CN104532392B - Porous super-bright polyester fiber and preparation method thereof - Google Patents
Porous super-bright polyester fiber and preparation method thereof Download PDFInfo
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Abstract
The invention relates to porous super-bright polyester fiber and a preparation method of the porous super-bright polyester fiber. According to the porous super-bright polyester fiber, melt spinning, multi-pore forming, section heteromorphosis and the like are conducted to make the polyester fiber have the super-bright flickering effect, and the material is modified polyester; a linear spinneret plate is adopted in the melt spinning process; the modified polyester is composed of polyester and amidogen fatty acid glycol ester, the amidogen fatty acid glycol ester is dispersed among the molecular chains of the polyester, and the free volume space of the porous super-bright polyester fiber polyester among the molecular chains inside the fiber is increased by 20 v/v% to 30 v/v% under the condition that the temperature ranges from 90 DEG C to 130 DEG C; the porous super-bright polyester fiber can be used for silk-like fabric, wool-like fabric, corduroy, other pile fabric, woolen yarn, decorative fabric and the like.
Description
Technical field
The invention belongs to modified fibre technical field, relate to a kind of porous superbright light polyester fiber and preparation method thereof.
Background technology
Polyethylene terephthalate (PET) fiber, since coming out, has obtained because of the performance of its excellence rapidly developing, its
Yield has become as the hat of world's synthetic fibers.Polyester fiber has fracture strength and elastic modelling quantity is high, and resilience is moderate, and heat is fixed
Type is excellent, and heat-resisting light resistance is good and a series of premium properties such as acid-fast alkali-proof corrosion resistance, and fabric has crease-resistant, stiffness
The advantage such as good, so, polyester fiber is widely used in the field such as clothing, home textile.
PET belongs to symmetric straight chain macromolecular, and strand does not contains side-chain radical, and regularity is the best, and its main chain contains
The phenyl ring of rigidity and flexible alkyl, and the ester group being directly connected with phenyl ring and phenyl ring constitute the conjugated system of rigidity, from
And constrain rotating freely of its soft segment.This structure is it will be evident that add molecule on the impact of glass transition temperature
The wall ridge of sub-chain motion, the glass transition temperature of PET is higher, needs to dye at very high temperatures, promote dye molecule to
The diffusion of fibrous inside.It addition, the strand of PET is regular, good crystallinity, strand arrangement closely, and does not has on strand
Having the polar group having an effect with dye molecule, the colouring making polyester fiber is more difficult.
For solving the problem of PET dyeing difficulty, now use techniques or methods mainly by introduce dye molecule accept base or
The method increasing polyester amorphous regions amount, although the dyeability of polyester can be improved, destroy the segment regularity of PET,
The raising of dyeability is obtained with the performance of reduction polyester fiber.In the case of not destroying polyester fiber crystallinity and permutation degree,
The method used at present has three kinds of colouring methods such as support methods, high temperature and high pressure method and high temperature thermosoling.
Porous superbright light polyester fiber, mainly by melt spinning, many hole counts, cross section special-shapedization etc., gives polyester fiber tool
There are the gloss as real silk and softness, fabric to become clear to feel and the silk light sensation of soft elegance, not only have outside excellent optical characteristics,
Owing to the radical of fiber is big, the arrangement between fiber cannot be tight, and space increases accordingly, thus fabric feeling is more abundant, fluffy
Property, good permeability, have superbright flash effect.Its product is mainly used in the floss classes such as silk like fabric fabric, wool-like fabric, corduroy
Fabric, knitting wool, drapery etc..Before especially having wide market in clothing, decoration and the big field of fabrics for industrial use three
Scape and economic benefit.
Summary of the invention
It is an object of the invention to provide a kind of porous superbright light polyester fiber and preparation method thereof, the present invention utilizes amino fatty acid second
Diol ester is when uniform temperature condition, and the increasing degree of free volume is far longer than the characteristic of polyester macromolecule chain, divides by improving
Dissipate dyestuff molecule and enter the degree within polyester, improve the dyeability of polyester；Simultaneously because amino fatty acid ethylene glycol
In the existence of the first amino in ester molecule, increase the hydrogen bond action between itself and polyester macromolecule chain, add the phase of it and polyester
Capacitive and dispersion in the polyester, decrease migration to greatest extent.Polyester construction regularity, crystallinity are not broken simultaneously
Bad, maintain the premium properties of polyester.
A kind of porous superbright light polyester fiber of the present invention, is obtained, described porous superbright light polyester fiber master by modified poly ester spinning
If by melt spinning, many hole counts, cross section special-shapedization etc., give polyester fiber superbright flash effect, described melt spinning mistake
Cheng Caiyong " one " font spinneret, the length-width ratio of spinneret orifice is 20:1, and described modified poly ester is by polyester and amino fatty acid second
Diol ester is constituted, and described amino ethylene glycol fatty acid is dispersed in the molecule interchain of described polyester, and described amino fatty acid second two
Alcohol ester has hydrogen bond action with the molecule interchain of described polyester, makes the described amino ethylene glycol fatty acid strand with described polyester
Position relatively is fixed；Described porous superbright light polyester fiber under the conditions of temperature is 90～130 DEG C, fibrous inside molecule interchain from
20～30% are increased by volumetric spaces；Described modified poly ester uses ring quenching technique in spinning process；Described porous superbright light gathers
Fracture strength >=the 3.0cN/dtex of ester fiber, elongation at break is 30.0 ± 3.0%；
The molecular structure of described amino ethylene glycol fatty acid is:
H2N(CH2)nCOOCH2CH2OOC(CH2)n NH2；
Wherein, n=10-50.
As preferred technical scheme:
Described a kind of porous superbright light polyester fiber, line density deviation ratio≤2.0% of described porous superbright light polyester fiber, disconnected
Resistance to spalling CV value≤5.0%, extension at break CV value≤10.0%, yarn unevenness CV≤2.00%, boiling water shrinkage 7.0 ±
0.5%, oil content 1.00 ± 0.20%.
Described a kind of porous superbright light polyester fiber, described amino ethylene glycol fatty acid accounts for described porous superbright light polyester fiber
Percentage by weight be 0.5～2.5%.
Present invention also offers the preparation method of a kind of porous superbright light polyester fiber, modified poly ester is blown through metering, extrusion, ring
Air cooling, oil, pre-Network device, stretching, thermal finalization, master network and winding, prepare porous superbright light polyester fiber；
The temperature of described extrusion is 280～290 DEG C；
The pathogenic wind-warm of described cooling is 21～23 DEG C；
Described ring blowing humidity is 80～85 DEG C；
Described oil nozzle away from plate identity distance from for 400～800mm；
Described pre-network pressure is 0.02～0.06Mpa；
Described network pressure is 0.20～0.30Mpa；
A described roller speed is 2200～2600m/min；
A described roll temperature is 75～85 DEG C；
Described two roller speed are 3600～3900m/min；
Described two roll temperatures are 115～135 DEG C；
The speed of described winding is 3600～3800m/min；
Filament number is 0.3～0.7dtex；
The preparation process of described modified poly ester includes:
(1) preparation of amino ethylene glycol fatty acid:
(1) preparation of amino ethylene glycol fatty acid:
1) binary of fatty acids is added in reactor with the amount of 1:1.5 mol ratio with methanol, under the catalysis of concentrated sulphuric acid, be heated to
80～110 DEG C, refuxing esterification, cooling, separating-purifying obtains binary of fatty acids mono-methyl；Described binary of fatty acids is dodecane two
Carboxylic acid is to the one in dopentacontane dicarboxylic acids；Reaction equation is:
HOOC(CH2)nCOOH+CH3OH→CH3OOC(CH2)nCOOH
Wherein n=10～50；
2) by described binary of fatty acids mono-methyl, lead tetraacetate and lithium bromide during 1:1:1 is dissolved in benzene in molar ratio, wherein binary fat
The concentration of fat acid mono-methyl is 0.05～0.1mol/L, and under nitrogen atmosphere, 80～90 DEG C of reactions, backflow, when no longer there being gas
During generation, add a certain amount of dilute sulfuric acid and react 2～3 hours, be washed out, purify and be dried, obtain product bromo fatty acid；
Reaction equation is:
3) by the ammonia of bromo fatty acid and 15～25wt% during 1:2 joins reactor in molar ratio, stirring, the most instead
Should, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is less than 70 DEG C, until bubble-free
Producing, i.e. stop distillation, then carry out cooling down and sucking filtration, filter cake is washed with deionized water to without bromide ion, by product vacuum
It is dried to obtain product amino fatty acid；Vacuum drying temperature can use 60～70 DEG C；Reaction equation is:
HOOC(CH2)nBr+NH3→HOOC(CH2)nNH2+NH4Br；
4) ethylene glycol and amino fatty acid are stirred for 1.1:2 in molar ratio, and one of press the percentage of amino fatty acid wt
Adding the sulphuric acid that concentration is 40～50wt% is catalyst, carries out esterification, and esterification reaction temperature is 160～220 DEG C, esterification water
It is esterification terminal that quantity of distillate reaches more than the 90% of theoretical value；The separated purification of product obtains amino fatty acid ethylene glycol
Ester；Reaction equation is:
HOOC(CH2)nNH2+HOCH2CH2OH→
H2N(CH2)nCOOCH2CH2OOC(CH2)nNH2；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
Use p-phthalic acid and ethylene glycol as raw material, carry out esterification after being made into uniform sizing material, obtain esterification products；Ester
Changing reaction to pressurize in nitrogen atmosphere, Stress control is at normal pressure～0.3MPa, and temperature is at 250～260 DEG C, and esterification water quantity of distillate reaches
More than the 90% of theoretical value is esterification terminal；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
In the described polycondensation reaction coarse vacuum stage, esterification products adds catalyst and stabilizer, under conditions of negative pressure, starts contracting
Poly-reaction, this staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, and temperature controls at 260～270 DEG C, during reaction
Between be 30～50 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino ethylene glycol fatty acid, and stir, generally stirring 15～20
Minute；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure drop
To absolute pressure less than 100Pa, reaction temperature controls at 275～280 DEG C, response time 50～90 minutes；
Prepare modified poly ester.
