CN107574502A - A kind of preparation method of high density fabric superfine denier terylene FDY filament - Google Patents
A kind of preparation method of high density fabric superfine denier terylene FDY filament Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of high density fabric superfine denier terylene FDY filament, first by the benzene sulfonic acid sodium salt of DMIP 5, ester exchange reaction is carried out after ethylene glycol and catalyst mixing, reaction adds ethylene glycol after terminating, ethylene glycol sodium and sulfuric acid are modulated, again by terephthalic acid (TPA), ethylene glycol, esterification is carried out after catalyst and stabilizer mixing, then product made from modulation after ester exchange reaction is added in the reaction system for having reached esterification terminal and carries out the obtained spinning melt of polycondensation reaction, last spinning melt is through metering, extrusion, cooling, oil, stretching, high density fabric superfine denier terylene FDY filament is made in thermal finalization and winding.The inventive method reduces the generation of the impurity in polyester FDY filament production process, so as to reduce the pressure liter of filament spinning component and filter, its service life is extended, ensure that the continuity and security of whole production procedure, there is good economic value and promotional value.
Description
Technical field
The invention belongs to Direct-spinning of PET Fiber field, is related to a kind of preparation method of high density fabric superfine denier terylene FDY filament.
Background technology
High density fabric, refer to that one kind used relatively low through weft yarn raw material yarn number and that its thread count is very big is knitted during fabric production
Thing.Density has through close and filling density point, and general yarn count is thinner, and the density that may accomplish is bigger, so high density fabric is past
Toward being that this kind of bafta lines is fine and closely woven premised on height props up, feel is thin refreshing and not penetrating, belong to high-grade fabric category.By change
When fine filament yarn fabric produce reality and application thereof carrys out Definition of Division fabric, be accustomed to by fiber number 50D (55.5dtex) below and warp
Close plus filling density regards as high branch (low denier) high density fabric in 1200/10cm and the above fabric.
The raw material for being generally used for weaving high density fabric is terylene, and terylene has fracture strength and modulus of elasticity height, returned
Elasticity is moderate, thermal finalization is excellent, heat-resisting light resistance is good and a series of premium properties such as acid-fast alkali-proof good corrosion resistance, in addition,
Fabric also has the advantages that crease-resistant money and the stiffness of exempting from is good, thus high density fabric is widely used in the fields such as clothes and home textile.But
Because polyester fiber has the characteristics such as high-crystallinity, high-orientation and high glass transition temperature, in situation existing for normal pressure carrier-free
Lower dyestuff difficulty is diffused into PET molecules, and dyeing is difficult, and therefore, the dyeing of PET need to be in HTHP or with the presence of carrier
In the case of carry out, also because highly dense super fine denier pck count is high, tightness is high, and yarn count is thin, causes its not easy dyeing, easily
The wrinkle that occur being difficult to eliminate, cut marks and drag dirt, it will often carry out cutting across processing in product inspection and produce more short
Code drop etc., has severely impacted the quality of product.
Cationic dye capable of dyeing PET sections (CDP) are to introduce third component in PET macromolecular chain to be allowed to formed
Copolymer, which overcome the achromatic shortcoming of terylene, have become has after light and semi-dull PET sections again at present after big
One important PET kinds, wherein third component typically contain the sodium group-SO of highly acid3Na, sodium group can be with sun
Ionic dye chemically reacts, and has compatibility to it, dyestuff is easily fastened on fiber, and the fabric after dyeing has
Bright, chromatogram are complete, dye-uptake is high and washing after the advantages that fugitive color does not fade, can fully meet that the modern life is various
The demand of change, therefore, cationic dye capable of dyeing PET is developed rapidly in recent years.
Yet with the addition of third component in CDP melts, its apparent viscosity is larger, caused impurity in production process
Accordingly increase, cause part filament spinning component pressure and filter the pressure difference rate of climb it is very fast, while have in inner-walls of duct
Coking material generation is carbonized, these charing coking materials are adhered to inner-walls of duct, easily cause the blocking of pipe-line system, and be not easy clear
Remove, very big difficulty is brought to pipe-dredging work, in addition, filter service life is big during this kind of fiber is produced
Width reduces, general only one week, and the service life of some other filament spinning components typically only has 10 days, thus just needs continually
Filament spinning component is cleaned and changed, so can not only increase operating cost, but also the continuous of whole production procedure can be influenceed
Property and security.
Therefore, need badly and work out a kind of caused high density fabric super fine denier that can effectively reduce impurity in production process
The preparation method of polyester FDY filament.
The content of the invention
In high density fabric with superfine denier terylene FDY filament production process, in order to improve the dye-uptake of polyester FDY filament often
Addition carries sulfonic group-SO3 -Third component, sulfonic group-SO3 -Architectural feature be：1) sulfonic acid-SO3 -Base has three oxygen originals
Son, it both can form the higher complex of structural dimensions by upper connection metal ion from different directions, hydrogen can also be used as
The acceptor of key receives three hydrogen bonds simultaneously in different orientation, forms the hydrogen bond of diversity；2) sulfonic group has stronger suction
Electronic capability, pi-electron density on phenyl ring can be reduced, can strengthen the Electricity Functional property of its metal complex, easily form hole
Shape complex；3) sulfonic complex formability is adjustable.Sulfonic group-SO3 -From the metal ion coordination mode that to share kind more than ten different, energy
It is coordinated with metal and transition metal.
High density fabric often adds Sb series catalysts (antimony glycol or oxidation with superfine denier terylene FDY filament polymerization stage
Antimony), addition is generally terephthalic acid (TPA) ten thousand/several, and Sb content is very high in coking material, it is evident that these Sb
Should all in catalyst, metal Sb enrichment be due to antimony ion in Sb series catalysts easily and third component
And/or sulfonic group-the SO in polymer3 -Caused by complex being combined to form by way of coordinate bond, once antimony ion
With sulfonic group-SO3 -It is enriched with a manner of mating reaction and may result in impurity in spinning melt and increase, in melt pipe inwall
Generation charing coking material, causes the blocking of pipe-line system, and this slightly solubility for carbonizing coking material brings non-to pipe-dredging work
Often big difficulty, while members pressure, the filter differential pressure rate of climb are very fast, have had a strong impact on filter and some components
Service life, the service life of filter is only one week, and the service life of component is only 10 days or so.Wash number and component
The increase of frequency is changed, can not only increase operating cost, but also the continuity and security of whole production procedure can be influenceed.
