CN109735979A - The preparation method of the different dye-uptake low elastic polyester filament of iso-fineness - Google Patents
The preparation method of the different dye-uptake low elastic polyester filament of iso-fineness Download PDFInfo
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Abstract
The present invention relates to a kind of preparation methods of the different dye-uptake low elastic polyester filament of iso-fineness, first by terephthalic acid (TPA), ethylene glycol and hexylene glycol with tert-butyl side group successively carries out esterification after mixing and modified poly ester is made in polycondensation reaction, then it will be processed after different modified poly ester POY of two kinds of filament numbers and silk by DTY technique, broken ditch roller and frequency conversion silk shifting device are set between zero roller of DTY equipment and first roller simultaneously, modified poly ester tow is passed through from broken ditch surface of roller, the different dye-uptake low elastic polyester filament of iso-fineness is made, broken ditch roller is the roller that circumferential surface is carved with multiple annular grooves, frequency conversion silk shifting device for drive polyester POY it is reciprocating along roller central axis in broken ditch roller circumferential surface, the moving period of frequency conversion silk shifting device is 5~99 reciprocal times/min.Rationally, the different dye-uptake low elastic polyester filament dyeability of fiber number obtained is good for preparation method operation of the invention.
Description
Technical field
The invention belongs to polyester fiber technical fields, are related to a kind of preparation side of different dye-uptake low elastic polyester filament of iso-fineness
Method.
Background technique
Terylene is the product name of China's polyester fiber, is an important species in synthetic fibers.With human lives
Horizontal continuous improvement, take, decorate and quantity and quality in terms of industry to fibrous material on requirement not yet
It is disconnected to improve.In order to adapt to people in the demand of clothing, decoration, industry and special dimension, needing to develop has new capability or additional
The fibre in differentiation of value.The flexibility of textile material shows as having comfortable sense of touch, smooth surface and lower anti-mostly
The advantages that curved performance, stiffness shows as touching elastic force mostly and recoverability is good and higher anti-bending strength, stiffness is
The feeling factor of the base style of fiber and the physiology of people and psychology.The fiber number of fiber affects the property of yarn and fabric
Can, effect that is compound, while making fiber generation be of different shades is carried out with fiber of the DTY equipment to different fiber numbers, is utilized
The effect can solve flexibility and stiffness a pair of contradictory body simultaneously, they are combined.
In recent years, people develop iso-fineness and similar natural silk are fine one after another by the research to natural fiber performance
The synthetic fibers of sense of touch and reflecting feel are tieed up, the application field and performance of synthetic fibers are improved and develop.It is controlled by process optimization,
The slub yarn with thickness structure can be produced, improves fabric air-permeability performance, and the corresponding crystallinity of thickness structure division is different,
Dye-uptake differs greatly, and beautiful ombre can be dyed when with same dyeing, and finished textile product is applied through surface
After the processing such as layer, press polish, it can be used for doing artificial leather top grade dress shell fabric, umbrella cloth, filtering material etc..
However, the single variety of the different dye-uptake low elastic polyester filament of prior art preparation iso-fineness, and the fiber number of monofilament and thick
Carefully all be restricted, manufactured fabric there are flexibility is insufficient and the shortcomings that can not dye beautiful ombre, this
Largely limit the development of the different dye-uptake low elastic polyester filament of iso-fineness.Simultaneously because not containing hydrophily on terylene molecule
Group belongs to hydrophobic fibre, and lacking in molecular structure can tie as cellulose or protein fibre with dyestuff
The active group of conjunction.Polyester fiber finished product is the supramolecular structure of partially crystallizable, and crystalline portion strand is parallel to each other, mostly
In anti conformation, and amorphous region is then in cisoid conformation more.By the molecular structure and crystallization situation of conventional PET it is found that its molecule
Arrangement is quite close, so that the dyeability of conventional PET fiber is poor.Therefore such as conventional polyester DTY tow dye of conventional PET fiber
Color generally uses disperse dyeing, and high-temperature pressure dyeing is usually taken.Using high-temperature pressure dyeing method the high requirements on the equipment,
Dyeing time is long, and energy consumption is high, and can not fundamentally change the problem of polyster fibre dyeing performance difference.
Therefore, how to overcome the problems, such as of the existing technology, study a kind of different fiber number while beauty can be dyed when dyeing
The preparation method of the different dye-uptake low elastic polyester filament of the good iso-fineness of the ombre and dyeing effect of sight has highly important
Meaning.
Summary of the invention
The purpose of the invention is to overcome above-mentioned problems of the prior art, a kind of different fiber number is provided while being contaminated
The preparation method of beautiful ombre and the good different dye-uptake low elastic polyester filament of iso-fineness of dyeing effect can be dyed when color.
In order to achieve the above object, the technical solution adopted by the present invention are as follows:
The preparation method of the different dye-uptake low elastic polyester filament of iso-fineness, by different modified poly ester POY of two kinds of filament numbers
And it is processed after silk by DTY technique, while broken ditch roller and frequency conversion shifting are set between zero roller of DTY equipment and first roller
Silk device, modified poly ester tow is passed through from broken ditch surface of roller, and the different dye-uptake low elastic polyester filament of iso-fineness is made；
Different modified poly ester POY of two kinds of filament numbers be by POY technique as made from modified poly ester melt；
The modified poly ester the preparation method comprises the following steps: terephthalic acid (TPA), ethylene glycol and hexylene glycol with tert-butyl side group are mixed
Esterification and polycondensation reaction are successively carried out after closing uniformly；
The structural formula of hexylene glycol with tert-butyl side group is as follows:
In formula, R is-H ,-CH2CH3Or-C (CH3)3；
The different dye-uptake low elastic polyester filament of iso-fineness of the invention, by introducing band tert-butyl side group in modified poly ester strand
Hexylene glycol segment, the presence of tert-butyl can cause the variation of main chain activity in the hexylene glycol with tert-butyl side group, to change
The interaction force between chain element is become, the distance between molecule chain element can also occur to change accordingly, lead to modified poly ester
Empty free volume increases, and the increase of empty free volume will be helpful to dye molecule and diffuse into fiber gap, improves
The dye-uptake of dyestuff reduces dyeing temperature and shortens dyeing time, improves dyeing effect；
Broken ditch roller is the roller that circumferential surface is carved with multiple annular grooves, multiple annular grooves around roller central axis, and
Along the central axis equidistantly distributed of roller, frequency conversion silk shifting device for drive polyester POY in broken ditch roller circumferential surface along roller center
Axis is reciprocating；
The diameter of broken ditch roller end face is 80mm；Spacing between adjacent two groove is 6mm, most along roller central axis direction
Two grooves in outside and be all 3.25mm away from the spacing between nearest roller end；The depth of groove is 2.6mm, width
For 4mm, quantity is 4；The moving period of frequency conversion silk shifting device is 5~99 reciprocal times/min, and the size influence in period is mainly
The ring number of unit length is related with the style of product；
The present invention prepares the different dye-uptake terylene of iso-fineness by adding brokenly ditch roller and frequency conversion silk shifting device in DTY equipment
Low stretch yarn breaks ditch surface of roller and is equipped with multiple annular grooves, and the perimeter due to breaking ditch roller in annular groove is less than annular groove
The perimeter of outer broken ditch roller, thus when the tension that is subject to of when fiber is outside annular groove is greater than in annular groove, fiber is in ring
Draw ratio when outside connected in star is larger (drafting multiple is controlled 1.6~1.8), draw ratio when fiber is in annular groove
Smaller (drafting multiple is controlled 1.2~1.3), frequency conversion silk shifting device is able to drive polyester POY in broken ditch roller circumferential surface along roller
Central axis is reciprocating, so that polyester POY draw ratios change in moment, obtains polyester DTY thickness of control
The effect of the change of segment so that polyester DTY occur it is different inhale the short variation of color chips segment lengths, on final iso-fineness obtained is different
Dye rate low elastic polyester filament slubbing and details are obvious, the feature of the different dye-uptake low elastic polyester filament of iso-fineness first is that the thickness of tow is deposited
Occurs density structure in different, fabric, the permeability of the fabric as made from iso-fineness different dye-uptake low elastic polyester filament
It is excellent that (vapor transfer rate of knitted fabric is 150-170g/m2H), simultaneously because slubbing and the corresponding crystallinity of detail section exist compared with
Big difference makes its dye-uptake there are biggish difference, and when textile dyeing as made from iso-fineness different dye-uptake low elastic polyester filament can
To dye beautiful ombre；
Second heater temperature of the DTY technique is 130~150 DEG C, is not heated with the second hot tank generally high-elastic
Silk, the generally low stretch yarn heated with the second hot tank, produced by the present invention is low stretch yarn.
