CN110241475A - A kind of preparation method of low-shrinkage type flame-resistant terylene industrial yarn - Google Patents
A kind of preparation method of low-shrinkage type flame-resistant terylene industrial yarn Download PDFInfo
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- CN110241475A CN110241475A CN201910448037.3A CN201910448037A CN110241475A CN 110241475 A CN110241475 A CN 110241475A CN 201910448037 A CN201910448037 A CN 201910448037A CN 110241475 A CN110241475 A CN 110241475A
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- phosphonic acid
- methylene phosphonic
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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
- 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
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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
- 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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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
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Abstract
The invention discloses a kind of macromolecular fibre production technical fields, more particularly to a kind of preparation method of low-shrinkage 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., low-shrinkage type flame-resistant terylene industrial yarn is finally obtained.It is an advantage of the invention that have good rub resistance, coherent, can greatly reduce stretch and rear weaving process in lousiness generation, the features such as low-shrinkage, halogen-free environmental, 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 low-shrinkage type flame-resistant terylene industrial yarn
Preparation method.
Background technique
Low-shrinkage type flame-resistant terylene industrial yarn is mainly used in tarpaulin, lamp box advertisement material, coating cloth, and airbag fabric etc. is wanted
Ask intensity high, xeothermic contraction is low, and 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 is only in yarn
Fire retardant is contained on line surface, and in rear weaving, due to by high temperature during arrangement, solvent, the influence of the processes such as friction, fire retardant is easy
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 can achieve 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 during silk, to affect spinnability and tensile property.The method oxygen index (OI) of current application CEPPA
(LOI) 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-resistance
Polyester industrial yarn is fired, and lousiness, broken end are also apparently higher than the non-flame resistant polyester industrial yarn of similar product.Due to the low of intensity and
Lousiness is more, increases the cost and difficulty of rear road application, also limits 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 low-shrinkage 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 lousiness
The features such as few.
A kind of low-shrinkage type flame-resistant terylene industrial yarn Denier range of the present invention includes: 250dtex~3000dtex, single
Thickness (fiber number/hole count) DPF range of root silk includes 2~10 polyester industrial yarn.Its breaking strength range: 6.0~7.5cN/
Dtex, extension at break range: 15.0~30.0%, dry-hot shrinkage (190 DEG C of * 15min*0.01cN/dtex): 1.5~
6.0%, limit oxygen index (LOI) >=32.0%.
The present invention is achieved by following technical proposals:
A kind of preparation method of low-shrinkage 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；
B component: the viscous PET slice of height, inherent viscosity are as follows: 0.95~1.10dl/g, the viscous PET slice of height includes big bright chip
And/or TiO2Less than 0.5% micro- delustring slice；Wherein PET is a kind of abbreviation of poly terephthalic acid class plastics；
(2) mixed process: component A is mixed with B component, and component A accounts for the mass ratio of raw material after mixing are as follows: and 5~10%,
Its viscosity is 0.95~1.10dl/g, 5000~9000PPM of phosphorus content；Wherein 6000~8000PPM of phosphorus content is preferable；A group
Part accounts for the mass ratio of raw material after mixing are as follows: more preferable when 7~8%；
(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；
(6) be cooled and shaped: the spinning sprayed through spinneret orifice carries out being cooled to tow through side cooling wind, and cooling wind controls temperature
It is 18~25 DEG C；
(7) drawing process: tow after cooling is subjected to stretching and thermal finalization, stretches total multiplying power 5~7, setting temperature 200
DEG C~230 DEG C；
(8) winding process: control winding speed 2000m/min~3000m/min.
It is cut preferably, polyester is added in a kind of preparation method of above-mentioned low-shrinkage type flame-resistant terylene industrial yarn in component A
Piece carries out heating melting, and fire-retardant master granule is made in slice；Wherein, mass ratio 20 of the macromolecule phosphorus flame retardant in fire-retardant master granule
~50%；Wherein polyester slice be PET, PBT (polybutylene terephthalate (PBT)) or PTT (a kind of polyesters tencel,
One or more of it is the fiber as made of terephthalic acid (TPA) and 1,3- propylene glycol polycondensation).
Preferably, the drying process of the step of preparation method of above-mentioned low-shrinkage type flame-resistant terylene industrial yarn (3) a kind of
In, by raw material in rotary drum vacuum drying, vacuum degree≤30Pa, 90~120 DEG C of drying temperature.Preferably, above-mentioned one
During the melting of the step of preparation method of kind low-shrinkage type flame-resistant terylene industrial yarn (4), spinning manifold is heated with biphenyl.