And high density fabric superfine denier terylene FDY filament, because line density is small, total fiber number is often less than 10dtex, thus spinning difficulty is big,
Requirement to spinning melt is high, reduces impurity level in melt, improves its spinnability and just seem extremely important, therefore, reduces this
The generation of impurity turns into the key point of high density fabric superfine denier terylene FDY filament spinning.
The invention aims to overcome above-mentioned problems of the prior art, there is provided one kind can effectively reduce life
The preparation method of the caused high density fabric superfine denier terylene FDY filament of impurity during production.
In order to achieve the above object, the technical solution adopted by the present invention is：
A kind of preparation method of high density fabric superfine denier terylene FDY filament, step are as follows：
A) spinning melt is prepared；
(1) ester exchange reaction is carried out after mixing DMIP -5- benzene sulfonic acid sodium salts, ethylene glycol and catalyst,
Reaction adds ethylene glycol, ethylene glycol sodium and sulfuric acid after terminating and is modulated；
The purpose that ethylene glycol is added after ester exchange reaction is for adjusting the double hydroxyl ethyl ester -5- sodium sulfonates of M-phthalic acid
(SIPE) percentage concentration in ethylene glycol solution, because when the concentration of the double hydroxyl ethyl ester -5- sodium sulfonates (SIPE) of M-phthalic acid
It can be precipitated during more than 40wt%, be unfavorable for the progress of subsequent reactions；High density fabric superfine denier terylene FDY in the prior art
The catalyst that uses of silk polymerization stage is generally antimony glycol or antimony oxide, and the antimony ion in catalyst in PET sections with introducing
Third component in sulfonic acid group can often occur coordination chemistry formed complex, complex is further with the 3rd group
The raw self-polymeric reaction of distribution is deposited on pipe surface and spinneret so as to generate coking material, is formed and blocked, second two in the present invention
Sodium alkoxide can provide a certain amount of coexisting ion that competitive relation with antimony ion be present, influence and weaken antimony ion and sulfonic acid group
Coordination, effectively reduce the complex that sulfonic acid group and catalyst are formed by coordination, that is, reduce in spinning melt
Impurity, the good mobile performance of polyester is maintained, and then ensure that the spinnability of high density fabric superfine denier terylene FDY filament；Sulphur
H in acid+The formation that can be reacted with sulfonic group to complex has an impact, due to H+Presence, sulfonic acid group is produced coordination anti-
The ability answered declines, and this case can be described as Radiation grafting, H+Concentration it is bigger, Radiation grafting is more obvious, and a certain amount of acid can be reduced
The formation of complex, but measure the excessive heat endurance for influencing whether polyester.The addition of a certain amount of sulfuric acid can reduce complex
Generation, make the flowing that polyester is more stable.
(2) esterification is carried out after mixing terephthalic acid (TPA), ethylene glycol, catalyst and stabilizer；
The addition of stabilizer can effectively reduce the side reaction in polyester esterification course of reaction；
(3) product of (1) is added in (2) and carries out the obtained spinning melt of polycondensation reaction；
B) spinning；
Spinning melt is through measuring, extruding, cooling down, oiling, stretching, thermal finalization and winding are made high density fabric and washed with super fine denier
Synthetic fibre FDY silks.
As preferable technical scheme：
A kind of preparation method of high density fabric superfine denier terylene FDY filament as described above, prepares the specific of spinning melt
Step is as follows：
(1) ester exchange reaction prepares the double hydroxyl ethyl ester -5- sodium sulfonates of M-phthalic acid；
DMIP -5- benzene sulfonic acid sodium salts and ethylene glycol input are prepared in kettle, add catalyst Z n (Ac)2Afterwards
Carry out terminating when ester exchange reaction reaches more than the 90% of theoretical value to the quantity of distillate of water at 175~185 DEG C, obtain isophthalic two
Double hydroxyl ethyl ester -5- the sodium sulfonates of formic acid, add ethylene glycol, ethylene glycol sodium and sulfuric acid and are modulated to obtain and contain 30~35wt% isophthalic two
The ethylene glycol solution of the double hydroxyl ethyl ester -5- sodium sulfonates of formic acid；
(2) esterification prepares ethylene glycol terephthalate；
Terephthalic acid (TPA) and ethylene glycol are made into after slurry add catalyst and stabilizer it is well mixed after be esterified it is anti-
Ethylene glycol terephthalate, esterification compressive reaction in nitrogen atmosphere should be obtained, moulding pressure is normal pressure~0.3MPa,
The temperature of esterification is 250~260 DEG C, is esterification when the water quantity of distillate in esterification reaches more than the 90% of theoretical value
Reaction end；
(3) polycondensation reaction prepares spinning melt；
The product of (1) is added in (2), the polycondensation reaction in low vacuum stage, the stage are carried out first under condition of negative pressure
Pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, and reaction temperature is 260~270 DEG C, and the reaction time is 30~50min,
Then proceed to vacuumize the polycondensation reaction for carrying out high vacuum stage of Fig, reaction pressure is down to absolute pressure and be less than 100Pa, reaction temperature
Spend for 275~285 DEG C, the reaction time is 50~90min, and spinning melt is made.
A kind of preparation method of high density fabric superfine denier terylene FDY filament as described above, in step (1), ester exchange is anti-
When should start, the mol ratio of DMIP -5- benzene sulfonic acid sodium salts and ethylene glycol is 10~12:1, catalyst Z n (Ac)2
Addition be DMIP -5- benzene sulfonic acid sodium salt additions 0.2~0.5wt%；
During modulation, the addition of ethylene glycol sodium for DMIP -5- benzene sulfonic acid sodium salt additions 1.5~
6wt%, the mass concentration of the sulfuric acid of addition is 40~60%, and the addition of sulfuric acid is DMIP -5- benzene sulfonic acids
1.5~6wt% of sodium addition.