As a preferred technical scheme:
The preparation method of the different dye-uptake low elastic polyester filament of iso-fineness as described above, the different modification of two kinds of filament numbers are poly-
The filament number that ester is POY is respectively 0.5~0.7dtex and 1.5~2.5dtex, in the different dye-uptake low elastic polyester filament of iso-fineness
Filament number biggish modified poly ester POY are 1~2:1~2 with the lesser modified poly ester POY fiber numbers ratio of filament number.
The preparation method of the different dye-uptake low elastic polyester filament of iso-fineness as described above, the different dye-uptake low elastic polyester filament of iso-fineness
Breaking strength >=2.8cN/dtex, elongation at break be 33.0 ± 3.0%, line density deviation ratio≤1.5%, breaking strength CV
Value≤5.0%, extension at break CV value≤10.0%, boiling water shrinkage are 5.9 ± 0.8%, and oil content is 2.50 ± 0.50wt%,
Crimp contraction is 14.0 ± 0.5%；The quality and quality phase of fiber of the present invention containing the hexylene glycol segment with tert-butyl side group
Than not reducing in the prior art, modified fiber still has good mechanical property and spinnability etc.；
Dye-uptake of the different dye-uptake low elastic polyester filament of iso-fineness under the conditions of 120 DEG C of temperature is 87.3~91.4%, resistance to
WASHING COLOR FASTNESS (washing staining and cotton staining) reaches 5 grades, and dry fastness reaches 5 grades, and fastness to wet rubbing is greater than 4 grades；At other
In the identical situation of test condition, dye-uptake of comparative sample under the conditions of 130 DEG C of temperature is 85.7%, and fastness to soaping is small
In 5 grades, washing staining is 4~5 grades, and cotton staining is 4 grades, and dry fastness is 4~5 grades, and fastness to wet rubbing is 3~4 grades, comparative sample
Difference with the different dye-uptake low elastic polyester filament of iso-fineness of the invention is only that its material is conventional polyester；
The different dye-uptake low elastic polyester filament of iso-fineness is in Bamboo-shaped, and slub length is 0.31~5.80/m, bamboo of the invention
The variation of nodular dacron thread thickness is obvious, has imitative slub yarn style, and fabric has special hollow out argyle design, and feel exquisiteness is relaxed
Suitable, drapability is good.
The preparation method of the different dye-uptake low elastic polyester filament of iso-fineness as described above, the different modification of two kinds of filament numbers are poly-
The cross section that ester is POY is all round.
The preparation method of the different dye-uptake low elastic polyester filament of iso-fineness as described above, the hexylene glycol with tert-butyl side group
Synthetic method are as follows: firstly, concentration is 300~350g/L's by the ratio for being 1.5~2:1 in the molar ratio of raw material A and sulfuric acid
The dilution heat of sulfuric acid mixing that raw material A solution and concentration are 200~300g/L is added in catholyte pond, then, will mix liquid cooling
But to 10~15 DEG C, then carry out electroreduction to raw material A concentration be lower than 10wt%, finally carry out crystallisation by cooling, separation and
Purification；
R is-H ,-CH2CH3With-C (CH3)3When, it is 2 that raw material A, which respectively corresponds, 2 methyl propanal, 2,2- dimethyl propione
With 2,24,4- tetramethyl propione.
The preparation method of the different dye-uptake low elastic polyester filament of iso-fineness as described above, the preparation step of the modified poly ester is such as
Under:
(1) esterification；
Terephthalic acid (TPA), ethylene glycol and hexylene glycol with tert-butyl side group are made into slurry, catalyst and stabilizer is added
After mixing, pressurization carries out esterification in nitrogen atmosphere, and moulding pressure is normal pressure~0.3MPa, the temperature of esterification
It is 250~260 DEG C, is esterification terminal when the water quantity of distillate in esterification reaches 90% or more of theoretical value；
(2) polycondensation reaction；
After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, the staged pressure 30~
Absolute pressure 500Pa being steadily evacuated to by normal pressure in 50min hereinafter, reaction temperature is 250~260 DEG C, the reaction time is 30~
50min then proceedes to vacuumize, and carries out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is made to be further reduced to absolute pressure
For 100Pa hereinafter, reaction temperature is 270~282 DEG C, the reaction time is 50~90min.
The preparation method of the different dye-uptake low elastic polyester filament of iso-fineness as described above, the terephthalic acid (TPA), ethylene glycol and
The molar ratio of hexylene glycol with tert-butyl side group is 1:1.2~2.0:0.03~0.05, the addition of the catalyst and stabilizer
Amount is respectively the 0.03~0.05wt% and 0.01~0.05wt% (mass percent) of terephthalic acid (TPA) additional amount；Of the invention
The additive amount of hexylene glycol with tert-butyl side group preferably range both can guarantee that modified fiber had good mechanical property
And crystallinity, while the dyeability of fiber can also be significantly improved, be conducive to the production and application of fiber, with tert-butyl side group
The additive amount of hexylene glycol can appropriate adjustment according to actual needs, but should not too, adding too much is to polyester macromolecule structure
Regularity destruction is too big, excessive to the crystallinity and Effect on Mechanical Properties of fiber, is unfavorable for the production and application of fiber, too low
Then dyeing effect is promoted unobvious.
The preparation method of the different dye-uptake low elastic polyester filament of iso-fineness as described above, the catalyst be antimony oxide,
Antimony glycol or antimony acetate, the stabilizer are triphenyl phosphate, trimethyl phosphate or Trimethyl phosphite.
The preparation method of the different dye-uptake low elastic polyester filament of iso-fineness as described above, the number-average molecular weight of modified poly ester are
25000~30000, molecular weight distributing index is 1.8~2.2.
The preparation method of the different dye-uptake low elastic polyester filament of iso-fineness as described above, the process of the POY technique are as follows: meter
Amount, spinneret squeeze out, are cooling, oiling and wind；
The parameter of the POY technique are as follows: 280~285 DEG C of spinning temperature, 17~20 DEG C of cooling temperature, winding speed 3200
~3600m/min；
The process of the DTY technique are as follows: seal wire, plying, network, heating stretching, false twisting, thermal finalization and winding；
The parameter of the DTY technique are as follows: 500~700m/min of spinning speed, overfeed rate of setting 3.5~5.5%, winding are super
Feed rate 3.0~5.5%, the first 180~200 DEG C of heater temperature, draw ratio 1.2~1.7.
Invention mechanism:
The different dye-uptake low elastic polyester filament of iso-fineness prepared by the present invention can dye the mechanism of beautiful ombre such as
Under:
The macromolecular chain and aggregated structure unit of POY fibers in drafting process of preorientation are unfolded, the degree of orientation
It improves, while can assign fiber higher energy when drawing-off, the stable state transformation for keeping molecular conformation constantly low to energy barrier, curling
Macromolecular is gradually stretched, and is easy to build into lattice, and active force is reinforced between macromolecular, and crystalline structure is more complete, finally makes crystallinity
Increase.During fiber hot gas spring, vying each other between orientation, relaxation disorientation and crystallization three occurs for strand, leads to
Cross reasonable combination drawing temperature and drafting multiple, the available product with different orientation and crystalline texture, the performance of product
Also difference therefore can be generated.
The present invention causes the draw ratio of fiber to generate by adding brokenly ditch roller and frequency conversion silk shifting device in DTY equipment
Difference breaks ditch surface of roller and is equipped with multiple annular grooves, and the perimeter due to breaking ditch roller in annular groove is less than outside annular groove
The perimeter of broken ditch roller, thus when the tension that is subject to of when fiber is outside annular groove is greater than in annular groove, fiber is in annular
Draw ratio when outside groove is larger (drafting multiple is controlled 1.6~1.8), draw ratio when fiber is in annular groove compared with
Small (drafting multiple control 1.2~1.3), frequency conversion silk shifting device are able to drive polyester POY in broken ditch roller circumferential surface along roller
Mandrel is reciprocating, so that polyester POY draw ratios change in moment, obtains polyester DTY thickness piece of control
The effect of the change of section, so that polyester DTY the short variation of different suction color chips segment lengths occur.
