CN104499084A - Polyester fiber FDY (Fully Drawn Yarn) with high dyeing rate and preparation method thereof - Google Patents
Polyester fiber FDY (Fully Drawn Yarn) with high dyeing rate and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a polyester fiber FDY (Fully Drawn Yarn) with high dyeing rate and a preparation method thereof. The polyester fiber FDY with high dyeing rate is prepared from modified polyester, the modified polyester is composed of polyester and aminoadipic acid gylcol ester, the aminoadipic acid gylcol ester is dispersed among molecular chains of the polyester, hydrogen-bond interaction exists between the aminoadipic acid gylcol ester and the molecular chains of the polyester, and the relative position of the aminoadipic acid gylcol ester and the molecular chains of the polyester is fixed; the free volume space among the molecular chains inside the fiber is increased by 20-30v/v% when the polyester fiber FDY with high dyeing rate is at 90-130 DEG C, the dying rate of the polyester fiber FDY with high dyeing rate is higher than that of the common fiber when the polyester fiber FDY with high dyeing rate adopts the same dyes such as disperse red 3B, disperse blue SE-2R, disperse bright blue S-GL and the like, less surface dyeing is formed after dyeing, and the polyester fiber FDY with high dyeing rate can be used for garment materials, bedding article decoration and the like.
Description
Technical field
The invention belongs to modified fibre technical field, relate to a kind of high dye-uptake polyester fiber FDY silk and preparation method thereof.
Background technology
Polyethylene terephthalate (PET) fiber is since appearance, and obtain because of the performance of its excellence and rapidly develop, its output has become the hat of world's synthetic fiber.Polyester fiber has fracture strength and elastic modelling quantity is high, and resilience is moderate, and HEAT SETTING is excellent, a series of premium properties such as the good and acid-fast alkali-proof corrosion resistance of heat-resisting light resistance, and fabric has the advantages such as crease-resistant, stiffness is good, so, the fields such as polyester fiber is widely used in clothes, family is spun.
PET belongs to symmetric straight chain macromolecular, strand is not containing side-chain radical, regularity is very good, its main chain contains the phenyl ring of rigidity and flexible alkyl, and the ester group be directly connected with phenyl ring and phenyl ring constitute the conjugated system of rigidity, thus constrain rotating freely of its soft segment.The impact of this structure on glass transition temperature is obvious, and add the wall ridge of molecule segment motion, the glass transition temperature of PET is higher, needs to dye at very high temperatures, promotes that dye molecule is to the diffusion of fibrous inside.In addition, the strand of PET is regular, good crystallinity, and strand arrangement is tight, and the polar group that strand is not had an effect with dye molecule, make the colouring of polyester fiber more difficult.
For solving the problem of PET dyeing difficulty, now adopt technology or method mainly by introducing the method that dye molecule accepts base or increases polyester amorphous regions amount, although the dyeability of polyester can be improved, destroy the segment regularity of PET, to reduce the performance of polyester fiber to obtain the raising of dyeability.
When not destroying polyester fiber crystallinity and permutation degree, the method adopted at present has three kinds of colouring methods such as support methods, high temperature and high pressure method and high temperature thermosoling.Carrier dyeing utilizes carrier auxiliary agent to the plasticising expanded performance of terylene, and make DISPERSE DYES can contaminate a kind of colouring method of terylene in the condition of normal pressure less than 100 DEG C, carrier to significantly improve class chemical assistant DISPERSE DYES contaminating terylene speed.But at present carrier dyeing, the carrier used is mostly or has certain toxicity or have certain taste, there is problem of environmental pollution, and residual support is not easily cleaned, affects dyefastness, industrially mostly no longer have employed.High temperature hot melt decoration method makes dyestuff that the colouring method of the continuous knot dyeing of set occur on fiber in 185-215 DEG C of dry heat condition, but because fabric is larger by tension force during dyeing, DYED FABRICS feel and colour brightness is even is affected, industrial only have some special kinds to adopt.High-temperature and high pressure dyeing process is at 120-130 DEG C, makes dyestuff that the colouring method of the continuous knot dyeing of set occur on fiber under 3 atmospheric pressure, and due to the particularity of polyster fibre, that only has guarantee fiber under High Temperature High Pressure has a certain amount of dye-uptake.But the energy consumption that high temperature and high pressure method brings and dye-uptake low be the subject matter faced now.