A kind of preparation method of high density fabric superfine denier terylene FDY filament as described above, in step (2), esterification
During beginning, the mol ratio of terephthalic acid (TPA) and ethylene glycol is 1.10~1.30:1, catalyst be antimony oxide, antimony glycol or
Antimony acetate, the addition of catalyst are 0.01~0.05wt% of terephthalic acid (TPA) addition, and stabilizer is triphenyl phosphate, phosphorus
Sour trimethyl or Trimethyl phosphite, the addition of stabilizer are 0.01~0.05wt% of terephthalic acid (TPA) addition.
A kind of preparation method of high density fabric superfine denier terylene FDY filament as described above, in step (3), polycondensation reaction
During beginning, the mol ratio of the double hydroxyl ethyl ester -5- sodium sulfonates of M-phthalic acid and ethylene glycol terephthalate is 1~3:100.
A kind of preparation method of high density fabric superfine denier terylene FDY filament as described above, in order to adapt in preparation process
The influence that the addition of the materials such as stabilizer, ethylene glycol, sulfuric acid and ethylene glycol sodium is processed to final spinning is, it is necessary to use high density fabric
The spinning technology parameter of superfine denier terylene FDY filament is adjusted, and the technological parameter of the spinning after adjustment is：
Spinning temperature：285~295 DEG C；
Chilling temperature：20~25 DEG C；
Network pressure：0.20~0.30MPa；
One roller speed：1000~1500m/min；
One roll temperature：86~95 DEG C；
Two roller speeds：3820~4200m/min；
Two roll temperatures：117~130 DEG C；
Winding speed：3800~4100m/min.
A kind of preparation method of high density fabric superfine denier terylene FDY filament as described above, in spinning process, filament spinning component
Pressure rise Δ P≤0.8bar/ days, the pressure of filter rises Δ P≤2.9bar/ days, the service life of filament spinning component for 36~
38 days, the service life of filter was 25~27 days.
A kind of preparation method of high density fabric superfine denier terylene FDY filament as described above, the high density fabric is with ultra-fine
The line density of denier terylene FDY filament is 7~8D, and filament number is 0.5~0.7dtex, fracture strength >=3.80cN/dtex, upper dye
Rate is more than 95%.
A kind of preparation method of high density fabric superfine denier terylene FDY filament as described above, the high density fabric is with ultra-fine
The elongation at break of denier terylene FDY filament is 40.0 ± 5.0%, line density deviation ratio≤0.8%, fracture strength CV value≤5.0%,
Extension at break CV value≤10.0%, yarn unevenness CV value≤1.5%.
Beneficial effect：
(1) preparation method of a kind of high density fabric superfine denier terylene FDY filament of the invention, reduces in production process and produces
Raw impurity, so as to reduce the pressure liter of filament spinning component and filter, its service life is extended, reduces production cost,
The continuity and security of whole production procedure are further ensured, there is good economic value and promotional value；
(2) preparation method of a kind of high density fabric superfine denier terylene FDY filament of the invention, ethylene glycol sodium and sulfuric acid
Add, reduce the formation of complex in production process, so as to reduce the impurity in spinning melt, it is good to maintain polyester
Mobile performance, and then ensure that the spinnability of high density fabric superfine denier terylene FDY filament；
(3) preparation method of a kind of high density fabric superfine denier terylene FDY filament of the invention, reduces in melt conveying
During impurity generation, solve high density fabric because yarn count density is too high, production difficulty is big, easily occur evenness fault,
The problem of phenomena such as cloth cover is not bright and clean enough, weavy grain is unclear, fault is more and quality is unstable.
Embodiment
The invention will be further elucidated with reference to specific embodiments.It should be understood that these embodiments are merely to illustrate this hair
Bright rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, art technology
Personnel can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Fixed scope.
Embodiment 1
A kind of preparation method of high density fabric superfine denier terylene FDY filament, step are as follows：
A) spinning melt is prepared；
(1) ester exchange reaction prepares the double hydroxyl ethyl ester -5- sodium sulfonates of M-phthalic acid；
It is 10 first by mol ratio:1 DMIP -5- benzene sulfonic acid sodium salts and ethylene glycol input is prepared in kettle,
Add catalyst Z n (Ac)2Carry out terminating when ester exchange reaction reaches the 90% of theoretical value to the quantity of distillate of water at 175 DEG C, obtain
To the double hydroxyl ethyl ester -5- sodium sulfonates of M-phthalic acid, it is subsequently added into ethylene glycol, ethylene glycol sodium and sulfuric acid and is modulated and is contained
The ethylene glycol solution of the double hydroxyl ethyl ester -5- sodium sulfonates of 30wt% M-phthalic acids, wherein catalyst Z n (Ac)2Addition be isophthalic
The 0.2wt% of dicarboxylic acid dimethyl ester -5- benzene sulfonic acid sodium salt additions, during modulation, the addition of ethylene glycol sodium is M-phthalic acid two
The 1.5wt% of methyl esters -5- benzene sulfonic acid sodium salt additions, the mass concentration of the sulfuric acid of addition is 40%, and the addition of sulfuric acid is isophthalic
The 1.5wt% of dicarboxylic acid dimethyl ester -5- benzene sulfonic acid sodium salt additions；
(2) esterification prepares ethylene glycol terephthalate；
It is 1.10 by mol ratio:1 terephthalic acid (TPA) and ethylene glycol adds antimony oxide and tricresyl phosphate after being made into slurry
Esterification being carried out at 250 DEG C after phenyl ester is well mixed and obtaining ethylene glycol terephthalate, esterification is in nitrogen atmosphere
Middle compressive reaction, moulding pressure are normal pressure, are esterification when the water quantity of distillate in esterification reaches the 90% of theoretical value
The addition of terminal, wherein antimony oxide is the 0.01wt% of terephthalic acid (TPA) addition, and the addition of triphenyl phosphate is
The 0.05wt% of terephthalic acid (TPA) addition；
(3) polycondensation reaction prepares spinning melt；
The product of (1) is added in (2), the polycondensation reaction in low vacuum stage, the stage are carried out first under condition of negative pressure
Pressure is steadily evacuated to absolute pressure 500Pa by normal pressure, and reaction temperature is 260 DEG C, reaction time 30min, then proceedes to take out very
Sky carries out the polycondensation reaction of high vacuum stage of Fig, and it is 99.5Pa reaction pressure is down to absolute pressure, and reaction temperature is 275 DEG C, instead
Be 50min between seasonable, spinning melt be made, when wherein polycondensation reaction starts, M-phthalic acid pair hydroxyl ethyl ester -5- sodium sulfonates with it is right
The mol ratio of PET is 1:100；
B) spinning；
Spinning melt is through measuring, extruding, cooling down, oiling, stretching, thermal finalization and winding are made high density fabric and washed with super fine denier
Synthetic fibre FDY silks；The technological parameter of spinning is：
Spinning temperature：285℃；
Chilling temperature：20℃；
Network pressure：0.20MPa；
One roller speed：1500m/min；
One roll temperature：86℃；
Two roller speeds：3820m/min；
Two roll temperatures：130℃；
Winding speed：3900m/min；
In spinning process, due to the modulation of ethylene glycol, ethylene glycol sodium and sulfuric acid, amount of impurities is greatly reduced in melt,
The pressure liter of filament spinning component and filter is effectively reduced, the wherein pressure of filament spinning component rises Δ P=0.7bar/ days, filter
Pressure rise Δ P=2.7bar/ days, the service life of filament spinning component is 38 days, and the service life of filter is 25 days.