The draw ratio of fiber generates difference and the thickness of fiber is enabled to generate regular variation.With drafting multiple
Increase, the fiber number of fiber constantly becomes smaller, and the macromolecular axis degree of orientation increases, and fibre strength increases, and elongation decline, initial modulus mentions
Height, crystallinity increase, and it is since selective suction has occurred to visible light in dyestuff contained in fiber that the fiber after dyeing, which has color,
Receipts reflect or color are presented through light absorbing complementary color, and the depth and fiber of color have the reflection of light and scattering power
It closes, the fiber number of fiber is smaller, and fiber is thinner, and the specific surface area of fiber is bigger, and fiber surface is stronger to the reflection of light, into fiber
Internal light is fewer, and the light for absorbing back reflection through fiber or transmiting is weaker, and the color of fiber is more shallow；Therefore, thin part
Crystallinity, the degree of orientation are big, and the apparent colour depth after dyeing is low；Thick some crystallinity, the degree of orientation are small, the apparent face after dyeing
Color depth is high, so that fiber generates iso-fineness, different dye-uptake phenomenon, therefore by the different dye-uptake low elastic polyester filament system of iso-fineness
Beautiful ombre can be dyed when the textile dyeing obtained.
The present invention solves the problems, such as the dyeing effect difference of the different dye-uptake low elastic polyester filament of the iso-fineness of prior art preparation
Mechanism is as follows:
Macromolecular chain in polymer is not closely to pile up completely, always with the presence of gap between macromolecular chain, this
Portion void volume is free volume.It penetrates into small molecule inside macromolecule, to have foot in macromolecule or between macromolecule
Enough big gaps, so pore size (the i.e. ruler of free volume in the permeability and diffusivity of small molecule and macromolecular structure
It is very little) it is related, in a certain range, the size of free volume is bigger, and the permeability of small molecule is higher, and diffusivity is better.Free body
Product is divided into empty free volume and slit free volume again, and empty free body has bigger bulk compared with slit free volume,
Promotion for the permeability of small molecule, empty free volume are more obvious compared with slit free volume effect.
The size and type of free volume depend primarily on the structure of polymer, and the principal element for influencing polymer architecture is
Steric hindrance, side group size, side group structure etc..When position a certain on main polymer chain is replaced by side group, necessarily cause main chain
The variation of activity, to change the interaction force of chain and interchain, chain can also occur to change accordingly at a distance from interchain,
As a result lead to the variation of cohesive energy and free volume, polarity, size, length of the substituent group on polymer side chain etc. are to strand
Rigid, intermolecular interaction so that the fractional free volume of polymer architecture all have a certain impact, therefore, substituent group
The effect that difference generates is different, and the permeability and separation performance for often leading to polymer is also different.
For the dihydric alcohols straight chain molecule such as ethylene glycol, butanediol, the C atom on main chain is arranged in indention one on the other
Column, when the H atom on main chain on some methylene is by methyl (- CH3) when replacing, C atom and main chain C atom in side group do not exist
In same plane, then, four sp3 hybridized orbits on the C of center are Chong Die with the unoccupied orbital on four C atoms around respectively, shape
It at four identical σ keys, is arranged in positive tetrahedron, four carbon atom is located at four vertex of positive tetrahedron, works as first
When three hydrogen of base is further replaced by methyl, it is at this moment equivalent to tert-butyl substitution, forms a bigger tetrahedral structure,
With respect to the strand that indention arranges, empty free volume significantly increases much the strand of this positive tetrahedron arrangement,
The permeability and diffusivity of small molecule can be significantly improved；And when the H atom on main chain on some methylene is replaced by long-chain branch
When base replaces, what is mainly increased is slit free volume, and increase amplitude is smaller, permeability and diffusible promotion to small molecule
Effect is limited, simultaneously because the rigidity for chain substituent of drawing money on credit is smaller, entanglement is easy to happen between strand, is unfavorable for free volume
Increase.
The present invention has been obviously improved polyester industrial yarn by introducing the hexylene glycol with tert-butyl side group in polyester molecule chain
Dyeability, the structural formula of the hexylene glycol with tert-butyl side group is as follows:
In formula, R is-H (hexylene glycol with tert-butyl side group is 2,2,5,5- tetramethyl -3,4- hexylene glycols),-CH2CH3(band
The hexylene glycol of tert-butyl side group is 2,2,5,5- tetramethyl -3,4- diethyl -3,4- hexylene glycol) or-C (CH3)3(band tert-butyl side
The hexylene glycol of base is 2,2,4,4- tetramethyl -3,4- di-t-butyl -3,4- hexylene glycol)；
The presence of tert-butyl can cause the variation of main chain activity in hexylene glycol with tert-butyl side group, to change chain
Interaction force between unit, the distance between molecule chain element can also occur to change accordingly, cause the cavity of modified poly ester from
Increased by volume.Compared with short-chain branch substituent group (such as methyl, ethyl group), tert-butyl occupies biggish spatial position,
Bigger free volume will be obtained in the mode of strand arrangement；Compared with chain substituent of drawing money on credit, one side tert-butyl increases
Be cavity, and draw money on credit chain substituent increase be slit free volume, another aspect tert-butyl rigidity taken greater than long-chain branch
Dai Ji, reduces the entanglement between strand, thus tert-butyl has compared with chain substituent is drawn money on credit in the mode that strand arranges
More free volumes.Since crystallizing polyester degree is high and surface is smooth, surface active groups are seldom, and dyeing effect is not ideal enough,
So that the empty free volume of modified poly ester increases, the increase of empty free volume will for the introducing of hexylene glycol with tert-butyl side group
Helping, which diffuses into portion's dye molecule in dyeing course, can reduce dyeing temperature in fiber gap, shorten dyeing when
Between, energy consumption is reduced, while also improving the dye-uptake of fiber.
The utility model has the advantages that
(1) preparation method of the different dye-uptake low elastic polyester filament of a kind of iso-fineness of the invention, by polyester molecule chain
Introducing, there is the hexylene glycol with tert-butyl side group of specific structure to keep dyestuff small to increase the empty free volume of polyester
Molecule is easier to penetrate into inside polyester, so as to improve the dyeability of low elastic polyester filament, improves the upper of low elastic polyester filament
Dye rate and color fastness, and then the dyeing quality of fabric can be improved；
(2) preparation method of the different dye-uptake low elastic polyester filament of a kind of iso-fineness of the invention, it is easy to operate, it is only necessary to polyester
It is modified while adding brokenly ditch roller and frequency conversion silk shifting device in DTY equipment, and control tow with specific frequency along certain party
Pass through to from broken ditch surface of roller；
(3) preparation method of the different dye-uptake low elastic polyester filament of a kind of iso-fineness of the invention, can be made slubbing and details
Clearly, permeability is excellent, dyeing effect is excellent and can dye beautiful ombre when being dyed with same dye bath
Low elastic polyester filament.
Detailed description of the invention
Fig. 1 is the reaction unit schematic diagram of the hexylene glycol of anamorphic zone tert-butyl side group of the present invention；
Fig. 2 is the structural schematic diagram of DTY equipment of the invention；
Fig. 3 is the front view of broken ditch roller of the invention；
Fig. 4 is the left view of broken ditch roller of the invention；
Fig. 5 is DTY device structure schematic diagram in the prior art.
Specific 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
It is bright rather than limit the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, art technology
Personnel can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Fixed range.