The preparation method of a kind of porous superbright light polyester fiber as above, described ethylene glycol and described p-phthalic acid mole
Ratio is 1.2～2.0:1.
The preparation method of a kind of porous superbright light polyester fiber as above, described catalyst is selected from antimony oxide, ethylene glycol
One in antimony and antimony acetate, catalyst amount is the 0.01%～0.05% of described p-phthalic acid weight.
The preparation method of a kind of porous superbright light polyester fiber as above, described stabilizer is selected from triphenyl phosphate, tricresyl phosphate
One in methyl ester and NSC 6513, stabilizing agent dosage is the 0.01%～0.05% of described p-phthalic acid weight.
The preparation method of a kind of porous superbright light polyester fiber as above, is washed with deionized water to without using nitre bromide ion
Acid silver solution detection.
The preparation method of a kind of porous superbright light polyester fiber as above, described concentrated sulphuric acid refers to that mass concentration is 70～80%
Sulphuric acid, concentrated sulphuric acid addition is the 1～3wt% of binary of fatty acids；Described a certain amount of dilute sulfuric acid refers to that mass concentration is 40～50%
Sulphuric acid, dilute sulfuric acid addition is the 1～3wt% of binary of fatty acids mono-methyl.
Polyester fiber is when dyeing, and disperse dyes can be divided into the following four stage to the upper dye process of polyester fiber:
1) disperse dyes flowing with dye liquor in dye liquor moves closer to fiber interface；2) disperse dyes are fast near fiber interface
Speed is adsorbed by fiber surface；3), after disperse dyes are adsorbed to fiber surface, in fiber, a concentration difference or inside and outside dyestuff are produced
Chemical potential difference, dyestuff will spread to fibrous inside；4) disperse dyes diffusion velocity and fiber unformed area content, hole or from
Relevant by volume content, therefore the dyeing speed of disperse dyes is in addition to dyestuff dissolubility in the solution, further depends on fiber
Structure is outer and during dyeing the degree of swelling of fiber relevant.
Polyster fibre is hydrophobic synthetic fibers, terylene molecular structure lacks as cellulose or protein fibre can and
There is the active group combined in dyestuff, terylene molecules align must compare closely, only exist less space in fiber, in dyeing
Time humidity under the conditions of, polyester fiber will not can be by the most swelling and make space increase as cotton fiber, dye molecule is difficult to join
Thoroughly to fibrous inside.Therefore, raising will assist in the carrying out of dyeing to the free volume between fiber molecule.
The molecular chain structure of polyester is the linear macromolecule containing benzene ring structure, the functional group's marshalling on strand, unbranched,
Macromole chain flexibility is poor.The regularity of polyester is good and rigidity is the biggest simultaneously, and intermolecular active force is bigger.High with other
Molecular material is compared, and the strand generation sliding of polyester, rotation the most more difficulty, these characteristics hinder dyestuff and enter in polyester
Portion, thus dyeability is poor.
It is main that amino ethylene glycol fatty acid is mainly with C-C, C-O key, has certain molecular weight simultaneously, i.e. has a fixed length
The strand of degree, strand flexibility is relatively big, and the amount of crimp of amino ethylene glycol fatty acid is compared with the linear macromolecule of benzene ring structure
Bigger, simultaneously strong compared with the linear macromolecule containing benzene ring structure to the sensitivity of temperature.When the temperature is changed, amino fatty acid second two
Alcohol ester moves prior to the linear macromolecule containing benzene ring structure, and the produced free volume of motion is far longer than containing benzene ring structure
Produced by linear macromolecule.
Added the free volume diffusion with increase dyestuff of polyester fiber by fatty acid ester, improve the dyeing of polyester fiber
Performance, makes fiber obtain high dye-uptake.
Oxygen in fatty acid ester can form hydrogen bond, but oxygen is when centre position, due to space steric effect and fatty acid ester
The factors such as the curling of molecule reduce the quantity of itself and the hydrogen evolution hydrogen bond in polyester macromolecule chain；If amino is on α position, i.e. ammonia
Base acids, owing to amino and carbonyl interact, is also unfavorable for amino and the hydrogen evolution hydrogen bond in polyester macromolecule chain；Work as amino
The amino of fatty acid ester is when the end position of macromole, and the curling of macromole is little on its impact, adds in amino fatty acid ester
Amino and the formation of the hydrogen evolution hydrogen bond in polyester macromolecule chain, improve between amino fatty acid ester and polyester macromolecule chain simultaneously
Active force, decrease sliding and the migration of amino fatty acid ester.
Add amino fatty acid ester and the compatibility of polyester and dispersion in the polyester, decrease migration to greatest extent.With
Time polyester construction regularity, crystallinity are not destroyed, maintain the premium properties of polyester.
Beneficial effect:
The modified poly ester of gained the most of the present invention, owing to amino ethylene glycol fatty acid is based on C-C, has certain molecular weight simultaneously,
I.e. having the strand of certain length, strand flexibility is relatively big, and amino adds the compatibility with polyester, the fibre of gained
It is good with the compatibility of amino ethylene glycol fatty acid to tie up.
2. due in amino ethylene glycol fatty acid molecule in the existence of the first amino, increase the hydrogen between it and polyester macromolecule chain
Key effect, adds its compatibility with polyester and dispersion in the polyester, decreases migration to greatest extent.
The modified poly ester of gained the most of the present invention, owing to the content of amino ethylene glycol fatty acid is less, to polyester construction regularity, knot
Crystalline substance does not destroy, and maintains the premium properties of polyester.
4. the amount of crimp of amino ethylene glycol fatty acid is bigger compared with the linear macromolecule of benzene ring structure, relatively contains the sensitivity of temperature simultaneously
The linear macromolecule having benzene ring structure is strong.When the temperature is changed, move prior to the linear macromolecule containing benzene ring structure, ammonia
The linear macromolecule that the produced free volume of motion of base ethylene glycol fatty acid is far longer than containing benzene ring structure is produced
, increase the diffusion of additive, improve the functional of polyester.
5. fatty acid ester adds the free volume diffusion with increase dyestuff of polyester fiber, improves the dyeability of polyester fiber.
6. porous superbright light polyester fiber has the gloss as real silk and softness, fabric become clear and feel and the silk light sensation of soft elegance, no
Only having outside excellent optical characteristics, fabric feeling is more abundant, bulkiness, good permeability, has superbright flash effect.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention is expanded on further.Should be understood that these embodiments be merely to illustrate the present invention and
It is not used in restriction the scope of the present invention.In addition, it is to be understood that after having read the content that the present invention lectures, those skilled in the art
Can make various changes or modifications the present invention, these equivalent form of values fall within the model that the application appended claims is limited equally
Enclose.