With the line density of superfine denier terylene FDY filament it is 8D by the high density fabric obtained by above-mentioned steps, filament number is
0.6dtex, fracture strength 3.90cN/dtex, dye-uptake 98%, elongation at break 40.0%, line density deviation ratio are
0.6%, fracture strength CV value are 5.0%, and extension at break CV values are 9.5%, and yarn unevenness CV values are 1.4%.
Comparative example 1
High density fabric is carried out in the case of HTHP with superfine denier terylene FDY filament fiber in the prior art, step
It is substantially the same manner as Example 1, unlike, in step (1), without using ethylene glycol, ethylene glycol sodium and sulphur after ester exchange reaction
Acid is modulated.It is 4.3bar/ days that the pressure of filament spinning component, which rises Δ P, during spinning is carried out, and the pressure of filter rises Δ P
For 8.7bar/ days, the service life of filament spinning component was 7 days, and the service life of filter is 10 days.The cation-dyeable prepared
The filament number of polyester fiber is 6.3dtex, fracture strength 2.87cN/dtex, dye-uptake 93.2%, and elongation at break is
34.6%, line density deviation ratio is 0.45%, fracture strength CV values 3.75%, extension at break CV values 7.87%, yarn unevenness
CV values 1.94%, contrast and find with embodiment 1, present invention significantly reduces the pressure of filament spinning component in spinning process and filter
Rise, substantially prolongs its service life, drastically increase production efficiency, reduce cost, properties of product of the invention also obtain
Improved to obvious, there is good economic benefit.
Embodiment 2
A kind of preparation method of high density fabric superfine denier terylene FDY filament, step are as follows：
A) spinning melt is prepared；
(1) ester exchange reaction prepares the double hydroxyl ethyl ester -5- sodium sulfonates of M-phthalic acid；
It is 11 first by mol ratio:1 DMIP -5- benzene sulfonic acid sodium salts and ethylene glycol input is prepared in kettle,
Add catalyst Z n (Ac)2Reach theoretical value with carrying out ester exchange reaction to the quantity of distillate of water after anti-ether agent NaAc at 178 DEG C
92% when terminate, obtain the double hydroxyl ethyl ester -5- sodium sulfonates of M-phthalic acid, be subsequently added into ethylene glycol, ethylene glycol sodium and sulfuric acid and enter
Row modulation obtains the ethylene glycol solution of the double hydroxyl ethyl ester -5- sodium sulfonates of M-phthalic acid containing 31wt%, wherein catalyst Z n (Ac)2's
Addition is the 0.3wt% of DMIP -5- benzene sulfonic acid sodium salt additions, and anti-ether agent NaAc addition is isophthalic two
The 0.13wt% of formic acid dimethyl ester -5- benzene sulfonic acid sodium salt additions；During modulation, the addition of ethylene glycol sodium is M-phthalic acid diformazan
The 2wt% of ester -5- benzene sulfonic acid sodium salt additions, the mass concentration of the sulfuric acid of addition is 45%, and the addition of sulfuric acid is isophthalic diformazan
The 3.5wt% of dimethyl phthalate -5- benzene sulfonic acid sodium salt additions；
(2) esterification prepares ethylene glycol terephthalate；
It is 1.15 by mol ratio:1 terephthalic acid (TPA) and ethylene glycol adds antimony glycol and tripotassium phosphate after being made into slurry
Ester, carry out esterification at 253 DEG C after well mixed and obtain ethylene glycol terephthalate, esterification is in nitrogen atmosphere
Compressive reaction, moulding pressure 0.1MPa, it is esterification when the water quantity of distillate in esterification reaches the 91% of theoretical value
The addition of terminal, wherein antimony glycol is the 0.02wt% of terephthalic acid (TPA) addition, and the addition of trimethyl phosphate is pair
The 0.04wt% of phthalic acid addition；
(3) polycondensation reaction prepares spinning melt；
By in the product (2) of (1), the polycondensation reaction in low vacuum stage, the staged pressure are carried out first under condition of negative pressure
Steadily be evacuated to absolute pressure 490Pa by normal pressure, reaction temperature is 262 DEG C, reaction time 35min, then proceed to vacuumize into
The polycondensation reaction of row high vacuum stage of Fig, reaction pressure is set to be down to absolute pressure 98Pa, reaction temperature is 277 DEG C, and the reaction time is
60min, spinning melt is made, when wherein polycondensation reaction starts, the double hydroxyl ethyl ester -5- sodium sulfonates of M-phthalic acid and terephthalic acid (TPA)
The mol ratio of glycol ester is 1.3:100；
B) spinning；
Spinning melt is through measuring, extruding, cooling down, oiling, stretching, thermal finalization and winding are made high density fabric and washed with super fine denier
Synthetic fibre FDY silks；The technological parameter of spinning is：
Spinning temperature：287℃；
Chilling temperature：21℃；
Network pressure：0.22MPa；
One roller speed：1400m/min；
One roll temperature：88℃；
Two roller speeds：3870m/min；
Two roll temperatures：124℃；
Winding speed：3870m/min；
In spinning process, the pressure of filament spinning component rises Δ P=0.8bar/ days, and the pressure of filter rises Δ P=2.9bar/
My god, the service life of filament spinning component is 37 days, and the service life of filter is 25 days.