FDY fiber fully stretches, and can be directly used in textile process.
Summary of the invention
The object of this invention is to provide a kind of high dye-uptake polyester fiber FDY silk and preparation method thereof, the present invention utilizes amino ethylene glycol fatty acid when uniform temperature condition, the increasing degree of free volume is far longer than the characteristic of polyester macromolecule chain, entering the degree of polyester inside by improving DISPERSE DYES molecule, improving the dyeability of polyester; Simultaneously due in amino ethylene glycol fatty acid molecule in the first amino existence, increase the hydrogen bond action between itself and polyester macromolecule chain, add compatibility and the dispersion in the polyester of it and polyester, decrease migration to greatest extent.Polyester construction regularity, crystallinity are not destroyed simultaneously, maintain the premium properties of polyester.
One of the present invention high dye-uptake polyester fiber FDY silk, material is modified poly ester, and described high dye-uptake polyester fiber FDY silk is under temperature is 90 ~ 130 DEG C of conditions, and the free volume space between fibrous inside strand increases 20 ~ 30v/v%; Fracture strength >=the 3.8cN/dtex of described high dye-uptake polyester fiber FDY silk, elongation at break is 33.0 ± 3.0%; Described modified poly ester is made up of polyester and amino ethylene glycol fatty acid, described amino ethylene glycol fatty acid is dispersed between the strand of described polyester, and have hydrogen bond action between the strand of described amino ethylene glycol fatty acid and described polyester, the relative position of the strand of described amino ethylene glycol fatty acid and described polyester is fixed;
The molecular structure of described amino ethylene glycol fatty acid is:
H
2N(CH
2)
nCOOCH
2CH
2OOC(CH
2)
nNH
2；
Wherein, n=10-50.
As preferred technical scheme:
Line density deviation ratio≤0.5% of described high dye-uptake polyester fiber FDY silk, fracture strength CV value≤5.0%, extension at break CV value≤10.0%, yarn unevenness CV≤2.00%, boiling water shrinkage 7.5 ± 0.5%, oil content 0.90 ± 0.20%.
The percentage by weight that described amino ethylene glycol fatty acid accounts for described high dye-uptake polyester fiber FDY silk is 0.5 ~ 2.5%.
Present invention also offers a kind of preparation method of high dye-uptake polyester fiber FDY silk, by polyester slice through measuring, extruding, cool, oil, stretch, HEAT SETTING and winding, obtained high dye-uptake polyester fiber FDY silk;
The described temperature extruded is 280 ~ 290 DEG C;
The wind-warm syndrome of described cooling is 20 ~ 25 DEG C;
The speed of described winding is 4000 ~ 4600m/min;
Filament number is 0.3 ~ 1.0dtex;
The preparation process of described modified poly ester comprises:
(1) preparation of amino ethylene glycol fatty acid:
1) add in reactor by binary of fatty acids and methyl alcohol with the amount of 1:1.5 mol ratio, under the catalysis of the concentrated sulfuric 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 that dodecanedicarboxylic acid is to the one in dopentacontane dicarboxylic acids; Reaction equation is:
HOOC(CH
2)
nCOOH+CH
3OH→CH
3OOC(CH
2)
nCOOH
Wherein n=10 ~ 50.