Embodiment 1
The preparation method of the different dye-uptake low elastic polyester filament of iso-fineness, steps are as follows:
(1) modified poly ester is prepared；
(1.1) 2,2,5,5- tetramethyl -3,4- hexylene glycols, method are synthesized are as follows: firstly, 2 are pressed, 2 methyl propanal and sulfuric acid
The ratio that molar ratio is 1.5:1 by concentration be 320g/L 2,2- butylic aldehyde solution and concentration be 200g/L dilution heat of sulfuric acid
Mixing is added in catholyte pond, then, mixed liquor is cooled to 12 DEG C, then progress electroreduction to 2,2 methyl propanal
Concentration is 9.5wt%, finally carries out crystallisation by cooling, separation and purification, reaction unit schematic diagram employed in synthesis process is such as
Shown in Fig. 1, reactive chemistry equation is as follows:
Shown in the structural formula such as formula (I) of obtained 2,2,5,5- tetramethyl -3,4- hexylene glycols, in formula, R is-H；
(1.2) esterification；
Terephthalic acid (TPA), ethylene glycol and 2,2,5,5- tetramethyl -3,4- hexylene glycol that molar ratio is 1:1.2:0.03 are matched
At slurry, antimony oxide and triphenyl phosphate is added after mixing, pressurization carries out esterification, pressurization in nitrogen atmosphere
Pressure is 0.1MPa, and the temperature of esterification is 250 DEG C, is when the water quantity of distillate in esterification reaches the 93% of theoretical value
The additional amount of esterification terminal, antimony oxide and triphenyl phosphate be respectively terephthalic acid (TPA) additional amount 0.03wt% and
0.02wt%；
(1.3) polycondensation reaction；
After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, the staged pressure is in 30min
The interior absolute pressure that is steadily evacuated to by normal pressure is 480Pa, and reaction temperature is 250 DEG C, reaction time 31min, then proceedes to take out true
Sky carries out the polycondensation reaction of high vacuum stage of Fig, and reaction pressure is made to be further reduced to absolute pressure 100Pa, reaction temperature 270
DEG C, reaction time 50min, the number-average molecular weight of modified poly ester obtained is 30000, molecular weight distributing index 2.0；
(2) different modified poly ester POY of two kinds of filament numbers are prepared；
It is round that modified poly ester melt, which is squeezed out, through metering, spinneret respectively, is cooling, is oiled and obtains cross section all after winding
Shape and filament number are respectively modified poly ester POY of 0.5dtex and 1.5dtex, the parameter of POY technique are as follows: spinning temperature 285
DEG C, 17 DEG C of cooling temperature, winding speed 3500m/min；
(3) the different dye-uptake low elastic polyester filament of iso-fineness is prepared；
It will be processed after different modified poly ester POY of two kinds of filament numbers and silk by DTY technique, be used for polyester DTY
The DTY equipment of technique, as shown in Fig. 2, including original silk rack, yarn cutter, zero roller, frequency conversion silk shifting device, broken ditch roller, first sieve
Drawing, sliding rail, the first hot tank, coldplate, scroll tube, tensiometer, the second roller, network nozzle, the second hot tank, third roller, oil
Wheel and coiler, wherein the front view and left view difference of broken ditch roller are as shown in Figures 3 and 4, and broken ditch roller is carved with more for circumferential surface
The roller of a annular groove, multiple annular grooves around roller central axis, and along the central axis equidistantly distributed of roller, frequency conversion
Silk shifting device is for driving modified poly ester POY, broken ditch roller end faces reciprocating along roller central axis in broken ditch roller circumferential surface
Diameter be 80mm；Spacing between adjacent two groove is 6mm, along outermost two groove of roller central axis direction and apart from it
Spacing between nearest roller end is all 3.25mm；The depth of groove is 2.6mm, and width 4mm, quantity is 4；
Modified poly ester POY on original silk rack are successively passed through yarn cutter, zero roller, frequency conversion again after wire leading pipe exports
Silk shifting device, broken ditch surface of roller, first roller, the first hot tank, coldplate, scroll tube, tensiometer, the second roller, network nozzle,
Second hot tank, third roller, oil tanker and coiler are to complete seal wire, plying, network, heating stretching, false twisting, thermal finalization and volume
DTY technique is completed around process and obtains the different dye-uptake low elastic polyester filament of iso-fineness, wherein the moving period of frequency conversion silk shifting device is 99
Reciprocal time/min, the parameter of DTY technique are as follows: spinning speed 400m/min, overfeed rate of setting 3.5%, winding overfeed rate
4.0%, the first 190 DEG C of heater temperature, the second 130 DEG C of heater temperature, draw ratio 1.7.
Filament number biggish modified poly ester POY and monofilament in the different dye-uptake low elastic polyester filament of final iso-fineness obtained
The lesser modified poly ester POY fiber numbers ratio of fiber number is 1:1；The breaking strength of the different dye-uptake low elastic polyester filament of iso-fineness is
2.92cN/dtex, elongation at break 30.0%, line density deviation ratio are 1.44%, and breaking strength CV value is 5.0%, fracture
Extending CV value is 9.8%, boiling water shrinkage 5.9%, oil content 2.2wt%, crimp contraction 19.0%；
Dye-uptake of the different dye-uptake low elastic polyester filament of iso-fineness under the conditions of 120 DEG C of temperature is 87.3%, resistance to color of soaping
Fastness reaches 5 grades, and dry fastness reaches 5 grades, and fastness to wet rubbing is 5 grades；
The different dye-uptake low elastic polyester filament of iso-fineness is in Bamboo-shaped, and slub length is 5.80/m.
Comparative example 1
A kind of preparation method of the different dye-uptake low elastic polyester filament of iso-fineness, step and embodiment 1 are almost the same, difference
It is not to be modified polyester, the biggish modified poly ester of filament number in the different dye-uptake low elastic polyester filament of iso-fineness obtained
POY are 1:1 with the lesser modified poly ester POY fiber numbers ratio of filament number；The different dye-uptake low elastic polyester filament of iso-fineness breaks
Resistance to spalling is 2.92cN/dtex, and elongation at break 30.0%, line density deviation ratio is 1.44%, and breaking strength CV value is
5.0%, extension at break CV value is 9.8%, boiling water shrinkage 5.9%, oil content 2.2wt%, and crimp contraction is
19.0%, slub length is 5.80/m；In situation identical with other test conditions of embodiment 1, comparative sample is at 130 DEG C
Dye-uptake under the conditions of temperature is 85.7%, and fastness to soaping is 4~5 grades, and dry fastness is 4~5 grades, fastness to wet rubbing
It is 3~4 grades, the difference of comparative sample and the different dye-uptake low elastic polyester filament of iso-fineness of the invention is only that its material is common poly-
Ester.The two compares it is found that the present invention substantially increases the dyeability and mechanical property of polyester fiber by being modified to polyester
It can be unaffected.
Comparative example 2
A kind of preparation method of the different dye-uptake low elastic polyester filament of iso-fineness, preparation step and embodiment 1 are almost the same, different
Place is, substitutes 2,2,5,5- tetramethyl -3,4- hexylene glycols using 1,2- dodecanediol in step (1), obtained different
Biggish modified poly ester POY of filament number and the lesser modified poly ester of filament number in the different dye-uptake low elastic polyester filament of fiber number
POY fiber number ratios are 1:1；The breaking strength of the different dye-uptake low elastic polyester filament of iso-fineness is 2.85cN/dtex, elongation at break
It is 32.0%, line density deviation ratio is 1.48%, and breaking strength CV value is 5.1%, and extension at break CV value is 9.8%, and boiling water is received
Shrinkage is 6.5%, oil content 2.2wt%, crimp contraction 19.0%, and slub length is 5.80/m.With embodiment 1
In the identical situation of other test conditions, the different dye-uptake low elastic polyester filament of iso-fineness obtained is under the conditions of 130 DEG C of temperature
Dye-uptake is 85.2%, and fastness to soaping is 4~5 grades, and dry fastness is 4 grades, and fastness to wet rubbing is 4 grades, is below this
Invention.
It compares with embodiment 1 it can be found that the hexylene glycol (2,2,5,5- tetramethyl -3,4- hexylene glycol) with tert-butyl side group
The dyeability for promoting fiber is more advantageous to relative to 1, the 2- dodecanediol containing chain substituent of drawing money on credit, this is primarily due to
On the one hand the free volume that the hexylene glycol with tert-butyl side group increases is more empty free volume, and chain substituent increasing of drawing money on credit
Big free volume is more slit free volume, and the rigidity of the hexylene glycol on the other hand with tert-butyl side group is greater than long-chain branch
Substituent group reduces the entanglement between strand, thus the hexylene glycol with tert-butyl side group relatively draws money on credit chain substituent in strand
There are more free volumes, the increase of empty free volume will be helpful to dyestuff and diffuse into fiber sky in the mode of arrangement
In gap, the dye-uptake of fiber is improved, reduce dyeing temperature and shortens dyeing time, chain substituent is more advantageous to relative to drawing money on credit
Promote the dyeability of fiber.