With the line density of superfine denier terylene FDY filament it is 7.2D by the high density fabric obtained by above-mentioned steps, filament number is
0.7dtex, fracture strength 3.84cN/dtex, dye-uptake 96.5%, elongation at break 35.0%, line density deviation ratio
For 0.7%, fracture strength CV values are 4.5%, and extension at break CV values are 8.8%, and yarn unevenness CV values are 1.3%.
Embodiment 3
A kind of preparation method of high density fabric superfine denier terylene FDY filament, step are as follows：
A) spinning melt is prepared；
(1) ester exchange reaction prepares the double hydroxyl ethyl ester -5- sodium sulfonates of M-phthalic acid；
It is 12 first by mol ratio:1 DMIP -5- benzene sulfonic acid sodium salts and ethylene glycol input is prepared in kettle,
Add catalyst Z n (Ac)2Reach theoretical value with carrying out ester exchange reaction to the quantity of distillate of water after anti-ether agent NaAc at 179 DEG C
91% when terminate, obtain the double hydroxyl ethyl ester -5- sodium sulfonates of M-phthalic acid, be subsequently added into ethylene glycol, ethylene glycol sodium and sulfuric acid and enter
Row modulation obtains the ethylene glycol solution of the double hydroxyl ethyl ester -5- sodium sulfonates of M-phthalic acid containing 32wt%, wherein catalyst Z n (Ac)2's
Addition is the 0.25wt% of DMIP -5- benzene sulfonic acid sodium salt additions, and anti-ether agent NaAc addition is isophthalic
The 0.15wt% of dicarboxylic acid dimethyl ester -5- benzene sulfonic acid sodium salt additions；During modulation, the addition of ethylene glycol sodium is M-phthalic acid two
The 2.5wt% of methyl esters -5- benzene sulfonic acid sodium salt additions, the mass concentration of the sulfuric acid of addition is 50%, and the addition of sulfuric acid is isophthalic
The 4wt% of dicarboxylic acid dimethyl ester -5- benzene sulfonic acid sodium salt additions；
(2) esterification prepares ethylene glycol terephthalate；
It is 1.20 by mol ratio:1 terephthalic acid (TPA) and ethylene glycol adds antimony acetate and phosphorous acid front three after being made into slurry
Ester, carry out esterification at 255 DEG C after well mixed and obtain ethylene glycol terephthalate, esterification is in nitrogen atmosphere
Compressive reaction, moulding pressure 0.15MPa, it is esterification when the water quantity of distillate in esterification reaches the 92% of theoretical value
The addition of terminal, wherein antimony acetate is the 0.03wt% of terephthalic acid (TPA) addition, and the addition of Trimethyl phosphite is pair
The 0.03wt% of phthalic acid addition；
(3) polycondensation reaction prepares spinning melt；
The product of (1) is added in (2), the polycondensation reaction in low vacuum stage, the stage are carried out first under condition of negative pressure
Pressure is steadily evacuated to absolute pressure 480Pa by normal pressure, and reaction temperature is 264 DEG C, reaction time 40min, then proceedes to take out very
Sky carries out the polycondensation reaction of high vacuum stage of Fig, and it is 98Pa reaction pressure is down to absolute pressure, and reaction temperature is 279 DEG C, reaction
Time is 70min, and spinning melt is made, when wherein polycondensation reaction starts, the double hydroxyl ethyl ester -5- sodium sulfonates of M-phthalic acid with to benzene
The mol ratio of naphthalate is 1.7:100；
B) spinning；
Spinning melt is through measuring, extruding, cooling down, oiling, stretching, thermal finalization and winding are made high density fabric and washed with super fine denier
Synthetic fibre FDY silks；The technological parameter of spinning is：
Spinning temperature：289℃；
Chilling temperature：22℃；
Network pressure：0.24MPa；
One roller speed：1300m/min；
One roll temperature：89℃；
Two roller speeds：3900m/min；
Two roll temperatures：122℃；
Winding speed：4100m/min；
In spinning process, the pressure of filament spinning component rises Δ P=0.7bar/ days, and the pressure of filter rises Δ P=2.9bar/
My god, the service life of filament spinning component is 38 days, and the service life of filter is 26 days.
With the line density of superfine denier terylene FDY filament it is 7.3D by the high density fabric obtained by above-mentioned steps, filament number is
0.57dtex, fracture strength 3.80cN/dtex, dye-uptake 95.8%, elongation at break 35.0%, line density deviation ratio
For 0.8%, fracture strength CV values are 4.1%, and extension at break CV values are 9.0%, and yarn unevenness CV values are 1.5%.