2) by described binary of fatty acids mono-methyl, lead tetraacetate and lithium bromide in molar ratio 1:1:1 be dissolved in benzene, 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 including gas and producing, adds a certain amount of dilute sulfuric acid reaction 2 ~ 3 hours, then wash, purify and drying, obtain product bromo aliphatic acid; Reaction equation is:
3) by the ammoniacal liquor of bromo aliphatic acid and 15 ~ 25wt% in molar ratio 1:2 join in reactor, stir, at room temperature react, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is no more than 70 DEG C, until bubble-free produces, namely stop distillation, then carry out cooling and suction filtration, filter cake deionized water is washed till without till bromide ion, product vacuumize is obtained the amino aliphatic acid of product; Vacuum drying temperature can adopt 60 ~ 70 DEG C; Reaction equation is:
HOOC(CH
2)
nBr+NH
3→HOOC(CH
2)
nNH
2+NH
4Br；
4) by ethylene glycol and amino aliphatic acid in molar ratio for 1.1:2 stirs, and by 1 ~ 3% of amino fatty acid wt, to add concentration be the sulfuric acid of 40 ~ 50wt% is catalyst, carry out esterification, esterification reaction temperature is 160 ~ 220 DEG C, and esterification water quantity of distillate reaches more than 90% of theoretical value for esterification terminal; Product obtains amino ethylene glycol fatty acid through separating-purifying; Reaction equation is:
(2) preparation of modified poly ester, comprises esterification and polycondensation reaction:
Described esterification:
Adopt terephthalic acid (TPA) 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 esterification water quantity of distillate reaches more than 90% of theoretical value for esterification terminal;
Described polycondensation reaction:
Comprise polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction low vacuum stage, in esterification products, add catalyst and stabilizing agent, under the condition of negative pressure, start polycondensation reaction, this staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, temperature controls at 260 ~ 270 DEG C, and the reaction time is 30 ~ 50 minutes;
After the described polycondensation reaction low vacuum stage terminates, add amino ethylene glycol fatty acid, and stir, mixing time 15 ~ 20 minutes;
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction low vacuum stage, continues to vacuumize, and makes reaction pressure be down to absolute pressure and is less than 100Pa, and reaction temperature controls at 275 ~ 280 DEG C, 50 ~ 90 minutes reaction time;
Obtained modified poly ester.
The preparation method of a kind of high dye-uptake polyester fiber FDY silk as above, the mol ratio of described ethylene glycol and described terephthalic acid (TPA) is 1.2 ~ 2.0:1.
The preparation method of a kind of high dye-uptake polyester fiber FDY silk as above, described catalyst is selected from the one in antimonous oxide, antimony glycol and antimony acetate, and catalyst amount is 0.01% ~ 0.05% of described terephthalic acid (TPA) weight.
The preparation method of a kind of high dye-uptake polyester fiber FDY silk as above, described stabilizing agent is selected from the one in triphenyl phosphate, trimethyl phosphate and Trimethyl phosphite, and stabilizing agent dosage is 0.01% ~ 0.05% of described terephthalic acid (TPA) weight.
The preparation method of a kind of high dye-uptake polyester fiber FDY silk as above, is washed till without adopting liquor argenti nitratis ophthalmicus to detect till bromide ion with deionized water.
The preparation method of a kind of high dye-uptake polyester fiber FDY silk as above, the described concentrated sulfuric acid refers to that mass concentration is the sulfuric acid of 70 ~ 80%, and concentrated sulfuric acid addition is 1 ~ 3wt% of binary of fatty acids; Described a certain amount of dilute sulfuric acid refers to that mass concentration is the sulfuric acid of 40 ~ 50%, and dilute sulfuric acid addition is 1 ~ 3wt% of binary of fatty acids mono-methyl.
Polyester fiber is when dyeing, and the upper dye process of DISPERSE DYES to polyester fiber can be divided into the next stage:
1) DISPERSE DYES in dye liquor with the flowing of dye liquor gradually near fiber interface; 2) DISPERSE DYES is adsorbed by fiber surface rapidly near fiber interface; 3), after DISPERSE DYES is adsorbed to fiber surface, in fiber, produce a concentration difference or inside and outside dyestuff chemistry potential difference, dyestuff will spread to fibrous inside; 4) DISPERSE DYES diffusion velocity and fiber unformed area content, hole or free volume content relevant, therefore the dyeing speed of DISPERSE DYES is except dyestuff solubility in the solution, is also decided by that the degree of swelling of fiber during the outer and dyeing of the structure of fiber is relevant.
Polyster fibre is hydrophobic synthetic fiber, the active group resembling energy cellulose or protein fibre and dyestuff and occur to combine is lacked in terylene molecular structure, terylene molecules align must be tightr, only less space is there is in fiber, under the wet condition when dyeing, polyester fiber can not by acutely swelling and make space increase as cotton fiber, and dye molecule is difficult to see through fibrous inside.Therefore, the free volume between improving fiber molecule will contribute to the carrying out of dyeing.