Comparative example 3
A kind of preparation method of dacron thread, preparation step and embodiment 1 are almost the same, the difference is that, preparation is washed
The DTY equipment used when synthetic fibre silk is as shown in figure 5, without frequency conversion silk shifting device and broken ditch roller in DTY equipment.Final terylene obtained
Silk is conventional polyester DTY, is not in Bamboo-shaped, embodiment 1 and comparative example 3 is compared as can be seen that just because of this Shen
The effect of frequency conversion silk shifting device and broken ditch roller please, it is low that the terylene in Bamboo-shaped beautiful and that quality is good can be made in the present invention
Elater.
Embodiment 2
The preparation method of the different dye-uptake low elastic polyester filament of iso-fineness, steps are as follows:
(1) modified poly ester is prepared；
(1.1) 2,2,5,5- tetramethyl -3,4- diethyl -3,4- hexylene glycols, method are synthesized are as follows: firstly, pressing 2,2- diformazan
The ratio that the molar ratio of base propione and sulfuric acid is 1.6:1 by concentration be 350g/L 2,2- dimethyl propione solution and concentration
It is added in catholyte pond for the dilution heat of sulfuric acid mixing of 210g/L, then, mixed liquor is cooled to 11 DEG C, is then electrolysed
The concentration for being restored to 2,2- dimethyl propione is 9.0wt%, finally progress crystallisation by cooling, separation and purification, in synthesis process
Used reaction unit and reactive chemistry equation and embodiment 1 are consistent, obtained 2,2,5,5- tetramethyl -3,4- diethyls
Shown in the structural formula of base -3,4- hexylene glycol such as formula (I), in formula, R is-CH2CH3；
(1.2) esterification；
Terephthalic acid (TPA), ethylene glycol and the 2,2,5,5- tetramethyl -3,4- diethyl-for being 1:1.5:0.034 by molar ratio
3,4- hexylene glycols are made into slurry, and antimony glycol and trimethyl phosphate is added after mixing, and pressurization carries out ester in nitrogen atmosphere
Change reaction, moulding pressure is normal pressure, and the temperature of esterification is 251 DEG C, when the water quantity of distillate in esterification reaches theoretical value
92% when be esterification terminal, the additional amount of antimony glycol and trimethyl phosphate is respectively terephthalic acid (TPA) additional amount
0.04wt% and 0.01wt%；
(1.3) polycondensation reaction；
After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, the staged pressure is in 30min
The interior absolute pressure that is steadily evacuated to by normal pressure is 500Pa, and reaction temperature is 252 DEG C, reaction time 30min, then proceedes to take out true
Sky carries out the polycondensation reaction of high vacuum stage of Fig, and reaction pressure is made to be further reduced to absolute pressure 100Pa, reaction temperature 271
DEG C, reaction time 55min, the number-average molecular weight of modified poly ester obtained is 29000, molecular weight distributing index 2.1；
(2) different modified poly ester POY of two kinds of filament numbers are prepared；
It is round that modified poly ester melt, which is squeezed out, through metering, spinneret respectively, is cooling, is oiled and obtains cross section all after winding
Shape and filament number are respectively modified poly ester POY of 0.5dtex and 2.5dtex, the parameter of POY technique are as follows: spinning temperature 280
DEG C, 17 DEG C of cooling temperature, winding speed 3200m/min；
(3) the different dye-uptake low elastic polyester filament of iso-fineness is prepared；
It will be processed after different modified poly ester POY of two kinds of filament numbers and silk by DTY technique, modified poly ester POY
Different fibre is made after DTY process flow substantially the same manner as Example 1 using DTY equipment identical with 1 structure of embodiment in silk
Spend different dye-uptake low elastic polyester filament, DTY technique difference from example 1 is that, the moving period of frequency conversion silk shifting device is 5 past
Again/min, the parameter of DTY technique are counted are as follows: spinning speed 500m/min, overfeed rate of setting 5.5%, winding overfeed rate 3.0%,
First 180 DEG C of heater temperature, the second 140 DEG C of heater temperature, draw ratio 1.65.
Filament number biggish modified poly ester POY and monofilament in the different dye-uptake low elastic polyester filament of final iso-fineness obtained
The lesser modified poly ester POY fiber numbers ratio of fiber number is 1.2:1；The breaking strength of the different dye-uptake low elastic polyester filament of iso-fineness is
2.8cN/dtex, elongation at break 33.0%, line density deviation ratio are 1.46%, and breaking strength CV value is 4.9%, and fracture is stretched
Long CV value is 9.9%, boiling water shrinkage 5.1%, oil content 3.0wt%, crimp contraction 9.0%；
Dye-uptake of the different dye-uptake low elastic polyester filament of iso-fineness under the conditions of 120 DEG C of temperature is 89.23%, resistance to color of soaping
Fastness reaches 5 grades, and dry fastness reaches 5 grades, and fastness to wet rubbing is 5 grades；
The different dye-uptake low elastic polyester filament of iso-fineness is in Bamboo-shaped, and slub length is 0.31/m.
Embodiment 3
The preparation method of the different dye-uptake low elastic polyester filament of iso-fineness, steps are as follows:
(1) modified poly ester is prepared；
(1.1) 2,2,4,4- tetramethyl -3,4- di-t-butyl -3,4- hexylene glycols, method are synthesized are as follows: firstly, pressing 2,24,4-
The ratio that the molar ratio of tetramethyl propione and sulfuric acid is 1.7:1 by concentration be 340g/L 2,24,4- tetramethyl propione it is molten
The dilution heat of sulfuric acid mixing that liquid and concentration are 230g/L is added in catholyte pond, then, mixed liquor is cooled to 10 DEG C, then
Carrying out electroreduction to the concentration of 2,24,4- tetramethyl propiones is 9.6wt%, finally carries out crystallisation by cooling, separation and purification,
Reaction unit employed in synthesis process and reactive chemistry equation and embodiment 1 are consistent, and obtained 2,2,4,4- tetramethyls-
Shown in the structural formula such as formula (I) of 3,4- di-t-butyl -3,4- hexylene glycols, in formula, R is-C (CH3)3；
(1.2) esterification；
Terephthalic acid (TPA), ethylene glycol and the tertiary fourth of 2,2,4,4- tetramethyl -3,4- two for being 1:1.8:0.037 by molar ratio
Base -3,4- hexylene glycol is made into slurry, and antimony acetate and Trimethyl phosphite is added after mixing, pressurizes and carries out in nitrogen atmosphere
Esterification, moulding pressure are normal pressure, and the temperature of esterification is 252 DEG C, when the water quantity of distillate in esterification reaches theoretical
Value 90% when be esterification terminal, the additional amount of antimony acetate and Trimethyl phosphite is respectively terephthalic acid (TPA) additional amount
0.04wt% and 0.03wt%；
(1.3) polycondensation reaction；
After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, the staged pressure is in 35min
The interior absolute pressure that is steadily evacuated to by normal pressure is 450Pa, and reaction temperature is 253 DEG C, reaction time 35min, then proceedes to take out true
Sky carries out the polycondensation reaction of high vacuum stage of Fig, and reaction pressure is made to be further reduced to absolute pressure 90Pa, reaction temperature 274
DEG C, reaction time 60min, the number-average molecular weight of modified poly ester obtained is 37500, molecular weight distributing index 2.2；
(2) different modified poly ester POY of two kinds of filament numbers are prepared；
It is round that modified poly ester melt, which is squeezed out, through metering, spinneret respectively, is cooling, is oiled and obtains cross section all after winding
Shape and filament number are respectively modified poly ester POY of 0.6dtex and 1.5dtex, the parameter of POY technique are as follows: spinning temperature 285
DEG C, 20 DEG C of cooling temperature, winding speed 3600m/min；
(3) the different dye-uptake low elastic polyester filament of iso-fineness is prepared；
It will be processed after different modified poly ester POY of two kinds of filament numbers and silk by DTY technique, modified poly ester POY
Different fibre is made after DTY process flow substantially the same manner as Example 1 using DTY equipment identical with 1 structure of embodiment in silk
Spend different dye-uptake low elastic polyester filament, DTY technique difference from example 1 is that, the moving period of frequency conversion silk shifting device is 15
Reciprocal time/min, the parameter of DTY technique are as follows: spinning speed 500m/min, overfeed rate of setting 3.5%, winding overfeed rate
3.0%, the first 180 DEG C of heater temperature, the second 150 DEG C of heater temperature, draw ratio 1.7.