A kind of porous superbright light polyester fiber of the present invention, material is modified poly ester, and described modified poly ester is by polyester and amino fat
Acid glycol ester is constituted, and described amino ethylene glycol fatty acid is dispersed in the molecule interchain of described polyester, and described amino fatty acid
Glycol ester has hydrogen bond action with the molecule interchain of described polyester, makes the molecule of described amino ethylene glycol fatty acid and described polyester
The relative position of chain is fixed；Described porous superbright light polyester fiber under the conditions of temperature is 90～130 DEG C, fibrous inside molecule interchain
Free volume space increase 20～30v/v%；Described modified poly ester uses ring quenching technique in spinning process；Described porous
Fracture strength >=the 3.0cN/dtex of superbright light polyester fiber, elongation at break is 30.0 ± 3.0%；
The molecular structure of described amino ethylene glycol fatty acid is:
H2N(CH2)nCOOCH2CH2OOC(CH2)n NH2；
Wherein, n=10-50.
Described a kind of porous superbright light polyester fiber, line density deviation ratio≤2.0% of described porous superbright light polyester fiber, disconnected
Resistance to spalling CV value≤5.0%, extension at break CV value≤10.0%, yarn unevenness CV≤2.00%, boiling water shrinkage 7.0 ±
0.5%, oil content 1.00 ± 0.20%.
Described a kind of porous superbright light polyester fiber, described amino ethylene glycol fatty acid accounts for described porous superbright light polyester fiber
Percentage by weight be 0.5～2.5%.
Colouring method: dyeing disperse dyes are Disperse Red 3B, the disperse blue SE-2R bright blue S-GL of dispersion, fiber is respectively at height
Temperature high-pressure unit dyes.Before dye, fiber nonionic surfactant processes 30 minutes at 60 DEG C.Dye dosage is 2.0% (o.w.f)；
Dispersant NNO1.2g/L, pH value is 5, and bath raio is 1:50,60 DEG C of people's dyes, is warming up to 90 DEG C, 100 DEG C, 110 DEG C, 120 DEG C
Each constant temperature dyeing 1h.
Dye uptake uses residual liquid colorimetry to determine, draws appropriate dyeing stock solution and dyeing residual liquid, adds N, N-2 methyl
Methanamide (DMF) and distilled water, the ratio making the DMF in dye liquor to be measured and water is 70/30 (v/v), dye liquor absorbance
Employing ultraviolet-visible spectrophotometer measures, and calculates dye uptake with following formula.
In above formula, A0 and A1 is respectively dyeing stock solution and the absorbance of dyeing residual liquid.
Embodiment 1
The preparation method of a kind of porous superbright light polyester fiber, comprises the following steps
(1) preparation of amino ethylene glycol fatty acid:
1) dodecanedicarboxylic acid is added in reactor with methanol with the amount of 1:1.5 mol ratio, under the catalysis of concentrated sulphuric acid, heating
To 80 DEG C, refuxing esterification, cooling, separating-purifying obtains dodecanedicarboxylic acid mono-methyl；Described concentrated sulphuric acid refers to that quality is dense
Degree is the sulphuric acid of 70%, and concentrated sulphuric acid addition is the 3wt% of dodecanedicarboxylic acid；
2) described dodecanedicarboxylic acid mono-methyl, lead tetraacetate and lithium bromide are dissolved in benzene (mol ratio 1:1:1), wherein 12
Alkane mono methyl dicarboxylate's concentration is 0.05mol/L, under nitrogen atmosphere, in 80 DEG C of reactions, backflow, produces when no longer there being gas
Time raw, add a certain amount of dilute sulfuric acid and react 2 hours, be washed out, purify and be dried, obtain product bromoundecane
Carboxylic acid；Described a certain amount of dilute sulfuric acid refers to the sulphuric acid that mass concentration is 40%, and dilute sulfuric acid addition is dodecanedicarboxylic acid
The 3wt% of mono-methyl；
3) by the ammonia of bromoundecane carboxylic acid Yu 15wt% during 1:2 joins reactor in molar ratio, stirring, the most instead
Should, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 60 DEG C, until bubble-free
Producing, i.e. stop distillation, then carry out cooling down and sucking filtration, filter cake is washed with deionized water to without bromide ion, uses nitre
Acid silver solution detection, obtains product amino-undecanoic carboxylic acid by product vacuum drying；
4) ethylene glycol and amino-undecanoic carboxylic acid are stirred for 1.1:2 in molar ratio, and press amino-undecanoic carboxylic acid weight
1% addition concentration is the sulphuric acid of 40wt%, carries out esterification, and esterification reaction temperature is 160 DEG C, and esterification water quantity of distillate reaches
It is esterification terminal to more than the 90% of theoretical value；The separated purification of product obtains amino-undecanoic carboxylic acid ethylene glycol
Ester；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
The p-phthalic acid using mol ratio to be 1:1.2 and ethylene glycol, as raw material, carry out esterification after being made into uniform sizing material,
To esterification products；Esterification is pressurizeed in nitrogen atmosphere, and Stress control is at 0.3MPa, and temperature is 250 DEG C, esterification water
It is esterification terminal that quantity of distillate reaches more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
In the described polycondensation reaction coarse vacuum stage, esterification products adds the antimony oxide of 0.01% of p-phthalic acid weight and right
The triphenyl phosphate of phthalic acid weight 0.01%, starts polycondensation reaction under conditions of negative pressure, and this staged pressure is put down by normal pressure
Surely being evacuated to below absolute pressure 500Pa, temperature controls at 260 DEG C, and the response time is 50 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino-undecanoic carboxylic acid glycol ester, and stir 15 minutes；Described
Amino-undecanoic carboxylic acid glycol ester, addition is the 0.5wt% of modified poly ester；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure drop
To absolute pressure less than 100Pa, reaction temperature controls at 275 DEG C, 90 minutes response time；
Prepare modified poly ester.
(3) preparation of porous superbright light polyester fiber
By modified poly ester through metering, extrusion, ring quenching, oil, pre-Network device, stretching, thermal finalization, master network and volume
Around, prepare porous superbright light polyester fiber；
The temperature of described extrusion is 290 DEG C；
The pathogenic wind-warm of described cooling is 21 DEG C；
Described ring blowing humidity is 80 DEG C；
Described oil nozzle away from plate identity distance from for 400mm；
Described pre-network pressure is 0.02Mpa；
Described network pressure is 0.20Mpa；
A described roller speed is 2200m/min；
A described roll temperature is 75 DEG C；
Described two roller speed are 3600m/min；
Described two roll temperatures are 115 DEG C；
The speed of described winding is 3800m/min；
Filament number is 0.7dtex；
Gained porous superbright light polyester fiber is under the conditions of temperature is 90 DEG C, and the free volume space of fibrous inside molecule interchain increases
20v/v%, line density deviation ratio-2.0%, fracture strength 3.0cN/dtex, fracture strength CV value 5.0%, elongation at break is
33.0%, extension at break CV value 10.0%, yarn unevenness CV value 2.00%, boiling water shrinkage 6.5%, oil content 1.20%.