Embodiment 4
A kind of preparation method of high density fabric superfine denier terylene FDY filament, step are as follows：
A) spinning melt is prepared；
(1) ester exchange reaction prepares the double hydroxyl ethyl ester -5- sodium sulfonates of M-phthalic acid；
It is 10.5 first by mol ratio:1 DMIP -5- benzene sulfonic acid sodium salts and ethylene glycol input prepares kettle
In, add catalyst Z n (Ac)2Reach theoretical with carrying out ester exchange reaction to the quantity of distillate of water after anti-ether agent NaAc at 180 DEG C
Value 93% when terminate, obtain the double hydroxyl ethyl ester -5- sodium sulfonates of M-phthalic acid, be subsequently added into ethylene glycol, ethylene glycol sodium and sulfuric acid
It is modulated to obtain the ethylene glycol solution of the double hydroxyl ethyl ester -5- sodium sulfonates of M-phthalic acid containing 33wt%, wherein catalyst Z n (Ac)2
Addition be DMIP -5- benzene sulfonic acid sodium salt additions 0.35wt%, between anti-ether agent NaAc addition is
The 0.2wt% of rutgers -5- benzene sulfonic acid sodium salt additions；During modulation, the addition of ethylene glycol sodium is M-phthalic acid
The 5wt% of dimethyl ester -5- benzene sulfonic acid sodium salt additions, the mass concentration of the sulfuric acid of addition is 55%, and the addition of sulfuric acid is isophthalic
The 4.5wt% of dicarboxylic acid dimethyl ester -5- benzene sulfonic acid sodium salt additions；
(2) esterification prepares ethylene glycol terephthalate；
It is 1.25 by mol ratio:1 terephthalic acid (TPA) and ethylene glycol adds antimony oxide and tricresyl phosphate after being made into slurry
Methyl esters, carry out esterification at 257 DEG C after well mixed and obtain ethylene glycol terephthalate, esterification is in nitrogen atmosphere
Middle compressive reaction, moulding pressure 0.2MPa are anti-for esterification when the water quantity of distillate in esterification reaches the 93% of theoretical value
Answer terminal, the wherein addition of antimony oxide is the 0.04wt% of terephthalic acid (TPA) addition, the addition of trimethyl phosphate
For the 0.02wt% of terephthalic acid (TPA) addition；
(3) polycondensation reaction prepares spinning melt；
The product of (1) is added in (2), the polycondensation reaction in low vacuum stage, the stage are carried out first under condition of negative pressure
Pressure is steadily evacuated to absolute pressure 470Pa by normal pressure, and reaction temperature is 265 DEG C, reaction time 40min, then proceedes to take out very
Sky carries out the polycondensation reaction of high vacuum stage of Fig, and it is 96Pa reaction pressure is down to absolute pressure, and reaction temperature is 280 DEG C, reaction
Time is 70min, and spinning melt is made, when wherein polycondensation reaction starts, the double hydroxyl ethyl ester -5- sodium sulfonates of M-phthalic acid with to benzene
The mol ratio of naphthalate is 2:100；
B) spinning；
Spinning melt is through measuring, extruding, cooling down, oiling, stretching, thermal finalization and winding are made high density fabric and washed with super fine denier
Synthetic fibre FDY silks；The technological parameter of spinning is：
Spinning temperature：293℃；
Chilling temperature：21.5℃；
Network pressure：0.26MPa；
One roller speed：1200m/min；
One roll temperature：90℃；
Two roller speeds：4000m/min；
Two roll temperatures：130℃；
Winding speed：3800m/min；
In spinning process, the pressure of filament spinning component rises Δ P=0.6bar/ days, and the pressure of filter rises Δ P=2.2bar/
My god, the service life of filament spinning component is 36 days, and the service life of filter is 27 days.
With the line density of superfine denier terylene FDY filament it is 8D by the high density fabric obtained by above-mentioned steps, filament number is
0.52dtex, fracture strength 3.91cN/dtex, dye-uptake 95.1%, elongation at break 45.0%, line density deviation ratio
For 0.77%, fracture strength CV values are 4.8%, and extension at break CV values are 10.0%, and yarn unevenness CV values are 1.2%.
Embodiment 5
A kind of preparation method of high density fabric superfine denier terylene FDY filament, step are as follows：
A) spinning melt is prepared；
(1) ester exchange reaction prepares the double hydroxyl ethyl ester -5- sodium sulfonates of M-phthalic acid；
It is 11.5 first by mol ratio:1 DMIP -5- benzene sulfonic acid sodium salts and ethylene glycol input prepares kettle
In, add catalyst Z n (Ac)2Reach theoretical with carrying out ester exchange reaction to the quantity of distillate of water after anti-ether agent NaAc at 182 DEG C
Value 96% when terminate, obtain the double hydroxyl ethyl ester -5- sodium sulfonates of M-phthalic acid, be subsequently added into ethylene glycol, ethylene glycol sodium and sulfuric acid
It is modulated to obtain the ethylene glycol solution of the double hydroxyl ethyl ester -5- sodium sulfonates of M-phthalic acid containing 34wt%, wherein catalyst Z n (Ac)2
Addition be DMIP -5- benzene sulfonic acid sodium salt additions 0.4wt%, anti-ether agent NaAc addition is isophthalic
The 0.13wt% of dicarboxylic acid dimethyl ester -5- benzene sulfonic acid sodium salt additions；During modulation, the addition of ethylene glycol sodium is M-phthalic acid two
The 4wt% of methyl esters -5- benzene sulfonic acid sodium salt additions, the mass concentration of the sulfuric acid of addition is 45%, and the addition of sulfuric acid is isophthalic two
The 5wt% of formic acid dimethyl ester -5- benzene sulfonic acid sodium salt additions；
(2) esterification prepares ethylene glycol terephthalate；
It is 1.30 by mol ratio:1 terephthalic acid (TPA) and ethylene glycol adds antimony glycol and phosphorous acid three after being made into slurry
Methyl esters, carry out esterification at 252 DEG C after well mixed and obtain ethylene glycol terephthalate, esterification is in nitrogen atmosphere
Middle compressive reaction, moulding pressure 0.25MPa are anti-for esterification when the water quantity of distillate in esterification reaches the 94% of theoretical value
Answer terminal, the wherein addition of antimony glycol is the 0.04wt% of terephthalic acid (TPA) addition, the addition of Trimethyl phosphite
For the 0.01wt% of terephthalic acid (TPA) addition；
(3) polycondensation reaction prepares spinning melt；
The product of (1) is added in (2), the polycondensation reaction in low vacuum stage, the stage are carried out first under condition of negative pressure
Pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, and reaction temperature is 268 DEG C, reaction time 45min, is then proceeded to
The polycondensation reaction for carrying out high vacuum stage of Fig is vacuumized, it is 95Pa reaction pressure is down to absolute pressure, and reaction temperature is 282 DEG C,
Reaction time is 80min, and spinning melt is made, when wherein polycondensation reaction starts, the double hydroxyl ethyl ester -5- sodium sulfonates of M-phthalic acid with
The mol ratio of ethylene glycol terephthalate is 2.5:100；
B) spinning；
Spinning melt is through measuring, extruding, cooling down, oiling, stretching, thermal finalization and winding are made high density fabric and washed with super fine denier
Synthetic fibre FDY silks；The technological parameter of spinning is：
Spinning temperature：295℃；
Chilling temperature：23℃；
Network pressure：0.25MPa；
One roller speed：1100m/min；
One roll temperature：93℃；
Two roller speeds：4200m/min；
Two roll temperatures：123℃；
Winding speed：4050m/min；
In spinning process, the pressure of filament spinning component rises Δ P=0.8bar/ days, and the pressure of filter rises Δ P=2.9bar/
My god, the service life of filament spinning component is 36 days, and the service life of filter is 25 days.