Filament number biggish modified poly ester POY and monofilament in the different dye-uptake low elastic polyester filament of final iso-fineness obtained
The lesser modified poly ester POY fiber numbers ratio of fiber number is 1.5:1.3；The breaking strength of the different dye-uptake low elastic polyester filament of iso-fineness is
2.95cN/dtex, elongation at break 33.0%, line density deviation ratio are 1.5%, and breaking strength CV value is 4.7%, and fracture is stretched
Long CV value is 10.0%, boiling water shrinkage 6.7%, oil content 2.50wt%, crimp contraction 14.5%；
Dye-uptake of the different dye-uptake low elastic polyester filament of iso-fineness under the conditions of 120 DEG C of temperature is 88.2%, resistance to color of soaping
Fastness reaches 5 grades, and dry fastness reaches 5 grades, and fastness to wet rubbing is 6 grades；
The different dye-uptake low elastic polyester filament of iso-fineness is in Bamboo-shaped, and slub length is 0.93/m.
Embodiment 4
The preparation method of the different dye-uptake low elastic polyester filament of iso-fineness, steps are as follows:
(1) modified poly ester is prepared；
(1.1) 2,2,5,5- tetramethyl -3,4- hexylene glycols, method are synthesized are as follows: firstly, 2 are pressed, 2 methyl propanal and sulfuric acid
The ratio that molar ratio is 1.8:1 by concentration be 300g/L 2,2- butylic aldehyde solution and concentration be 250g/L dilution heat of sulfuric acid
Mixing is added in catholyte pond, then, mixed liquor is cooled to 15 DEG C, then progress electroreduction to 2,2 methyl propanal
Concentration is 9.3wt%, finally carries out crystallisation by cooling, separation and purification, reaction unit and reaction employed in synthesis process
Chemical equation and embodiment 1 are consistent, shown in the structural formula such as formula (I) of obtained 2,2,5,5- tetramethyl -3,4- hexylene glycols, formula
In, R is-H；
(1.2) esterification；
Terephthalic acid (TPA), ethylene glycol and 2,2,5,5- tetramethyl -3,4- hexylene glycol that molar ratio is 1:1.9:0.04 are matched
At slurry, antimony acetate and triphenyl phosphate is added after mixing, pressurization carries out esterification, moulding pressure in nitrogen atmosphere
For 0.3MPa, the temperature of esterification is 254 DEG C, is esterification when the water quantity of distillate in esterification reaches the 96% of theoretical value
The additional amount of reaction end, antimony acetate and triphenyl phosphate be respectively terephthalic acid (TPA) additional amount 0.03wt% and
0.05wt%；
(1.3) polycondensation reaction；
After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, the staged pressure is in 40min
The interior absolute pressure that is steadily evacuated to by normal pressure is 410Pa, and reaction temperature is 255 DEG C, reaction time 32min, then proceedes to take out true
Sky carries out the polycondensation reaction of high vacuum stage of Fig, and reaction pressure is made to be further reduced to absolute pressure 95Pa, reaction temperature 275
DEG C, reaction time 70min, the number-average molecular weight of modified poly ester obtained is 25000, molecular weight distributing index 2.2；
(2) different modified poly ester POY of two kinds of filament numbers are prepared；
It is round that modified poly ester melt, which is squeezed out, through metering, spinneret respectively, is cooling, is oiled and obtains cross section all after winding
Shape and filament number are respectively modified poly ester POY of 0.6dtex and 2.0dtex, the parameter of POY technique are as follows: spinning temperature 282
DEG C, 20 DEG C of cooling temperature, winding speed 3500m/min；
(3) the different dye-uptake low elastic polyester filament of iso-fineness is prepared；
It will be processed after different modified poly ester POY of two kinds of filament numbers and silk by DTY technique, modified poly ester POY
Different fibre is made after DTY process flow substantially the same manner as Example 1 using DTY equipment identical with 1 structure of embodiment in silk
Spend different dye-uptake low elastic polyester filament, DTY technique difference from example 1 is that, the moving period of frequency conversion silk shifting device is 25
Reciprocal time/min, the parameter of DTY technique are as follows: spinning speed 500m/min, overfeed rate of setting 4.5%, winding overfeed rate
5.5%, the first 200 DEG C of heater temperature, the second 150 DEG C of heater temperature, draw ratio 1.4.
Filament number biggish modified poly ester POY and monofilament in the different dye-uptake low elastic polyester filament of final iso-fineness obtained
The lesser modified poly ester POY fiber numbers ratio of fiber number is 2:1；The breaking strength of the different dye-uptake low elastic polyester filament of iso-fineness is
2.96cN/dtex, elongation at break 36.0%, line density deviation ratio are 1.38%, and breaking strength CV value is 4.85%, fracture
Extending CV value is 9.7%, boiling water shrinkage 5.9%, oil content 2.0wt%, crimp contraction 13.5%；
Dye-uptake of the different dye-uptake low elastic polyester filament of iso-fineness under the conditions of 120 DEG C of temperature is 91.4%, resistance to color of soaping
Fastness reaches 5 grades, and dry fastness reaches 5 grades, and fastness to wet rubbing is 6 grades；
The different dye-uptake low elastic polyester filament of iso-fineness is in Bamboo-shaped, and slub length is 1.53/m.
Embodiment 5
The preparation method of the different dye-uptake low elastic polyester filament of iso-fineness, steps are as follows:
(1) modified poly ester is prepared；
(1.1) 2,2,5,5- tetramethyl -3,4- diethyl -3,4- hexylene glycols, method are synthesized are as follows: firstly, pressing 2,2- diformazan
The ratio that the molar ratio of base propione and sulfuric acid is 1.9:1 by concentration be 310g/L 2,2- dimethyl propione solution and concentration
It is added in catholyte pond for the dilution heat of sulfuric acid mixing of 300g/L, then, mixed liquor is cooled to 15 DEG C, is then electrolysed
The concentration for being restored to 2,2- dimethyl propione is 8.8wt%, finally progress crystallisation by cooling, separation and purification, in synthesis process
Used reaction unit and reactive chemistry equation and embodiment 1 are consistent, obtained 2,2,5,5- tetramethyl -3,4- diethyls
Shown in the structural formula of base -3,4- hexylene glycol such as formula (I), in formula, R is-CH2CH3；
(1.2) esterification；
Terephthalic acid (TPA), ethylene glycol and the 2,2,5,5- tetramethyl -3,4- diethyl-for being 1:2.0:0.042 by molar ratio
3,4- hexylene glycols are made into slurry, and antimony glycol and Trimethyl phosphite is added after mixing, pressurize and carry out in nitrogen atmosphere
Esterification, moulding pressure 0.2MPa, the temperature of esterification is 256 DEG C, when the water quantity of distillate in esterification reaches reason
By value 99% when be esterification terminal, the additional amount of antimony glycol and Trimethyl phosphite is respectively that terephthalic acid (TPA) is added
The 0.03wt% and 0.04wt% of amount；
(1.3) polycondensation reaction；
After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, the staged pressure is in 45min
The interior absolute pressure that is steadily evacuated to by normal pressure is 490Pa, and reaction temperature is 257 DEG C, reaction time 40min, then proceedes to take out true
Sky carries out the polycondensation reaction of high vacuum stage of Fig, and reaction pressure is made to be further reduced to absolute pressure 90Pa, reaction temperature 277
DEG C, reaction time 75min, the number-average molecular weight of modified poly ester obtained is 27800, molecular weight distributing index 1.8；
(2) different modified poly ester POY of two kinds of filament numbers are prepared；
It is round that modified poly ester melt, which is squeezed out, through metering, spinneret respectively, is cooling, is oiled and obtains cross section all after winding
Shape and filament number are respectively modified poly ester POY of 0.7dtex and 2.2dtex, the parameter of POY technique are as follows: spinning temperature 280
DEG C, 17 DEG C of cooling temperature, winding speed 3200m/min；
(3) the different dye-uptake low elastic polyester filament of iso-fineness is prepared；
It will be processed after different modified poly ester POY of two kinds of filament numbers and silk by DTY technique, modified poly ester POY
Different fibre is made after DTY process flow substantially the same manner as Example 1 using DTY equipment identical with 1 structure of embodiment in silk
Spend different dye-uptake low elastic polyester filament, DTY technique difference from example 1 is that, the moving period of frequency conversion silk shifting device is 50
Reciprocal time/min, the parameter of DTY technique are as follows: spinning speed 700m/min, overfeed rate of setting 4.0%, winding overfeed rate
4.5%, the first 195 DEG C of heater temperature, the second 130 DEG C of heater temperature, draw ratio 1.2.