The molecular chain structure of polyester is the linear macromolecule containing benzene ring structure, the functional group's marshalling on strand, and unbranched, the flexibility of macromolecular chain is poor.Simultaneously the good and rigidity of the regularity of polyester all comparatively greatly, and intermolecular active force is larger.Compared with other macromolecular materials, the strand generation slippage of polyester, rotation all comparatively difficulty, these characteristics hinder dyestuff and enter polyester inside, and thus dyeability is poor.
Amino ethylene glycol fatty acid is mainly with C-C, C-O key is main, there is certain molecular weight simultaneously, namely there is the strand of certain length, strand flexibility is larger, the amount of crimp of amino ethylene glycol fatty acid is larger compared with the linear macromolecule of benzene ring structure, simultaneously strong to the linear macromolecule of sensitivity comparatively containing benzene ring structure of temperature.When the temperature is changed, amino ethylene glycol fatty acid moves prior to the linear macromolecule containing benzene ring structure, and the free volume linear macromolecule be far longer than containing benzene ring structure that motion produces produces.
Added the free volume of polyester fiber by fatty acid ester to increase the diffusion of dyestuff, improve the dyeability of polyester fiber, make fiber obtain high dye-uptake.
Oxygen in fatty acid ester can form hydrogen bond, but oxygen is when centre position, and the factor hydrogen reduced in itself and polyester macromolecule chain such as curling due to space steric effect and fatty acid ester molecules forms the quantity of hydrogen bond; If amino is on α position, i.e. amino acids, because amino and carbonyl interact, be also unfavorable for that the hydrogen in amino and polyester macromolecule chain forms hydrogen bond; When the amino of amino fatty acid ester is in macromolecular end position, macromolecular curling little on its impact, add the formation that the amino in amino fatty acid ester and the hydrogen in polyester macromolecule chain form hydrogen bond, improve the active force between amino fatty acid ester and polyester macromolecule chain simultaneously, decrease slippage and the migration of amino fatty acid ester.
Add compatibility and the dispersion in the polyester of amino fatty acid ester and polyester, decrease migration to greatest extent.Polyester construction regularity, crystallinity are not destroyed simultaneously, maintain the premium properties of polyester.
Beneficial effect:
1. the high dye-uptake polyester fiber FDY silk of gained of the present invention, because amino ethylene glycol fatty acid is based on C-C, has certain molecular weight simultaneously, namely has the strand of certain length, and strand flexibility is comparatively large, and amino adds the compatibility with polyester.The fiber of gained and the compatibility of amino ethylene glycol fatty acid good, make FDY fiber obtain high dye-uptake.
2. due in amino ethylene glycol fatty acid molecule in the first amino existence, increase and hydrogen bond action between it and polyester macromolecule chain, add compatibility and the dispersion in the polyester of it and polyester, decrease migration to greatest extent.
3. the modified poly ester of gained of the present invention, because the content of amino ethylene glycol fatty acid is less, does not destroy polyester construction regularity, crystallinity, maintains the premium properties of polyester.
4. the amount of crimp of amino ethylene glycol fatty acid is larger compared with the linear macromolecule of benzene ring structure, simultaneously strong to the linear macromolecule of sensitivity comparatively containing benzene ring structure of temperature.When the temperature is changed, move prior to the linear macromolecule containing benzene ring structure, the free volume linear macromolecule be far longer than containing benzene ring structure that the motion of amino ethylene glycol fatty acid produces produces, and increases the diffusion of additive, improves the functional of polyester.
5. fatty acid ester adds the free volume of polyester fiber to increase the diffusion of dyestuff, improves the dyeability of polyester fiber.
Detailed description of the invention
Below in conjunction with detailed description of the invention, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
One of the present invention high dye-uptake polyester fiber FDY silk, material is modified poly ester, and described high dye-uptake polyester fiber FDY silk is under temperature is 90 ~ 130 DEG C of conditions, and the free volume space between fibrous inside strand increases 20 ~ 30v/v%; Described high dye-uptake polyester fiber FDY silk fracture strength >=3.8cN/dtex, extension at break CV value≤10.0%; Described modified poly ester is made up of polyester and amino ethylene glycol fatty acid, described amino ethylene glycol fatty acid is dispersed between the strand of described polyester, and have hydrogen bond action between the strand of described amino ethylene glycol fatty acid and described polyester, the relative position of the strand of described amino ethylene glycol fatty acid and described polyester is fixed;
The molecular structure of described amino ethylene glycol fatty acid is:
H
2N(CH
2)
nCOOCH
2CH
2OOC(CH
2)
nNH
2；
Wherein, n=10-50.