Being dyeed by porous superbright light polyester fiber, its dye-uptake is as follows:
The dye uptake (%) of fiber
| Dyestuff | Temperature | 90℃ | 100℃ | 110℃ | 120℃ | 130℃ |
| Disperse Red 3B | Modified fibre | 48.8 | 80.1 | 89.7 | 90.5 | 91.4 |
| General fibre | 28.2 | 46.3 | 78.5 | 81.7 | 90.2 | |
| Disperse blue SE-2R | Modified fibre | 52.5 | 85.1 | 92.1 | 93.4 | 93.4 |
| General fibre | 12.3 | 35.2 | 73.4 | 88.9 | 91.3 | |
| Disperse bright blue S-GL | Modified fibre | 48.5 | 73.8 | 84.6 | 87.1 | 88.7 |
| General fibre | 11.8 | 36.3 | 70.9 | 75.6 | 82.6 |
Embodiment 2
The preparation method of a kind of porous superbright light polyester fiber, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) dopentacontane dicarboxylic acids is added in reactor with the amount of 1:1.5 mol ratio with methanol, under the catalysis of concentrated sulphuric acid, add
Heat is to 110 DEG C, and refuxing esterification, cooling, separating-purifying obtains dopentacontane mono methyl dicarboxylate；Described concentrated sulphuric acid refers to matter
Amount concentration is the sulphuric acid of 70%, and concentrated sulphuric acid addition is the 3wt% of dopentacontane dicarboxylic acids；
2) described dopentacontane mono methyl dicarboxylate, lead tetraacetate and lithium bromide are dissolved in benzene (mol ratio 1:1:1), Qi Zhongwu
Dodecanedicarboxylic acid mono-methyl concentration is 0.07mol/L, and under nitrogen atmosphere, 85 DEG C of reactions, backflow, when no longer there being gas
When body produces, add a certain amount of dilute sulfuric acid and react 3 hours, be washed out, purify and be dried, obtain product bromo five
Hendecane carboxylic acid；Described a certain amount of dilute sulfuric acid refers to the sulphuric acid that mass concentration is 40%, and dilute sulfuric acid addition is 52
The 3wt% of alkane mono methyl dicarboxylate；
3) by the ammonia of bromo henpentacontane carboxylic acid Yu 25wt% during 1:2 joins reactor in molar ratio, stirring, at room temperature
Reaction, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 62 DEG C, until depletion of QI
Bubble produces, and i.e. stops distillation, then carries out cooling down and sucking filtration, and filter cake is washed with deionized water to without bromide ion, uses
Silver nitrate solution detects, and product vacuum drying is obtained product amino henpentacontane carboxylic acid；
4) ethylene glycol and amino henpentacontane carboxylic acid are stirred for 1.1:2 in molar ratio, and press amino henpentacontane carboxylic acid weight
2% addition concentration of amount is the sulphuric acid of 45wt%, carries out esterification, and esterification reaction temperature is 220 DEG C, and esterification water distillates
It is esterification terminal that amount reaches more than the 90% of theoretical value；The separated purification of product obtains amino henpentacontane carboxylic acid
Glycol ester；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
The p-phthalic acid using mol ratio to be 1:2.0 and ethylene glycol, as raw material, carry out esterification after being made into uniform sizing material,
To esterification products；Esterification is pressurizeed in nitrogen atmosphere, Stress control at 0.2MPa, temperature at 260 DEG C, esterification water
It is esterification terminal that quantity of distillate reaches more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
In the described polycondensation reaction coarse vacuum stage, esterification products adds the antimony oxide of 0.05% of p-phthalic acid weight and right
The triphenyl phosphate of phthalic acid weight 0.05%, starts polycondensation reaction under conditions of negative pressure, and this staged pressure is put down by normal pressure
Surely being evacuated to below absolute pressure 500Pa, temperature controls at 270 DEG C, and the response time is 30 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino henpentacontane carboxylic acid glycol ester, and stir 20 minutes；Institute
Stating the percentage by weight that amino henpentacontane carboxylic acid glycol ester addition is modified poly ester is 2.5%；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure drop
To absolute pressure less than 100Pa, reaction temperature controls at 280 DEG C, 50 minutes response time；
Prepare modified poly ester.
(3) preparation of porous superbright light polyester fiber
By modified poly ester through metering, extrusion, ring quenching, oil, pre-Network device, stretching, thermal finalization, master network and volume
Around, prepare porous superbright light polyester fiber；
The temperature of described extrusion is 280 DEG C；
The pathogenic wind-warm of described cooling is 23 DEG C；
Described ring blowing humidity is 85 DEG C；
Described oil nozzle away from plate identity distance from for 800mm；
Described pre-network pressure is 0.06Mpa；
Described network pressure is 0.30Mpa；
A described roller speed is 2600m/min；
A described roll temperature is 85 DEG C；
Described two roller speed are 3900m/min；
Described two roll temperatures are 135 DEG C；
The speed of described winding is 3600m/min；
Filament number is 0.3dtex；
Gained porous superbright light polyester fiber is under the conditions of temperature is 100 DEG C, and the free volume space of fibrous inside molecule interchain increases
Big 25v/v%, line density deviation ratio 2.0%, fracture strength 4.0cN/dtex, fracture strength CV value 4.0%, elongation at break is
27.0%, extension at break CV value 9.0%, yarn unevenness CV value 1.50%, boiling water shrinkage 7.5%, oil content 0.80%.
Being dyeed by porous superbright light polyester fiber, its dye-uptake is as follows:
The dye uptake (%) of fiber
| Dyestuff | Temperature | 90℃ | 100℃ | 110℃ | 120℃ | 130℃ |
| Disperse Red 3B | Modified fibre | 48.4 | 80.3 | 89.9 | 90.8 | 91.6 |
| General fibre | 28.2 | 46.3 | 78.5 | 81.7 | 90.2 | |
| Disperse blue SE-2R | Modified fibre | 52.4 | 85.8 | 92.4 | 93.8 | 94.1 |
| General fibre | 12.3 | 35.2 | 73.4 | 88.9 | 91.3 | |
| Disperse bright blue S-GL | Modified fibre | 48.7 | 74.0 | 84.8 | 87.3 | 88.9 |
| General fibre | 11.8 | 36.3 | 70.9 | 75.6 | 82.6 |
Embodiment 3
The preparation method of a kind of porous superbright light polyester fiber, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) pentacosane dicarboxylic acid is added in reactor with methanol with the amount of 1:1.5 mol ratio, under the catalysis of concentrated sulphuric acid, heating
To 85 DEG C, refuxing esterification, cooling, separating-purifying obtains pentacosane dicarboxylic acid mono-methyl；Described concentrated sulphuric acid refers to that quality is dense
Degree is the sulphuric acid of 70%, and concentrated sulphuric acid addition is the 3wt% of pentacosane dicarboxylic acid；
2) described pentacosane dicarboxylic acid mono-methyl, lead tetraacetate and lithium bromide are dissolved in benzene (mol ratio 1:1:1), wherein 15
Alkane mono methyl dicarboxylate's concentration is 0.08mol/L, under nitrogen atmosphere, in 90 DEG C of reactions, backflow, produces when no longer there being gas
Time raw, add a certain amount of dilute sulfuric acid and react 2.5 hours, be washed out, purify and be dried, obtain product bromotetradecane
Carboxylic acid；Described a certain amount of dilute sulfuric acid refers to the sulphuric acid that mass concentration is 50%, and dilute sulfuric acid addition is pentacosane dicarboxylic acid
The 3wt% of mono-methyl；
3) by the ammonia of bromotetradecane carboxylic acid Yu 20wt% during 1:2 joins reactor in molar ratio, stirring, the most instead
Should, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 60 DEG C, until bubble-free
Producing, i.e. stop distillation, then carry out cooling down and sucking filtration, filter cake is washed with deionized water to without bromide ion, uses nitre
Acid silver solution detection, obtains product amino tetradecane carboxylic acid by product vacuum drying；
4) ethylene glycol and amino tetradecane carboxylic acid are stirred for 1.1:2 in molar ratio, and press amino tetradecane carboxylic acid weight
2% addition concentration is the sulphuric acid of 50wt%, carries out esterification, and esterification reaction temperature is 190 DEG C, and esterification water quantity of distillate reaches
It is esterification terminal to more than the 90% of theoretical value；The separated purification of product obtains amino tetradecane carboxylic acid ethylene glycol
Ester；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
The p-phthalic acid using mol ratio to be 1:1.6 and ethylene glycol, as raw material, carry out esterification after being made into uniform sizing material,
To esterification products；Esterification is pressurizeed in nitrogen atmosphere, Stress control at 0.3MPa, temperature at 255 DEG C, esterification water
It is esterification terminal that quantity of distillate reaches more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
In the described polycondensation reaction coarse vacuum stage, esterification products adds the antimony oxide of 0.03% of p-phthalic acid weight and right
The triphenyl phosphate of phthalic acid weight 0.03%, starts polycondensation reaction under conditions of negative pressure, and this staged pressure is put down by normal pressure
Surely being evacuated to below absolute pressure 500Pa, temperature controls at 265 DEG C, and the response time is 40 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino tetradecane carboxylic acid glycol ester, and stir 16 minutes；Described
Amino tetradecane carboxylic acid glycol ester addition be the percentage by weight of modified poly ester be 1.0%；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure drop
To absolute pressure less than 100Pa, reaction temperature controls at 276 DEG C, 70 minutes response time；
Prepare modified poly ester.
(3) preparation of porous superbright light polyester fiber
By modified poly ester through metering, extrusion, ring quenching, oil, pre-Network device, stretching, thermal finalization, master network and volume
Around, prepare porous superbright light polyester fiber；
The temperature of described extrusion is 285 DEG C；
The pathogenic wind-warm of described cooling is 21 DEG C；
Described ring blowing humidity is 81 DEG C；
Described oil nozzle away from plate identity distance from for 450mm；
Described pre-network pressure is 0.03Mpa；
Described network pressure is 0.22Mpa；
A described roller speed is 2300m/min；
A described roll temperature is 77 DEG C；
Described two roller speed are 3700m/min；
Described two roll temperatures are 120 DEG C；
The speed of described winding is 3700m/min；
Filament number is 0.5dtex；
Gained porous superbright light polyester fiber is under the conditions of temperature is 130 DEG C, and the free volume space of fibrous inside molecule interchain increases
Big 30v/v%, line density deviation ratio-1.0%, fracture strength 3.3cN/dtex, fracture strength CV value 5.3%, elongation at break
It is 31.0%, extension at break CV value 9.8%, yarn unevenness CV value 1.90%, boiling water shrinkage 6.6%, oil content 1.00%.