Filament number biggish modified poly ester POY and monofilament in the different dye-uptake low elastic polyester filament of final iso-fineness obtained
The lesser modified poly ester POY fiber numbers ratio of fiber number is 2:1.4；The breaking strength of the different dye-uptake low elastic polyester filament of iso-fineness is
2.9cN/dtex, elongation at break 33.0%, line density deviation ratio are 1.5%, and breaking strength CV value is 4.7%, and fracture is stretched
Long CV value is 10.0%, boiling water shrinkage 5.5%, oil content 2.5wt%, crimp contraction 14.0%；
Dye-uptake of the different dye-uptake low elastic polyester filament of iso-fineness under the conditions of 120 DEG C of temperature is 89.3%, resistance to color of soaping
Fastness reaches 5 grades, and dry fastness reaches 5 grades, and fastness to wet rubbing is 5 grades；
The different dye-uptake low elastic polyester filament of iso-fineness is in Bamboo-shaped, and slub length is 3.13/m.
Embodiment 6
The preparation method of the different dye-uptake low elastic polyester filament of iso-fineness, steps are as follows:
(1) modified poly ester is prepared；
(1) modified poly ester is prepared；
(1.1) 2,2,4,4- tetramethyl -3,4- di-t-butyl -3,4- hexylene glycols, method are synthesized are as follows: firstly, pressing 2,24,4-
The 2,24,4- tetramethyl propione solution that concentration is 350g/L by the ratio that the molar ratio of tetramethyl propione and sulfuric acid is 2:1
With concentration be 220g/L dilution heat of sulfuric acid mixing be added catholyte pond in, then, mixed liquor is cooled to 13 DEG C, then into
The concentration of row electroreduction to 2,24,4- tetramethyl propiones is 9.6wt%, finally carries out crystallisation by cooling, separation and purification, is closed
It is consistent at used reaction unit and reactive chemistry equation and embodiment 1 in the process, obtained 2,2,4,4- tetramethyl -3,
Shown in the structural formula such as formula (I) of 4- di-t-butyl -3,4- hexylene glycol, in formula, R is-C (CH3)3；
(1.2) esterification；
Terephthalic acid (TPA), ethylene glycol and the tertiary fourth of 2,2,4,4- tetramethyl -3,4- two for being 1:1.2:0.045 by molar ratio
Base -3,4- hexylene glycol is made into slurry, and antimony oxide and trimethyl phosphate is added after mixing, pressurize in nitrogen atmosphere into
Row esterification, moulding pressure 0.2MPa, the temperature of esterification is 258 DEG C, when the water quantity of distillate in esterification reaches
Theoretical value 95% when be esterification terminal, the additional amount of antimony oxide and trimethyl phosphate is respectively that terephthalic acid (TPA) adds
Enter the 0.04wt% and 0.01wt% of amount；
(1.3) polycondensation reaction；
After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, the staged pressure is in 35min
The interior absolute pressure that is steadily evacuated to by normal pressure is 430Pa, and reaction temperature is 258 DEG C, reaction time 40min, then proceedes to take out true
Sky carries out the polycondensation reaction of high vacuum stage of Fig, and reaction pressure is made to be further reduced to absolute pressure 94Pa, reaction temperature 280
DEG C, reaction time 80min, the number-average molecular weight of modified poly ester obtained is 29100, molecular weight distributing index 1.9；
(2) different modified poly ester POY of two kinds of filament numbers are prepared；
It is round that modified poly ester melt, which is squeezed out, through metering, spinneret respectively, is cooling, is oiled and obtains cross section all after winding
Shape and filament number are respectively modified poly ester POY of 0.7dtex and 2.5dtex, the parameter of POY technique are as follows: spinning temperature 283
DEG C, 20 DEG C of cooling temperature, winding speed 3600m/min；
(3) the different dye-uptake low elastic polyester filament of iso-fineness is prepared；
It will be processed after different modified poly ester POY of two kinds of filament numbers and silk by DTY technique, modified poly ester POY
Different fibre is made after DTY process flow substantially the same manner as Example 1 using DTY equipment identical with 1 structure of embodiment in silk
Spend different dye-uptake low elastic polyester filament, DTY technique difference from example 1 is that, the moving period of frequency conversion silk shifting device is 75
Reciprocal time/min, the parameter of DTY technique are as follows: spinning speed 700m/min, overfeed rate of setting 5.5%, winding overfeed rate
5.5%, the first 200 DEG C of heater temperature, the second 150 DEG C of heater temperature, draw ratio 1.2.
Filament number biggish modified poly ester POY and monofilament in the different dye-uptake low elastic polyester filament of final iso-fineness obtained
The lesser modified poly ester POY fiber numbers ratio of fiber number is 1.5:2；The breaking strength of the different dye-uptake low elastic polyester filament of iso-fineness is
3.0cN/dtex, elongation at break 30.0%, line density deviation ratio are 1.5%, and breaking strength CV value is 4.7%, and fracture is stretched
Long CV value is 9.8%, boiling water shrinkage 5.1%, oil content 2.5wt%, crimp contraction 14.5%；
Dye-uptake of the different dye-uptake low elastic polyester filament of iso-fineness under the conditions of 120 DEG C of temperature is 91.4%, resistance to color of soaping
Fastness reaches 5 grades, and dry fastness reaches 5 grades, and fastness to wet rubbing is 5 grades；
The different dye-uptake low elastic polyester filament of iso-fineness is in Bamboo-shaped, and slub length is 4.63/m.
Embodiment 7
The preparation method of the different dye-uptake low elastic polyester filament of iso-fineness, steps are as follows:
(1) modified poly ester is prepared；
(1.1) 2,2,5,5- tetramethyl -3,4- hexylene glycols, method are synthesized are as follows: firstly, 2 are pressed, 2 methyl propanal and sulfuric acid
The ratio that molar ratio is 1.5:1 by concentration be 340g/L 2,2- butylic aldehyde solution and concentration be 260g/L dilution heat of sulfuric acid
Mixing is added in catholyte pond, then, mixed liquor is cooled to 13 DEG C, then progress electroreduction to 2,2 methyl propanal
Concentration is 9.5wt%, finally carries out crystallisation by cooling, separation and purification, reaction unit and reaction employed in synthesis process
Chemical equation and embodiment 1 are consistent, shown in the structural formula such as formula (I) of obtained 2,2,5,5- tetramethyl -3,4- hexylene glycols, formula
In, R is-H；
(1.2) esterification；
Terephthalic acid (TPA), ethylene glycol and 2,2,5,5- tetramethyl -3,4- hexylene glycol that molar ratio is 1:2.0:0.05 are matched
At slurry, antimony glycol and triphenyl phosphate is added after mixing, pressurization carries out esterification, pressurization pressure in nitrogen atmosphere
Power is 0.3MPa, and it is ester when the water quantity of distillate in esterification reaches the 91% of theoretical value that the temperature of esterification, which is 260 DEG C,
Change reaction end, the additional amount of antimony glycol and triphenyl phosphate be respectively terephthalic acid (TPA) additional amount 0.05wt% and
0.05wt%；
(1.3) polycondensation reaction；
After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, the staged pressure is in 50min
The interior absolute pressure that is steadily evacuated to by normal pressure is 400Pa, and reaction temperature is 260 DEG C, reaction time 50min, then proceedes to take out true
Sky carries out the polycondensation reaction of high vacuum stage of Fig, and reaction pressure is made to be further reduced to absolute pressure 88Pa, reaction temperature 282
DEG C, reaction time 90min, the number-average molecular weight of modified poly ester obtained is 5000, molecular weight distributing index 2.1；
(2) different modified poly ester POY of two kinds of filament numbers are prepared；
It is round that modified poly ester melt, which is squeezed out, through metering, spinneret respectively, is cooling, is oiled and obtains cross section all after winding
Shape and filament number are respectively modified poly ester POY of 0.55dtex and 1.5dtex, the parameter of POY technique are as follows: spinning temperature
280 DEG C, 20 DEG C of cooling temperature, winding speed 3500m/min；
(3) the different dye-uptake low elastic polyester filament of iso-fineness is prepared；
It will be processed after different modified poly ester POY of two kinds of filament numbers and silk by DTY technique, modified poly ester POY
Different fibre is made after DTY process flow substantially the same manner as Example 1 using DTY equipment identical with 1 structure of embodiment in silk
Spend different dye-uptake low elastic polyester filament, DTY technique difference from example 1 is that, the moving period of frequency conversion silk shifting device is 90
Reciprocal time/min, the parameter of DTY technique are as follows: spinning speed 700m/min, overfeed rate of setting 3.5%, winding overfeed rate
5.0%, the first 180 DEG C of heater temperature, the second 145 DEG C of heater temperature, draw ratio 1.5.