With the line density of superfine denier terylene FDY filament it is 7D by the high density fabric obtained by above-mentioned steps, filament number is
0.55dtex, fracture strength 3.80cN/dtex, dye-uptake 96%, elongation at break 40.0%, line density deviation ratio are
0.75%, fracture strength CV value are 4.9%, and extension at break CV values are 10.0%, and yarn unevenness CV values are 1.5%.
Embodiment 6
A kind of preparation method of high density fabric superfine denier terylene FDY filament, step are as follows：
A) spinning melt is prepared；
(1) ester exchange reaction prepares the double hydroxyl ethyl ester -5- sodium sulfonates of M-phthalic acid；
It is 12 first by mol ratio:1 DMIP -5- benzene sulfonic acid sodium salts and ethylene glycol input is prepared in kettle,
Add catalyst Z n (Ac)2Reach theoretical value with carrying out ester exchange reaction to the quantity of distillate of water after anti-ether agent NaAc at 185 DEG C
94% when terminate, obtain the double hydroxyl ethyl ester -5- sodium sulfonates of M-phthalic acid, be subsequently added into ethylene glycol, ethylene glycol sodium and sulfuric acid and enter
Row modulation obtains the ethylene glycol solution of the double hydroxyl ethyl ester -5- sodium sulfonates of M-phthalic acid containing 35wt%, wherein catalyst Z n (Ac)2's
Addition is the 0.5wt% of DMIP -5- benzene sulfonic acid sodium salt additions, and anti-ether agent NaAc addition is isophthalic two
The 0.2wt% of formic acid dimethyl ester -5- benzene sulfonic acid sodium salt additions；During modulation, the addition of ethylene glycol sodium is M-phthalic acid diformazan
The 6wt% of ester -5- benzene sulfonic acid sodium salt additions, the mass concentration of the sulfuric acid of addition is 60%, and the addition of sulfuric acid is isophthalic diformazan
The 6wt% of dimethyl phthalate -5- benzene sulfonic acid sodium salt additions；
(2) esterification prepares ethylene glycol terephthalate；
It is 1.25 by mol ratio:1 terephthalic acid (TPA) and ethylene glycol adds antimony acetate and triphenyl phosphate after being made into slurry,
Esterification being carried out at 260 DEG C after well mixed and obtaining ethylene glycol terephthalate, esterification adds in nitrogen atmosphere
Pressure reaction, moulding pressure 0.3MPa are whole for esterification when the water quantity of distillate in esterification reaches the 90% of theoretical value
The addition of point, wherein antimony acetate is the 0.05wt% of terephthalic acid (TPA) addition, and the addition of triphenyl phosphate is to benzene two
The 0.35wt% of formic acid addition；
(3) polycondensation reaction prepares spinning melt；
The product of (1) is added in (2), the polycondensation reaction in low vacuum stage, the stage are carried out first under condition of negative pressure
Pressure is steadily evacuated to absolute pressure 500Pa by normal pressure, and reaction temperature is 270 DEG C, reaction time 50min, then proceedes to take out very
Sky carries out the polycondensation reaction of high vacuum stage of Fig, and it is 94Pa reaction pressure is down to absolute pressure, and reaction temperature is 285 DEG C, reaction
Time is 90min, and spinning melt is made, when wherein polycondensation reaction starts, the double hydroxyl ethyl ester -5- sodium sulfonates of M-phthalic acid with to benzene
The mol ratio of naphthalate is 3:100；
B) spinning；
Spinning melt is through measuring, extruding, cooling down, oiling, stretching, thermal finalization and winding are made high density fabric and washed with super fine denier
Synthetic fibre FDY silks；The technological parameter of spinning is：
Spinning temperature：291℃；
Chilling temperature：25℃；
Network pressure：0.30MPa；
One roller speed：1000m/min；
One roll temperature：95℃；
Two roller speeds：4160m/min；
Two roll temperatures：117℃；
Winding speed：3900m/min；
In spinning process, the pressure of filament spinning component rises Δ P=0.7bar/ days, and the pressure of filter rises Δ P=2.85bar/
My god, the service life of filament spinning component is 36 days, and the service life of filter is 26 days.
With the line density of superfine denier terylene FDY filament it is 7.8D by the high density fabric obtained by above-mentioned steps, filament number is
0.5dtex, fracture strength 3.83cN/dtex, dye-uptake 95.6%, elongation at break 35.0%, line density deviation ratio
For 0.8%, fracture strength CV values are 5.0%, and extension at break CV values are 9.2%, and yarn unevenness CV values are 1.3%.
