acid magnesium, penta methylene phosphonic acid magnesium.
Further, after step (7) drawing process, tow is made under the action of level pressure sky by network nozzle to tow
Network node is generated, the coherent of tow can be increased.
Claims (7)
1. a kind of preparation method of high mode and low mode type flame-resistant terylene industrial yarn, which is characterized in that include the following steps:
(1) raw material is selected
Component A: macromolecule phosphorus flame retardant, design parameter are as follows: molecular weight 40000~100000, phosphorus content: 8~12%, Tg；
100~105 DEG C；The macromolecule phosphorus flame retardant is a kind of containing polyphosphonate carbonates altogether, and polyphosphonates are copolymerized phosphonate ester
It is one or more, be formed by scion grafting to PET strand；
Component B: the viscous PET slice of height, design parameter are as follows: special industry viscosity is 1.10~1.20dl/g, and the viscous PET slice of height includes having greatly
Light and/or micro- delustring are sliced TiO2≤ 0.5%；
(2) mixed process: component A is mixed with component B, component A account for mixing after raw material mass ratio be 5~10%, glue
Degree is 1.0~1.20dl/g, 5000~9000PPM of phosphorus content；
(3) drying process: mixed raw material in step (2) is dried；
(4) melting process: by step (3) through dry feedstock in N2Under protection, raw material is carried out within the scope of 265 DEG C~310 DEG C
Melting is heated, is entered back into spinning manifold, the temperature of spinning manifold is controlled at 265~310 DEG C；
(5) measure spinning process: the melt through abundant melting carries out spinning by metering pump；
(6) be cooled and shaped: the spinning sprayed through spinneret orifice be cooled to tow by ring blowing cooling wind, cooling wind controlled at
40~65 DEG C；
(7) drawing process: tow after cooling is subjected to stretching and thermal finalization, stretches total multiplying power 1.5~3.0, setting temperature 235
DEG C~260 DEG C；
(8) winding process: control winding speed 4000m/min~6500m/min.
2. a kind of preparation method of high mode and low mode type flame-resistant terylene industrial yarn according to claim 1, which is characterized in that A
Polyester slice is added in component and carries out heating melting, fire-retardant master granule is made in slice；Wherein, macromolecule phosphorus flame retardant is in fire-retardant mother
Mass ratio 20~50% in grain；Wherein polyester slice is one or more of PET, PBT or PTT.
3. a kind of preparation method of high mode and low mode type flame-resistant terylene industrial yarn according to claim 1, which is characterized in that step
Suddenly in the drying process of (3), by raw material in rotary drum vacuum drying, vacuum degree≤30Pa, 90~120 DEG C of drying temperature.
4. a kind of preparation method of high mode and low mode type flame-resistant terylene industrial yarn according to claim 1, which is characterized in that step
Suddenly during the melting of (4), spinning manifold is heated with biphenyl.
5. a kind of preparation method of high mode and low mode type flame-resistant terylene industrial yarn according to claim 1, which is characterized in that step
Suddenly it before the drawing process of (7), oils to tow, the finish is by monohydric alcohol fatty acid, polyol fatty acid, organic phosphoric acid
Salt, dimethyl siloxane or polysiloxanes, potassium oleate, fatty acid composition, the mass ratio of each component are as follows:
Organic phosphate therein are as follows: methylene phosphonic acid potassium, methylene phosphonic acid sodium, methylene phosphonic acid magnesium, di 2 ethylhexyl phosphonic acid potassium, tri methylene phosphonic acid
Potassium, tetra methylene phosphonic acid potassium, penta methylene phosphonic acid potassium, di 2 ethylhexyl phosphonic acid sodium, tri methylene phosphonic acid sodium, tetra methylene phosphonic acid sodium, penta methylene phosphonic acid sodium, di 2 ethylhexyl phosphonic acid magnesium, tri methylene phosphonic acid magnesium, four
One or more of phosphonic acids magnesium, penta methylene phosphonic acid magnesium.
6. a kind of preparation method of high mode and low mode type flame-resistant terylene industrial yarn according to claim 5, which is characterized in that institute
The mass ratio of the composition and each component of stating finish is as follows:
Organic phosphate therein are as follows: one of methylene phosphonic acid potassium, di 2 ethylhexyl phosphonic acid potassium, penta methylene phosphonic acid potassium.
7. a kind of preparation method of high mode and low mode type flame-resistant terylene industrial yarn according to claim 1, which is characterized in that step
After (7) drawing process, so that tow is generated network node under the action of level pressure sky by network nozzle on tow suddenly.
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| CN113403700A (en) * | 2021-05-27 | 2021-09-17 | 广东大红马纺织新材料有限公司 | Flame-retardant FDY spinning process |
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| CN113403700A (en) * | 2021-05-27 | 2021-09-17 | 广东大红马纺织新材料有限公司 | Flame-retardant FDY spinning process |
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Application publication date: 20190823 |