Preferably, the drawing process of the step of preparation method of above-mentioned low-shrinkage type flame-resistant terylene industrial yarn (7) a kind of
Before, it oils to tow, the finish is by monohydric alcohol fatty acid, polyol fatty acid, organic phosphate, 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, 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 drawing process of the step of preparation method of above-mentioned low-shrinkage type flame-resistant terylene industrial yarn (7) a kind of
Afterwards, tow is made to generate network node under the action of level pressure sky by network nozzle on tow, to increase the coherent of tow.
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
Temperature melting Shi Nengyu PET melt crosslinks reaction, grafts it in PET molecule completely, and 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 is set to decline to a great extent, this uses institute
The melt obtained has excellent tension property and heat resistance.
The utility model has the advantages that the spinning oil that the present invention uses has good antifriction in production terylene industrial yarn spinning oil agent
Wiping property, coherent can greatly reduce the generation stretched with lousiness in rear weaving process, low-shrinkage, halogen-free environmental, flame retardant property
Well, the features such as spinning lousiness is few.
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；
B component: the viscous PET slice of height, inherent viscosity are as follows: 0.95~1.10dl/g, the viscous PET slice of height includes big bright chip
And/or TiO2Less than 0.5% micro- delustring slice；
Wherein fiber polyester chip is by wherein delustering agent TiO2Content different can be divided into again: it is super to there is light (to have greatly
Light), have light, be semi-dull, (complete) delustring polyester slice.In addition there are also cationic polyesters to be sliced；
(2) mixed process: component A is mixed with B component, and component A accounts for the mass ratio of raw material after mixing are as follows: and 7~10%,
Its viscosity is 0.95~1.10dl/g, 5000~9000PPM of phosphorus content；Preferable mixed proportion is 8%；
(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 through side cooling wind, and cooling wind controls temperature
It is 18~25 DEG C；
(7) drawing process: tow after cooling is subjected to stretching and thermal finalization, stretches total multiplying power 5~7, setting temperature 230
DEG C~260 DEG C；
(8) winding process: control winding speed 2000m/min~3000m/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；
Wherein, the mass ratio that one or more of PET slice, PBT or PTT of component A is added is the 30%~40% of component A
In range, the inherent viscosity of PET slice are as follows: within the scope of 0.66~0.68dl/g；In the drying process of step (3), raw material is existed
Vacuum drying in rotary drum, vacuum degree≤30Pa, 105 DEG C of drying temperature；During the melting of step (4), spinning manifold connection
Benzene 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, tow is made to generate network node under the action of level pressure sky by network nozzle on tow, to increase
The coherent of tow.
Claims (7)
1. a kind of preparation method of low-shrinkage 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；
B component: the viscous PET slice of height, inherent viscosity are as follows: 0.95~1.10dl/g, the viscous PET slice of height include big bright chip and/
Or TiO2 is sliced less than 0.5% micro- delustring；
(2) mixed process: component A is mixed with B component, and component A accounts for the mass ratio of raw material after mixing are as follows: and 5~10%, it glues
Degree is 0.95~1.10dl/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 carries out being cooled to tow through side cooling wind, and cooling wind is controlled at 18
~25 DEG C；
(7) drawing process: tow after cooling stretch and thermal finalization, stretches total multiplying power 5~7, and 230 DEG C of setting temperature~
260℃；
(8) winding process: control winding speed 2000m/min~3000m/min.
2. a kind of preparation method of low-shrinkage type flame-resistant terylene industrial yarn according to claim 1, which is characterized in that component A
Middle addition polyester slice carries out heating melting, and fire-retardant master granule is made in slice；Wherein, macromolecule phosphorus flame retardant is in fire-retardant master granule
Mass ratio 20~50%；Wherein polyester slice is one or more of PET, PBT or PTT.
3. a kind of preparation method of low-shrinkage type flame-resistant terylene industrial yarn according to claim 1, which is characterized in that step
(3) in drying process, 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 low-shrinkage type flame-resistant terylene industrial yarn according to claim 1, which is characterized in that step
(4) during melting, spinning manifold is heated with biphenyl.
5. a kind of preparation method of low-shrinkage type flame-resistant terylene industrial yarn according to claim 1, which is characterized in that step
(7) it before drawing process, 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 low-shrinkage type flame-resistant terylene industrial yarn according to claim 5, which is characterized in that the oil
The composition of agent 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.
7. a kind of preparation method of low-shrinkage type flame-resistant terylene industrial yarn according to claim 1, which is characterized in that step
(7) after drawing process, tow is made to generate network node under the action of level pressure sky by network nozzle on tow, to increase
The coherent of tow.
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| CN111926398A (en) * | 2020-06-22 | 2020-11-13 | 湖州市中跃化纤有限公司 | Technological method of super-elastic flame-retardant coarse denier porous PET-DTY |
| WO2020238686A1 (en) * | 2019-05-27 | 2020-12-03 | 浙江海利得新材料股份有限公司 | Preparation method for low-shrinkage flame-retardant polyester industrial yarns |
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Application publication date: 20190917 |