Being dyeed by porous superbright light polyester fiber, its dye-uptake is as follows:
The dye uptake (%) of fiber
| Dyestuff | Temperature | 90℃ | 100℃ | 110℃ | 120℃ | 130℃ |
| Disperse Red 3B | Modified fibre | 48.5 | 79.8 | 89.1 | 903 | 91.0 |
| General fibre | 28.2 | 46.3 | 78.5 | 81.7 | 90.2 | |
| Disperse blue SE-2R | Modified fibre | 52.7 | 85.0 | 91.5 | 93.0 | 93.5 |
| General fibre | 12.3 | 35.2 | 73.4 | 88.9 | 91.3 | |
| Disperse bright blue S-GL | Modified fibre | 48.1 | 73.4 | 84.2 | 87.1 | 88.5 |
| General fibre | 11.8 | 36.3 | 70.9 | 75.6 | 82.6 |
Embodiment 4
The preparation method of a kind of porous superbright light polyester fiber, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) eicosane dicarboxylic acids is added in reactor with methanol with the amount of 1:1.5 mol ratio, under the catalysis of concentrated sulphuric acid, heating
To 85 DEG C, refuxing esterification, cooling, separating-purifying obtains eicosane mono methyl dicarboxylate；Described concentrated sulphuric acid refers to that quality is dense
Degree is the sulphuric acid of 70%, and concentrated sulphuric acid addition is the 3wt% of eicosane dicarboxylic acids；
2) described eicosane mono methyl dicarboxylate, lead tetraacetate and lithium bromide are dissolved in benzene (mol ratio 1:1:1), wherein 20
Alkane mono methyl dicarboxylate's concentration is 0.09mol/L, under nitrogen atmosphere, in 80 DEG C of reactions, backflow, produces when no longer there being gas
Time raw, add a certain amount of dilute sulfuric acid and react 2.1 hours, be washed out, purify and be dried, obtain product bromo nonadecane
Carboxylic acid；Described a certain amount of dilute sulfuric acid refers to the sulphuric acid that mass concentration is 43%, and dilute sulfuric acid addition is eicosane dicarboxylic acids
The 2wt% of mono-methyl；
3) by the ammonia of bromo nonadecane carboxylic acid Yu 16wt% during 1:2 joins reactor in molar ratio, stirring, the most instead
Should, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 69 DEG C, until bubble-free
Producing, i.e. stop distillation, then carry out cooling down and sucking filtration, filter cake is washed with deionized water to without bromide ion, uses nitre
Acid silver solution detection, obtains product amino nonadecane carboxylic acid by product vacuum drying；
4) ethylene glycol and amino nonadecane carboxylic acid are stirred for 1.1:2 in molar ratio, and press amino nonadecane carboxylic acid weight
2% addition concentration is the sulphuric acid of 42wt%, carries out esterification, and esterification reaction temperature is 160 DEG C, and esterification water quantity of distillate reaches
It is esterification terminal to more than the 90% of theoretical value；The separated purification of product obtains amino nonadecane carboxylic acid ethylene glycol
Ester；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
The p-phthalic acid using mol ratio to be 1:1.2 and ethylene glycol, as raw material, carry out esterification after being made into uniform sizing material,
To esterification products；Esterification is pressurizeed in nitrogen atmosphere, Stress control at 0.15MPa, temperature at 251 DEG C, esterification water
It is esterification terminal that quantity of distillate reaches more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
In the described polycondensation reaction coarse vacuum stage, esterification products adds the antimony oxide of 0.02% of p-phthalic acid weight and right
The triphenyl phosphate of phthalic acid weight 0.02%, starts polycondensation reaction under conditions of negative pressure, and this staged pressure is put down by normal pressure
Surely being evacuated to below absolute pressure 500Pa, temperature controls at 262 DEG C, and the response time is 33 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino nonadecane carboxylic acid glycol ester, and stir 17 minutes；Described
Amino nonadecane carboxylic acid glycol ester addition be the percentage by weight of modified poly ester be 1.5%；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure drop
To absolute pressure less than 100Pa, reaction temperature controls at 277 DEG C, 55 minutes response time；
Prepare modified poly ester.
(3) preparation of porous superbright light polyester fiber
By modified poly ester through metering, extrusion, ring quenching, oil, pre-Network device, stretching, thermal finalization, master network and volume
Around, prepare porous superbright light polyester fiber；
The temperature of described extrusion is 288 DEG C；
The pathogenic wind-warm of described cooling is 22 DEG C；
Described ring blowing humidity is 82 DEG C；
Described oil nozzle away from plate identity distance from for 500mm；
Described pre-network pressure is 0.04Mpa；
Described network pressure is 0.24Mpa；
A described roller speed is 2400m/min；
A described roll temperature is 79 DEG C；
Described two roller speed are 3800m/min；
Described two roll temperatures are 125 DEG C；
The speed of described winding is 3800m/min；
Filament number is 0.6dtex
Gained porous superbright light polyester fiber is under the conditions of temperature is 120 DEG C, and the free volume space of fibrous inside molecule interchain increases
Big 30v/v%, line density deviation ratio-0.5%, fracture strength 3.8cN/dtex, fracture strength CV value 4.9%, elongation at break
It is 32.0%, extension at break CV value 9.7%, yarn unevenness CV value 1.70%, boiling water shrinkage 6.8%, oil content 1.10%.
Being dyeed by porous superbright light polyester fiber, its dye-uptake is as follows:
The dye uptake (%) of fiber
| Dyestuff | Temperature | 90℃ | 100℃ | 110℃ | 120℃ | 130℃ |
| Disperse Red 3B | Modified fibre | 49.0 | 80.4 | 88.9 | 90.7 | 91.7 |
| General fibre | 28.2 | 46.3 | 78.5 | 81.7 | 90.2 | |
| Disperse blue SE-2R | Modified fibre | 52.9 | 85.5 | 92.4 | 93.9 | 93.9 |
| General fibre | 12.3 | 35.2 | 73.4 | 88.9 | 91.3 | |
| Disperse bright blue S-GL | Modified fibre | 48.8 | 74.0 | 84.9 | 87.4 | 88.3 |
| General fibre | 11.8 | 36.3 | 70.9 | 75.6 | 82.6 |
Embodiment 5
The preparation method of a kind of porous superbright light polyester fiber, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) melissane dicarboxylic acids is added in reactor with methanol with the amount of 1:1.5 mol ratio, under the catalysis of concentrated sulphuric acid, heating
To 90 DEG C, refuxing esterification, cooling, separating-purifying obtains melissane mono methyl dicarboxylate；Described concentrated sulphuric acid refers to that quality is dense
Degree is the sulphuric acid of 70%, and concentrated sulphuric acid addition is the 3wt% of melissane dicarboxylic acids；
2) described melissane mono methyl dicarboxylate, lead tetraacetate and lithium bromide are dissolved in benzene (mol ratio 1:1:1), wherein 30
Alkane mono methyl dicarboxylate's concentration be 0.10mol/L under nitrogen atmosphere, 85 DEG C of reactions, backflow, produce when no longer there being gas
Time raw, add a certain amount of dilute sulfuric acid and react 2.3 hours, be washed out, purify and be dried, obtain product bromo 29
Alkane carboxylic acid；Described a certain amount of dilute sulfuric acid refers to the sulphuric acid that mass concentration is 40%, and dilute sulfuric acid addition is melissane dicarboxyl
The 3wt% of acid mono-methyl；
3) by the ammonia of bromo nonacosane carboxylic acid Yu 18wt% during 1:2 joins reactor in molar ratio, stirring, at room temperature
Reaction, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 67 DEG C, until depletion of QI
Bubble produces, and i.e. stops distillation, then carries out cooling down and sucking filtration, and filter cake is washed with deionized water to without bromide ion, uses
Silver nitrate solution detects, and product vacuum drying is obtained product amino nonacosane carboxylic acid；
4) ethylene glycol and amino nonacosane carboxylic acid are stirred for 1.1:2 in molar ratio, and press amino nonacosane carboxylic acid weight
2% addition concentration of amount is the sulphuric acid of 48wt%, carries out esterification, and esterification reaction temperature is 170 DEG C, and esterification water distillates
It is esterification terminal that amount reaches more than the 90% of theoretical value；The separated purification of product obtains amino nonacosane carboxylic acid
Glycol ester；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
The p-phthalic acid using mol ratio to be 1:1.5 and ethylene glycol, as raw material, carry out esterification after being made into uniform sizing material,
To esterification products；Esterification is pressurizeed in nitrogen atmosphere, Stress control at 0.3MPa, temperature at 254 DEG C, esterification water
It is esterification terminal that quantity of distillate reaches more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction coarse vacuum stage, in esterification products add p-phthalic acid weight 0.01% antimony glycol and to benzene
The trimethyl phosphate of dioctyl phthalate weight 0.03%, starts polycondensation reaction under conditions of negative pressure, and this staged pressure is steady by normal pressure
Being evacuated to below absolute pressure 500Pa, temperature controls at 266 DEG C, and the response time is 39 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino nonacosane carboxylic acid glycol ester, and stir 18 minutes；Institute
Stating the percentage by weight that amino nonacosane carboxylic acid glycol ester addition is modified poly ester is 2.5%；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure drop
To absolute pressure less than 100Pa, reaction temperature controls at 278 DEG C, 60 minutes response time；
Prepare modified poly ester.