Claims (9)
1. a kind of preparation method of high density fabric superfine denier terylene FDY filament, it is characterized in that, step is as follows：
A) spinning melt is prepared；
(1) ester exchange reaction is carried out after mixing DMIP -5- benzene sulfonic acid sodium salts, ethylene glycol and catalyst, is reacted
Ethylene glycol, ethylene glycol sodium and sulfuric acid is added after end to be modulated；
(2) esterification is carried out after mixing terephthalic acid (TPA), ethylene glycol, catalyst and stabilizer；
(3) product of (1) is added in (2) and carries out the obtained spinning melt of polycondensation reaction；
B) spinning；
Spinning melt is through measuring, extruding, cooling down, oiling, stretching, high density fabric superfine denier polyester is made in thermal finalization and winding
FDY silks.
A kind of 2. preparation method of high density fabric superfine denier terylene FDY filament according to claim 1, it is characterised in that
Prepare comprising the following steps that for spinning melt：
(1) ester exchange reaction prepares the double hydroxyl ethyl ester -5- sodium sulfonates of M-phthalic acid；
DMIP -5- benzene sulfonic acid sodium salts and ethylene glycol input are prepared in kettle, add catalyst Z n (Ac)2Afterwards 175
Carry out terminating when ester exchange reaction reaches more than the 90% of theoretical value to the quantity of distillate of water at~185 DEG C, obtain M-phthalic acid
Double hydroxyl ethyl ester -5- sodium sulfonates, add ethylene glycol, ethylene glycol sodium and sulfuric acid and be modulated to obtain the M-phthalic acid containing 30~35wt%
The ethylene glycol solution of double hydroxyl ethyl ester -5- sodium sulfonates；
(2) esterification prepares ethylene glycol terephthalate；
Terephthalic acid (TPA) and ethylene glycol are made into after slurry add catalyst and stabilizer it is well mixed after carry out esterification and obtain
To ethylene glycol terephthalate, esterification compressive reaction in nitrogen atmosphere, moulding pressure is normal pressure~0.3MPa, esterification
The temperature of reaction is 250~260 DEG C, is esterification when the water quantity of distillate in esterification reaches more than the 90% of theoretical value
Terminal；
(3) polycondensation reaction prepares spinning melt；
The product of (1) is added in (2), the polycondensation reaction in low vacuum stage, the staged pressure are carried out first under condition of negative pressure
Steadily it is evacuated to by normal pressure below absolute pressure 500Pa, reaction temperature is 260~270 DEG C, and the reaction time is 30~50min, then
Continue to vacuumize the polycondensation reaction for carrying out high vacuum stage of Fig, reaction pressure is down to absolute pressure and be less than 100Pa, reaction temperature is
275~285 DEG C, the reaction time is 50~90min, and spinning melt is made.
A kind of 3. preparation method of high density fabric superfine denier terylene FDY filament according to claim 2, it is characterised in that
In step (1), when ester exchange reaction starts, the mol ratio of DMIP -5- benzene sulfonic acid sodium salts and ethylene glycol for 10~
12:1, catalyst Z n (Ac)2Addition be DMIP -5- benzene sulfonic acid sodium salt additions 0.2~0.5wt%；
During modulation, the addition of ethylene glycol sodium is 1.5~6wt% of DMIP -5- benzene sulfonic acid sodium salt additions, is added
The mass concentration of the sulfuric acid entered is 40~60%, and the addition of sulfuric acid is DMIP -5- benzene sulfonic acid sodium salt additions
1.5~6wt%.
A kind of 4. preparation method of high density fabric superfine denier terylene FDY filament according to claim 2, it is characterised in that
In step (2), when esterification starts, the mol ratio of terephthalic acid (TPA) and ethylene glycol is 1.10~1.30:1, catalyst three
Two antimony, antimony glycol or antimony acetate are aoxidized, the addition of catalyst is 0.01~0.05wt% of terephthalic acid (TPA) addition, surely
It is triphenyl phosphate, trimethyl phosphate or Trimethyl phosphite to determine agent, and the addition of stabilizer is terephthalic acid (TPA) addition
0.01~0.05wt%.
A kind of 5. preparation method of high density fabric superfine denier terylene FDY filament according to claim 2, it is characterised in that
In step (3), when polycondensation reaction starts, the double hydroxyl ethyl ester -5- sodium sulfonates of M-phthalic acid and ethylene glycol terephthalate rub
You are than being 1~3:100.
A kind of 6. preparation method of high density fabric superfine denier terylene FDY filament according to claim 1, it is characterised in that
The technological parameter of the spinning is：
Spinning temperature：285~295 DEG C；
Chilling temperature：20~25 DEG C；
Network pressure：0.20~0.30MPa；
One roller speed：1000~1500m/min；
One roll temperature：86~95 DEG C；
Two roller speeds：3820~4200m/min；
Two roll temperatures：117~130 DEG C；
Winding speed：3800~4100m/min.
A kind of 7. preparation method of high density fabric superfine denier terylene FDY filament according to claim 6, it is characterised in that
In spinning process, the pressure of filament spinning component rises Δ P≤0.8bar/ days, and the pressure of filter rises Δ P≤2.9bar/ days, spinning group
The service life of part is 36~38 days, and the service life of filter is 25~27 days.
A kind of 8. preparation method of high density fabric superfine denier terylene FDY filament according to claim 1, it is characterised in that
The line density of the high density fabric superfine denier terylene FDY filament is 7~8D, and filament number is 0.5~0.7dtex, fracture strength
>=3.80cN/dtex, dye-uptake are more than 95%.
A kind of 9. preparation method of high density fabric superfine denier terylene FDY filament according to claim 8, it is characterised in that
The elongation at break of the high density fabric superfine denier terylene FDY filament is 40.0 ± 5.0%, line density deviation ratio≤0.8%, is broken
Resistance to spalling CV value≤5.0%, extension at break CV value≤10.0%, yarn unevenness CV value≤1.5%.
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| CN110387596A (en) * | 2019-07-18 | 2019-10-29 | 新凤鸣集团股份有限公司 | A kind of preparation method of the CDP fabrics long filament |
| CN112853513A (en) * | 2020-12-31 | 2021-05-28 | 江苏恒科新材料有限公司 | Superfine denier terylene FDY fiber for high-density fabric and preparation method thereof |
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