Described one high dye-uptake polyester fiber FDY silk, line density deviation ratio≤0.5% of described high dye-uptake polyester fiber FDY silk, fracture strength CV value≤5.0%, elongation at break is 33.0 ± 3.0%, yarn unevenness CV≤2.00%, boiling water shrinkage 7.5 ± 0.5%, oil content 0.90 ± 0.20%.
Described one high dye-uptake polyester fiber FDY silk, the percentage by weight that described amino ethylene glycol fatty acid accounts for described high dye-uptake polyester fiber FDY silk is 0.5 ~ 2.5%.
Colouring method: dyeing DISPERSE DYES is Disperse Red 3B, and disperse blue SE-2R disperses bright blue S-GL, and fiber dyes respectively in High Temperature High Pressure machine.Before dye, fiber non-ionic surface active agent was 60 DEG C of process 30 minutes.Dye dosage is 2.0% (o.w.f); Dispersant NNO1.2g/L, pH value is 5, and bath raio is 1:50, and 60 DEG C enter dye, are warming up to 90 DEG C, 100 DEG C, 110 DEG C, 120 DEG C each constant temperature dyeing 1h.
Dye uptake adopts raffinate colorimetric method to determine, draw appropriate dyeing stoste and dyeing residual liquid, add N, N-2 methylformamide (DMF) and distilled water, be the ratio of DMF in dye liquor to be measured and water be 70/30 (v/v), dye liquor absorbance adopts ultraviolet-visible spectrophotometer to measure, and calculates dye uptake with following formula.
In above formula, A0 and A1 is respectively the absorbance of dyeing stoste and dyeing residual liquid.
Embodiment 1
A preparation method for high dye-uptake polyester fiber FDY silk, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) add in reactor by dodecanedicarboxylic acid and methyl alcohol with the amount of 1:1.5 mol ratio, under the catalysis of the concentrated sulfuric acid, be heated to 80 DEG C, refuxing esterification, cooling, separating-purifying obtains dodecanedicarboxylic acid mono-methyl; The described concentrated sulfuric acid refers to that mass concentration is the sulfuric acid of 70%, and concentrated sulfuric acid addition is the 3wt% of dodecanedicarboxylic acid;
2) described dodecanedicarboxylic acid mono-methyl, lead tetraacetate and lithium bromide are dissolved in (mol ratio 1:1:1) in benzene, wherein dodecanedicarboxylic acid mono-methyl concentration is 0.05mol/L, under nitrogen atmosphere, 80 DEG C of reactions, backflow, when no longer including gas and producing, adds a certain amount of dilute sulfuric acid and reacts 2 hours, then wash, purify and drying, obtain product bromoundecane carboxylic acid; Described a certain amount of dilute sulfuric acid refers to that mass concentration is the sulfuric acid of 40%, and dilute sulfuric acid addition is the 3wt% of dodecanedicarboxylic acid mono-methyl;
3) by the ammoniacal liquor of bromoundecane carboxylic acid and 15wt% in molar ratio 1:2 join in reactor, stir, at room temperature react, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 60 DEG C, until bubble-free produces, namely stops distillation, then carry out cooling and suction filtration, filter cake deionized water is washed till without till bromide ion, adopts liquor argenti nitratis ophthalmicus to detect, product vacuumize is obtained product amino-undecanoic carboxylic acid;
4) by ethylene glycol and amino-undecanoic carboxylic acid in molar ratio for 1.1:2 stirs, and add by 1% of amino-undecanoic carboxylic acid weight the sulfuric acid that concentration is 40wt%, carry out esterification, esterification reaction temperature is 160 DEG C, and esterification water quantity of distillate reaches more than 90% of theoretical value for esterification terminal; Product obtains amino-undecanoic carboxylic acid glycol ester through separating-purifying;
(2) preparation of modified poly ester, comprises esterification and polycondensation reaction:
Described esterification:
Adopt mol ratio be the terephthalic acid (TPA) of 1:1.2 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 0.3MPa, and temperature is 250 DEG C, and esterification water quantity of distillate reaches more than 90% of theoretical value for esterification terminal;
Described polycondensation reaction:
Comprise polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction low vacuum stage, the antimonous oxide of 0.01% of terephthalic acid (TPA) weight and the triphenyl phosphate of terephthalic acid (TPA) weight 0.01% is added in esterification products, polycondensation reaction is started under the condition of negative pressure, this staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, temperature controls at 260 DEG C, and the reaction time is 50 minutes;
After the described polycondensation reaction low 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 low vacuum stage, continues to vacuumize, and makes reaction pressure be down to absolute pressure and is less than 100Pa, and reaction temperature controls at 275 DEG C, 90 minutes reaction time;
Obtained modified poly ester, viscosity average molecular weigh is 15000.