Filament number biggish modified poly ester POY and monofilament in the different dye-uptake low elastic polyester filament of final iso-fineness obtained
The lesser modified poly ester POY fiber numbers ratio of fiber number is 1.7:2；The breaking strength of the different dye-uptake low elastic polyester filament of iso-fineness is
2.8cN/dtex, elongation at break 34.0%, line density deviation ratio are 1.38%, and breaking strength CV value is 4.85%, fracture
Extending CV value is 9.8%, boiling water shrinkage 5.1%, oil content 2.8wt%, crimp contraction 14.0%；
Dye-uptake of the different dye-uptake low elastic polyester filament of iso-fineness under the conditions of 120 DEG C of temperature is 90.3%, resistance to color of soaping
Fastness reaches 5 grades, and dry fastness reaches 5 grades, and fastness to wet rubbing is 6 grades；
The different dye-uptake low elastic polyester filament of iso-fineness is in Bamboo-shaped, and slub length is 5.53/m.
Claims (10)
1. the preparation method of the different dye-uptake low elastic polyester filament of iso-fineness, it is characterized in that: two kinds of different modifications of filament number are gathered
It is processed after ester POY and silk by DTY technique, while broken ditch roller is set between zero roller of DTY equipment and first roller
With frequency conversion silk shifting device, modified poly ester tow is passed through from broken ditch surface of roller, the different dye-uptake low elastic polyester filament of iso-fineness is made；
Different modified poly ester POY of two kinds of filament numbers be by POY technique as made from modified poly ester melt；
The modified poly ester the preparation method comprises the following steps: terephthalic acid (TPA), ethylene glycol and hexylene glycol with tert-butyl side group are mixed equal
Esterification and polycondensation reaction are successively carried out after even；
The structural formula of hexylene glycol with tert-butyl side group is as follows:
In formula, R is-H ,-CH2CH3Or-C (CH3)3；
Broken ditch roller is the roller that circumferential surface is carved with multiple annular grooves, multiple annular grooves around roller central axis, and along sieve
The central axis equidistantly distributed of drawing, frequency conversion silk shifting device are made in broken ditch roller circumferential surface along roller central axis for driving polyester POY
It moves back and forth；
The diameter of broken ditch roller end face is 80mm；Spacing between adjacent two groove is 6mm, along roller central axis direction outermost
Two grooves and be all 3.25mm away from the spacing between nearest roller end；The depth of groove is 2.6mm, and width is
4mm, quantity are 4；The moving period of frequency conversion silk shifting device is 5~99 reciprocal times/min；
Second heater temperature of the DTY technique is 130~150 DEG C.
2. the preparation method of the different dye-uptake low elastic polyester filament of iso-fineness according to claim 1, which is characterized in that two kinds of lists
Modified poly ester POY different filament numbers of silk size are respectively 0.5~0.7dtex and 1.5~2.5dtex, and iso-fineness is different
In dye-uptake low elastic polyester filament biggish modified poly ester POY of filament number with filament number lesser modified poly ester POY
Fiber number ratio is 1~2:1~2.
3. the preparation method of the different dye-uptake low elastic polyester filament of iso-fineness according to claim 1, which is characterized in that iso-fineness
Breaking strength >=2.8cN/dtex of different dye-uptake low elastic polyester filament, elongation at break are 33.0 ± 3.0%, line density deviation ratio
≤ 1.5%, breaking strength CV value≤5.0%, extension at break CV value≤10.0%, boiling water shrinkage is 5.9 ± 0.8%, oil-containing
Rate is 2.50 ± 0.50wt%, and crimp contraction is 14.0 ± 0.5%；The different dye-uptake low elastic polyester filament of iso-fineness is at 120 DEG C
Dye-uptake under the conditions of temperature is 87.3~91.4%, and fastness to soaping reaches 5 grades, and dry fastness reaches 5 grades, wet friction
Fastness is greater than 4 grades；The different dye-uptake low elastic polyester filament of iso-fineness is in Bamboo-shaped, and slub length is 0.31~5.80/m.
4. the preparation method of the different dye-uptake low elastic polyester filament of iso-fineness according to claim 1, which is characterized in that two kinds of lists
Modified poly ester POY different cross sections of silk size are all round.
5. the preparation method of the different dye-uptake low elastic polyester filament of iso-fineness according to claim 1, which is characterized in that the band
The synthetic method of the hexylene glycol of tert-butyl side group are as follows: firstly, will be dense in the ratio that raw material A and the molar ratio of sulfuric acid are 1.5~2:1
Catholyte pond is added in the raw material A solution that degree is 300~350g/L and the dilution heat of sulfuric acid mixing that concentration is 200~300g/L
In, then, mixed liquor is cooled to 10~15 DEG C, then carries out electroreduction to the concentration of raw material A and be lower than 10wt%, it is most laggard
Row crystallisation by cooling, separation and purification；
R is-H ,-CH2CH3With-C (CH3)3When, it is 2 that raw material A, which respectively corresponds, 2 methyl propanal, 2,2- dimethyl propione and 2,
24,4- tetramethyl propione.
6. the preparation method of the different dye-uptake low elastic polyester filament of iso-fineness according to claim 5, which is characterized in that described to change
The preparation step of property polyester is as follows:
(1) esterification；
Terephthalic acid (TPA), ethylene glycol and hexylene glycol with tert-butyl side group are made into slurry, catalyst and stabilizer mixing is added
After uniformly, pressurization carries out esterification in nitrogen atmosphere, and moulding pressure is normal pressure~0.3MPa, and the temperature of esterification is
250~260 DEG C, be esterification terminal when the water quantity of distillate in esterification reaches 90% or more of theoretical value；
(2) polycondensation reaction；
After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, the staged pressure is in 30~50min
Interior to be steadily evacuated to absolute pressure 500Pa hereinafter, reaction temperature is 250~260 DEG C by normal pressure, the reaction time is 30~50min, so
After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, so that reaction pressure is further reduced to absolute pressure 100Pa hereinafter,
Reaction temperature is 270~282 DEG C, and the reaction time is 50~90min.
7. the preparation method of the different dye-uptake low elastic polyester filament of iso-fineness according to claim 6, which is characterized in that described right
The molar ratio of phthalic acid, ethylene glycol and the hexylene glycol with tert-butyl side group is 1:1.2~2.0:0.03~0.05, the catalysis
The additional amount of agent and stabilizer is respectively the 0.03~0.05wt% and 0.01~0.05wt% of terephthalic acid (TPA) additional amount.
8. the preparation method of the different dye-uptake low elastic polyester filament of iso-fineness according to claim 7, which is characterized in that described to urge
Agent is antimony oxide, antimony glycol or antimony acetate, and the stabilizer is triphenyl phosphate, trimethyl phosphate or phosphorous acid three
Methyl esters.
9. the preparation method of the different dye-uptake low elastic polyester filament of iso-fineness according to claim 8, which is characterized in that modified poly-
The number-average molecular weight of ester is 25000~30000, and molecular weight distributing index is 1.8~2.2.
10. the preparation method of the different dye-uptake low elastic polyester filament of iso-fineness according to claim 1, which is characterized in that described
The process of POY technique are as follows: metering, spinneret squeeze out, are cooling, oiling and wind；
The parameter of the POY technique are as follows: 280~285 DEG C of spinning temperature, 17~20 DEG C of cooling temperature, winding speed 3200~
3600m/min；
The process of the DTY technique are as follows: seal wire, plying, network, heating stretching, false twisting, thermal finalization and winding；
The parameter of the DTY technique are as follows: 500~700m/min of spinning speed, overfeed rate of setting 3.5~5.5%, winding overfeed rate
3.0~5.5%, the first 180~200 DEG C of heater temperature, draw ratio 1.2~1.7.
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