(3) preparation of porous superbright light polyester fiber
By modified poly ester through metering, extrusion, ring quenching, oil, pre-Network device, stretching, thermal finalization, master network and volume
Around, prepare porous superbright light polyester fiber；
The temperature of described extrusion is 282 DEG C；
The pathogenic wind-warm of described cooling is 21 DEG C；
Described ring blowing humidity is 83 DEG C；
Described oil nozzle away from plate identity distance from for 550mm；
Described pre-network pressure is 0.05Mpa；
Described network pressure is 0.26Mpa；
A described roller speed is 2300m/min；
A described roll temperature is 81 DEG C；
Described two roller speed are 3700m/min；
Described two roll temperatures are 126 DEG C；
The speed of described winding is 3600m/min；
Filament number is 0.4dtex；
Gained porous superbright light polyester fiber is under the conditions of temperature is 120 DEG C, and the free volume space of fibrous inside molecule interchain increases
Big 30v/v%, line density deviation ratio-0.1%, fracture strength 4.0cN/dtex, fracture strength CV value 4.4%, elongation at break
It is 28.0%, extension at break CV value 9.0%, yarn unevenness CV value 1.60%, boiling water shrinkage 6.9%, oil content 0.80%.
Being dyeed by porous superbright light polyester fiber, its dye-uptake is as follows:
The dye uptake (%) of fiber
| Dyestuff | Temperature | 90℃ | 100℃ | 110℃ | 120℃ | 130℃ |
| Disperse Red 3B | Modified fibre | 49.7 | 80.6 | 89.8 | 90.9 | 91.7 |
| General fibre | 28.2 | 46.3 | 78.5 | 81.7 | 90.2 | |
| Disperse blue SE-2R | Modified fibre | 53.3 | 86.1 | 92.4 | 93.7 | 94.8 |
| General fibre | 12.3 | 35.2 | 73.4 | 88.9 | 91.3 | |
| Disperse bright blue S-GL | Modified fibre | 48.8 | 74.5 | 84.9 | 87.5 | 89.5 |
| General fibre | 11.8 | 36.3 | 70.9 | 75.6 | 82.6 |
Embodiment 6
The preparation method of a kind of porous superbright light polyester fiber, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) pentatriacontane dicarboxylic acids is added in reactor with the amount of 1:1.5 mol ratio with methanol, under the catalysis of concentrated sulphuric acid, add
Heat is to 95 DEG C, and refuxing esterification, cooling, separating-purifying obtains pentatriacontane mono methyl dicarboxylate；Described concentrated sulphuric acid refers to matter
Amount concentration is the sulphuric acid of 70%, and concentrated sulphuric acid addition is the 2wt% of pentatriacontane dicarboxylic acids；
2) described pentatriacontane mono methyl dicarboxylate, lead tetraacetate and lithium bromide are dissolved in benzene (mol ratio 1:1:1), Qi Zhongsan
Pentacosane dicarboxylic acid mono-methyl concentration be 0.09mol/L under nitrogen atmosphere, 90 DEG C of reactions, backflow, when no longer there being gas
When body produces, add a certain amount of dilute sulfuric acid and react 2.6 hours, be washed out, purify and be dried, obtain product bromo three
Tetradecane carboxylic acid；Described a certain amount of dilute sulfuric acid refers to the sulphuric acid that mass concentration is 45%, and dilute sulfuric acid addition is 35
The 1wt% of alkane mono methyl dicarboxylate
3) by the ammonia of bromo tetratriacontane carboxylic acid Yu 20wt% during 1:2 joins reactor in molar ratio, stirring, at room temperature
Reaction, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 69 DEG C, until depletion of QI
Bubble produces, and i.e. stops distillation, then carries out cooling down and sucking filtration, and filter cake is washed with deionized water to without bromide ion, uses
Silver nitrate solution detects, and product vacuum drying is obtained product amino tetratriacontane carboxylic acid；
4) ethylene glycol and amino tetratriacontane carboxylic acid are stirred for 1.1:2 in molar ratio, and press amino tetratriacontane carboxylic acid weight
1% addition concentration of amount is the sulphuric acid of 50wt%, carries out esterification, and esterification reaction temperature is 180 DEG C, and esterification water distillates
It is esterification terminal that amount reaches more than the 90% of theoretical value；The separated purification of product obtains amino tetratriacontane carboxylic acid
Glycol ester；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
The p-phthalic acid using mol ratio to be 1:1.6 and ethylene glycol, as raw material, carry out esterification after being made into uniform sizing material,
To esterification products；Esterification is pressurizeed in nitrogen atmosphere, Stress control at 0.4MPa, temperature at 256 DEG C, esterification water
It is esterification terminal that quantity of distillate reaches more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction coarse vacuum stage, in esterification products add p-phthalic acid weight 0.04% antimony acetate and to benzene two
The NSC 6513 of formic acid weight 0.02%, starts polycondensation reaction under conditions of negative pressure, and this staged pressure is steady by normal pressure
Being evacuated to below absolute pressure 500Pa, temperature controls at 267 DEG C, and the response time is 40 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino tetratriacontane carboxylic acid glycol ester, and stir 18 minutes；Institute
Stating the percentage by weight that amino tetratriacontane carboxylic acid glycol ester addition is modified poly ester is 2.0%；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure drop
To absolute pressure less than 100Pa, reaction temperature controls at 275 DEG C, 70 minutes response time；
Prepare modified poly ester.
(3) preparation of porous superbright light polyester fiber
By modified poly ester through metering, extrusion, ring quenching, oil, pre-Network device, stretching, thermal finalization, master network and volume
Around, prepare porous superbright light polyester fiber；
The temperature of described extrusion is 288 DEG C；
The pathogenic wind-warm of described cooling is 23 DEG C；
Described ring blowing humidity is 84 DEG C；
Described oil nozzle away from plate identity distance from for 650mm；
Described pre-network pressure is 0.02Mpa；
Described network pressure is 0.28Mpa；
A described roller speed is 2400m/min；
A described roll temperature is 83 DEG C；
Described two roller speed are 3800m/min；
Described two roll temperatures are 130 DEG C；
The speed of described winding is 3800m/min；
Filament number is 0.6dtex
Gained porous superbright light polyester fiber is under the conditions of temperature is 110 DEG C, and the free volume space of fibrous inside molecule interchain increases
Big 25v/v%, line density deviation ratio 0.8%, fracture strength 3.6cN/dtex, fracture strength CV value 4.3%, elongation at break is
30.0%, extension at break CV value 9.7%, yarn unevenness CV value 1.90%, boiling water shrinkage 7.0%, oil content 0.90%.
Being dyeed by porous superbright light polyester fiber, its dye-uptake is as follows:
The dye uptake (%) of fiber
| Dyestuff | Temperature | 90℃ | 100℃ | 110℃ | 120℃ | 130℃ |
| Disperse Red 3B | Modified fibre | 49.4 | 81.3 | 89.2 | 90.7 | 91.0 |
| General fibre | 28.2 | 46.3 | 78.5 | 81.7 | 90.2 | |
| Disperse blue SE-2R | Modified fibre | 53.5 | 85.0 | 92.0 | 93.7 | 93.0 |
| General fibre | 12.3 | 35.2 | 73.4 | 88.9 | 91.3 | |
| Disperse bright blue S-GL | Modified fibre | 48.7 | 73.2 | 84.9 | 87.6 | 88.6 |
| General fibre | 11.8 | 36.3 | 70.9 | 75.6 | 82.6 |
Embodiment 7
The preparation method of a kind of porous superbright light polyester fiber, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) tetracontane dicarboxylic acids is added in reactor with methanol with the amount of 1:1.5 mol ratio, under the catalysis of concentrated sulphuric acid, heating
To 100 DEG C, refuxing esterification, cooling, separating-purifying obtains tetracontane mono methyl dicarboxylate；Described concentrated sulphuric acid refers to that quality is dense
Degree is the sulphuric acid of 70%, and concentrated sulphuric acid addition is the 3wt% of tetracontane dicarboxylic acids；
2) described tetracontane mono methyl dicarboxylate, lead tetraacetate and lithium bromide are dissolved in benzene (mol ratio 1:1:1), wherein 40
Alkane mono methyl dicarboxylate's concentration be 0.06mol/L under nitrogen atmosphere, 80 DEG C of reactions, backflow, produce when no longer there being gas
Time raw, add a certain amount of dilute sulfuric acid and react 2.7 hours, be washed out, purify and be dried, obtain product bromo 39
Alkane carboxylic acid；Described a certain amount of dilute sulfuric acid refers to the sulphuric acid that mass concentration is 48%, and dilute sulfuric acid addition is tetracontane dicarboxyl
The 2wt% of acid mono-methyl；
3) by the ammonia of bromo nonatriacontane carboxylic acid Yu 22wt% during 1:2 joins reactor in molar ratio, stirring, at room temperature
Reaction, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 60 DEG C, until depletion of QI
Bubble produces, and i.e. stops distillation, then carries out cooling down and sucking filtration, and filter cake is washed with deionized water to without bromide ion, uses
Silver nitrate solution detects, and product vacuum drying is obtained product amino nonatriacontane carboxylic acid；
4) ethylene glycol and amino nonatriacontane carboxylic acid are stirred for 1.1:2 in molar ratio, and press amino nonatriacontane carboxylic acid weight
2% addition concentration of amount is the sulphuric acid of 46wt%, carries out esterification, and esterification reaction temperature is 190 DEG C, and esterification water distillates
It is esterification terminal that amount reaches more than the 90% of theoretical value；The separated purification of product obtains amino nonatriacontane carboxylic acid
Glycol ester；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
The p-phthalic acid using mol ratio to be 1:1.8 and ethylene glycol, as raw material, carry out esterification after being made into uniform sizing material,
To esterification products；Esterification is pressurizeed in nitrogen atmosphere, Stress control at 0.2MPa, temperature at 258 DEG C, esterification water
It is esterification terminal that quantity of distillate reaches more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction coarse vacuum stage, in esterification products add p-phthalic acid weight 0.05% antimony acetate and to benzene two
The trimethyl phosphate of formic acid weight 0.03%, starts polycondensation reaction under conditions of negative pressure, and this staged pressure is steadily taken out by normal pressure
To absolute pressure 500Pa, temperature controls at 268 DEG C, and the response time is 45 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino nonatriacontane carboxylic acid glycol ester, and stir 16 minutes；Institute
Stating the percentage by weight that amino nonatriacontane carboxylic acid glycol ester addition is modified poly ester is 1.5%；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure drop
To absolute pressure less than 100Pa, reaction temperature controls at 275 DEG C, 75 minutes response time；
Prepare modified poly ester.
(3) preparation of porous superbright light polyester fiber
By modified poly ester through metering, extrusion, ring quenching, oil, pre-Network device, stretching, thermal finalization, master network and volume
Around, prepare porous superbright light polyester fiber；
The temperature of described extrusion is 286 DEG C；
The pathogenic wind-warm of described cooling is 22 DEG C；
Described ring blowing humidity is 80 DEG C；
Described oil nozzle away from plate identity distance from for 700mm；
Described pre-network pressure is 0.05Mpa；
Described network pressure is 0.29Mpa；
A described roller speed is 2500m/min；
A described roll temperature is 84 DEG C；
Described two roller speed are 3700m/min；
Described two roll temperatures are 132 DEG C；
The speed of described winding is 3700m/min；
Filament number is 0.4dtex；
Gained porous superbright light polyester fiber is under the conditions of temperature is 100 DEG C, and the free volume space of fibrous inside molecule interchain increases
Big 20v/v%, line density deviation ratio 1.1%, fracture strength 4.0cN/dtex, fracture strength CV value 4.5%, elongation at break is
31.0%, extension at break CV value 9.0%, yarn unevenness CV value 1.60%, boiling water shrinkage 7.2%, oil content 0.90%.
Being dyeed by porous superbright light polyester fiber, its dye-uptake is as follows:
The dye uptake (%) of fiber
| Dyestuff | Temperature | 90℃ | 100℃ | 110℃ | 120℃ | 130℃ |
| Disperse Red 3B | Modified fibre | 48.3 | 80.0 | 89.4 | 90.9 | 91.5 |
| General fibre | 28.2 | 46.3 | 78.5 | 81.7 | 90.2 | |
| Disperse blue SE-2R | Modified fibre | 52.7 | 85.9 | 92.4 | 93.0 | 93.1 |
| General fibre | 12.3 | 35.2 | 73.4 | 88.9 | 91.3 | |
| Disperse bright blue S-GL | Modified fibre | 48.4 | 73.4 | 84.9 | 88.5 | 88.4 |
| General fibre | 11.8 | 36.3 | 70.9 | 75.6 | 82.6 |
Embodiment 8
The preparation method of a kind of porous superbright light polyester fiber, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) pentatetracontane dicarboxylic acids is added in reactor with the amount of 1:1.5 mol ratio with methanol, under the catalysis of concentrated sulphuric acid, add
Heat is to 110 DEG C, and refuxing esterification, cooling, separating-purifying obtains pentatetracontane mono methyl dicarboxylate；Described concentrated sulphuric acid refers to matter
Amount concentration is the sulphuric acid of 70%, and concentrated sulphuric acid addition is the 2wt% of pentatetracontane dicarboxylic acids；
2) described pentatetracontane mono methyl dicarboxylate, lead tetraacetate and lithium bromide are dissolved in benzene (mol ratio 1:1:1), Qi Zhongsi
Pentacosane dicarboxylic acid mono-methyl concentration is 0.07mol/L, and under nitrogen atmosphere, 88 DEG C of reactions, backflow, when no longer there being gas
When body produces, add a certain amount of dilute sulfuric acid and react 2.3 hours, be washed out, purify and be dried, obtain product bromo four
Tetradecane carboxylic acid；Described a certain amount of dilute sulfuric acid refers to the sulphuric acid that mass concentration is 45%, and dilute sulfuric acid addition is 45
The 2wt% of alkane mono methyl dicarboxylate；
3) by the ammonia of bromo tetratetracontane carboxylic acid Yu 25wt% during 1:2 joins reactor in molar ratio, stirring, at room temperature
Reaction, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is less than 70 DEG C, until
Bubble-free produces, and i.e. stops distillation, then carries out cooling down and sucking filtration, and filter cake is washed with deionized water to without bromide ion,
Employing silver nitrate solution detects, and product vacuum drying is obtained product amino tetratetracontane carboxylic acid；
4) ethylene glycol and amino tetratetracontane carboxylic acid are stirred for 1.1:2 in molar ratio, and press amino tetratetracontane carboxylic acid weight
1% addition concentration of amount is the sulphuric acid of 50wt%, carries out esterification, and esterification reaction temperature is 210 DEG C, and esterification water distillates
It is esterification terminal that amount reaches more than the 90% of theoretical value；The separated purification of product obtains amino tetratetracontane carboxylic acid
Glycol ester；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
The p-phthalic acid using mol ratio to be 1:2.0 and ethylene glycol, as raw material, carry out esterification after being made into uniform sizing material,
To esterification products；Esterification is pressurizeed in nitrogen atmosphere, Stress control at 0.3MPa, temperature at 260 DEG C, esterification water
It is esterification terminal that quantity of distillate reaches more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction coarse vacuum stage, in esterification products add p-phthalic acid weight 0.02% antimony glycol and to benzene
The trimethyl phosphate of dioctyl phthalate weight 0.05%, starts polycondensation reaction under conditions of negative pressure, and this staged pressure is steady by normal pressure
Being evacuated to below absolute pressure 500Pa, temperature controls at 270 DEG C, and the response time is 50 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino tetratetracontane carboxylic acid glycol ester, and stir 20 minutes；Institute
Stating the percentage by weight that amino tetratetracontane carboxylic acid glycol ester addition is modified poly ester is 2.0%；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure drop
To absolute pressure less than 100Pa, reaction temperature controls at 280 DEG C, 85 minutes response time
Prepare modified poly ester.
(3) preparation of porous superbright light polyester fiber
By modified poly ester through metering, extrusion, ring quenching, oil, pre-Network device, stretching, thermal finalization, master network and volume
Around, prepare porous superbright light polyester fiber；
The temperature of described extrusion is 286 DEG C；
The pathogenic wind-warm of described cooling is 21 DEG C；
Described ring blowing humidity is 85 DEG C；
Described oil nozzle away from plate identity distance from for 750mm；
Described pre-network pressure is 0.06Mpa；
Described network pressure is 0.30Mpa；
A described roller speed is 2600m/min；
A described roll temperature is 84 DEG C；
Described two roller speed are 3800m/min；
Described two roll temperatures are 134 DEG C；
The speed of described winding is 3600m/min；
Filament number is 0.4dtex；
Gained porous superbright light polyester fiber is under the conditions of temperature is 110 DEG C, and the free volume space of fibrous inside molecule interchain increases
Big 25v/v%, line density deviation ratio 1.6%, fracture strength 4.0cN/dtex, fracture strength CV value 4.5%, elongation at break is
31.0%, extension at break CV value 9.0%, yarn unevenness CV value 1.60%, boiling water shrinkage 7.4%, oil content 0.90%.
Being dyeed by porous superbright light polyester fiber, its dye-uptake is as follows:
The dye uptake (%) of fiber
| Dyestuff | Temperature | 90℃ | 100℃ | 110℃ | 120℃ | 130℃ |
| Disperse Red 3B | Modified fibre | 48.4 | 80.0 | 89.4 | 90.9 | 91.5 |
| General fibre | 28.2 | 46.3 | 78.5 | 81.7 | 90.2 | |
| Disperse blue SE-2R | Modified fibre | 52.7 | 85.8 | 92.4 | 93.0 | 93.1 |
| General fibre | 12.3 | 35.2 | 73.4 | 88.9 | 91.3 | |
| Disperse bright blue S-GL | Modified fibre | 48.4 | 73.4 | 84.9 | 88.5 | 88.4 |
| General fibre | 11.8 | 36.3 | 70.9 | 75.6 | 82.6 |
Claims (9)
1. a porous superbright light polyester fiber, is characterized in that: described porous superbright light polyester fiber, mainly by melt spinning, many hole counts, cross section special-shapedization, gives polyester fiber superbright flash effect, and material is modified poly ester；Described melt spinning process uses " one " font spinneret, and the length-width ratio of spinneret orifice is 20:1；Described modified poly ester is made up of with amino ethylene glycol fatty acid polyester, described amino ethylene glycol fatty acid is dispersed in the molecule interchain of described polyester, and the molecule interchain of described amino ethylene glycol fatty acid and described polyester has hydrogen bond action, described amino ethylene glycol fatty acid is made to fix with the relative position of the strand of described polyester；It is 0.5～2.5% that described amino ethylene glycol fatty acid accounts for the percentage by weight of described porous superbright light polyester fiber；Described porous superbright light polyester fiber polyester is under the conditions of temperature is 90～130 DEG C, and the free volume space of fibrous inside molecule interchain increases 20～30v/v%；Described modified poly ester uses ring quenching technique in spinning process；Fracture strength >=the 3.0cN/dtex of described porous superbright light polyester fiber, elongation at break is 30.0 ± 3.0%；
The molecular structure of described amino ethylene glycol fatty acid is:
H2N(CH2)nCOOCH2CH2OOC(CH2)n NH2；
Wherein, n=10-50.
A kind of porous superbright light polyester fiber the most according to claim 1, it is characterized in that, line density deviation ratio≤2.0% of described porous superbright light polyester fiber, fracture strength CV value≤5.0%,, extension at break CV value≤10.0%, yarn unevenness CV≤2.00%, boiling water shrinkage 7.0 ± 0.5%, oil content 1.00 ± 0.20%.
The preparation method of a kind of porous superbright light polyester fiber the most as claimed in claim 1, it is characterized in that by modified poly ester through metering, extrusion, ring quenching, oil, pre-Network device, stretching, thermal finalization, master network and winding, prepare porous superbright light polyester fiber；
The temperature of described extrusion is 280～290 DEG C；
The pathogenic wind-warm of described cooling is 20～23 DEG C；
Described ring blowing humidity is 80～85 DEG C；
Described oil nozzle away from plate identity distance from for 400～800mm；
Described pre-network pressure is 0.02～0.06MPa；
Described network pressure is 0.20～0.30MPa；
A described roller speed is 2200～2600m/min；
A described roll temperature is 75～85 DEG C；
Described two roller speed are 3600～3900m/min；
Described two roll temperatures are 115～135 DEG C；
The speed of described winding is 3600～3800m/min；
Filament number is 0.3～0.7dtex；
The preparation process of described modified poly ester includes:
(1) preparation of amino ethylene glycol fatty acid:
1) being added in reactor with the amount of 1:1.5 mol ratio with methanol by binary of fatty acids, under the catalysis of concentrated sulphuric acid, be heated to 80～110 DEG C, refuxing esterification, cooling, separating-purifying obtains binary of fatty acids mono-methyl；Described binary of fatty acids is dodecanedicarboxylic acid to the one in dopentacontane dicarboxylic acids；
2) by described binary of fatty acids mono-methyl, lead tetraacetate and lithium bromide during 1:1:1 is dissolved in benzene in molar ratio, wherein the concentration of binary of fatty acids mono-methyl is 0.05～0.1mol/L, under nitrogen atmosphere, 80～90 DEG C of reactions, backflow, when no longer there being gas to produce, adds a certain amount of dilute sulfuric acid and reacts 2～3 hours, it is washed out, purifies and is dried, obtain product bromo fatty acid；
3) by the ammonia of bromo fatty acid and 15～25wt% during 1:2 joins reactor in molar ratio, stirring, at room temperature react, then product is added thermal distillation, and absorb ammonia with cold water, add the temperature of thermal distillation less than 70 DEG C, until bubble-free produces, i.e. stop distillation, then carry out cooling down and sucking filtration, filter cake is washed with deionized water to without bromide ion, and product vacuum drying is obtained product amino fatty acid；
4) ethylene glycol and amino fatty acid are stirred for 1.1:2 in molar ratio, and add, by the 1～3% of amino fatty acid wt, the sulphuric acid that concentration is 40～50wt%, carry out esterification, esterification reaction temperature is 160～220 DEG C, and it is esterification terminal that esterification water quantity of distillate reaches more than the 90% of theoretical value；The separated purification of product obtains amino ethylene glycol fatty acid；
(2) preparation of modified poly ester, including esterification and polycondensation reaction:
Described esterification:
Use p-phthalic acid and ethylene glycol as raw material, carry out esterification after being made into uniform sizing material, obtain esterification products；Esterification is pressurizeed in nitrogen atmosphere, and Stress control is at normal pressure～0.3MPa, and temperature is at 250～260 DEG C, and it is esterification terminal that esterification water quantity of distillate reaches more than the 90% of theoretical value；
Described polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction coarse vacuum stage, adding catalyst and stabilizer in esterification products, start polycondensation reaction under conditions of negative pressure, this staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, temperature controls at 260～270 DEG C, and the response time is 30～50 minutes；
After the described polycondensation reaction coarse vacuum stage terminates, add amino ethylene glycol fatty acid, and stir；
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure be down to absolute pressure and is less than 100Pa, and reaction temperature controls at 275～280 DEG C, response time 50～90 minutes；
Prepare modified poly ester.
The preparation method of a kind of porous superbright light polyester fiber the most according to claim 3, it is characterised in that described ethylene glycol is 1.2～2.0:1 with the mol ratio of described p-phthalic acid.
The preparation method of a kind of porous superbright light polyester fiber the most according to claim 3, it is characterized in that, described catalyst one in antimony oxide, antimony glycol and antimony acetate, catalyst amount is the 0.01%～0.05% of described p-phthalic acid weight.
The preparation method of a kind of porous superbright light polyester fiber the most according to claim 3, it is characterized in that, described stabilizer one in triphenyl phosphate, trimethyl phosphate and NSC 6513, stabilizing agent dosage is the 0.01%～0.05% of described p-phthalic acid weight.
The preparation method of a kind of porous superbright light polyester fiber the most according to claim 3, it is characterised in that adding the stirring after amino ethylene glycol fatty acid, the time is 15～20 minutes.
The preparation method of a kind of porous superbright light polyester fiber the most according to claim 3, it is characterised in that be washed with deionized water to without bromide ion, uses silver nitrate solution detection.
The preparation method of a kind of porous superbright light polyester fiber the most according to claim 3, it is characterised in that described concentrated sulphuric acid refers to the sulphuric acid that mass concentration is 70～80%, and concentrated sulphuric acid addition is the 1～3wt% of binary of fatty acids；Described a certain amount of dilute sulfuric acid refers to the sulphuric acid that mass concentration is 40～50%, and dilute sulfuric acid addition is the 1～3wt% of binary of fatty acids mono-methyl.
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