(3) preparation of high dye-uptake polyester fiber FDY silk
By modified poly ester through measuring, extruding, cool, oil, stretch, HEAT SETTING and winding, obtained high dye-uptake polyester fiber FDY silk;
The described temperature extruded is 280 DEG C;
The wind-warm syndrome of described cooling is 20 DEG C;
The speed of described winding is 4000m/min;
Filament number is 0.3dtex;
Gained height dye-uptake polyester fiber FDY silk is under temperature is 90 DEG C of conditions, free volume space between fibrous inside strand increases 20v/v%, line density deviation ratio is 1.5%, fracture strength is 3.8cN/dtex, fracture strength CV value is 5.0%, and elongation at break is 30%, extension at break CV value is 10.0%, yarn unevenness CV is 2.00%, boiling water shrinkage 7%, oil content 0.70%.Dyeed by high dye-uptake polyester fiber FDY silk, 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 | 89.4 | 90.5 | 91.4 |
| General fibre | 28.2 | 46.3 | 78.5 | 81.7 | 90.2 | |
| Disperse blue SE-2R | Modified fibre | 53.2 | 85.1 | 92.0 | 92.4 | 93.8 |
| General fibre | 12.3 | 35.2 | 73.4 | 88.9 | 91.3 | |
| Disperse bright blue S-GL | Modified fibre | 48.5 | 73.9 | 84.6 | 87.1 | 88.9 |
| General fibre | 11.8 | 36.3 | 70.9 | 75.6 | 82.6 |
Embodiment 2
A preparation method for high dye-uptake polyester fiber FDY silk, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) add in reactor by dopentacontane dicarboxylic acids and methyl alcohol with the amount of 1:1.5 mol ratio, under the catalysis of the concentrated sulfuric acid, be heated to 110 DEG C, refuxing esterification, cooling, separating-purifying obtains dopentacontane mono methyl dicarboxylate; The described concentrated sulfuric acid refers to that mass concentration is the sulfuric acid of 70%, and concentrated sulfuric acid addition is the 3wt% of dopentacontane dicarboxylic acids;
2) described dopentacontane mono methyl dicarboxylate, lead tetraacetate and lithium bromide are dissolved in (mol ratio 1:1:1) in benzene, wherein dopentacontane mono methyl dicarboxylate concentration is 0.07mol/L, under nitrogen atmosphere, 85 DEG C of reactions, backflow, when no longer including gas and producing, adds a certain amount of dilute sulfuric acid and reacts 3 hours, then wash, purify and drying, obtain product bromo henpentacontane carboxylic acid; Described a certain amount of dilute sulfuric acid refers to that mass concentration is the sulfuric acid of 40%, and dilute sulfuric acid addition is the 3wt% of dopentacontane mono methyl dicarboxylate;
3) by the ammoniacal liquor of bromo henpentacontane carboxylic acid and 25wt% in molar ratio 1:2 join in reactor, stir, at room temperature react, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 62 DEG C, until bubble-free produces, namely stops distillation, then carry out cooling and suction filtration, filter cake deionized water is washed till without till bromide ion, adopts liquor argenti nitratis ophthalmicus to detect, and product vacuumize is obtained the amino henpentacontane carboxylic acid of product;
4) by ethylene glycol and amino henpentacontane carboxylic acid in molar ratio for 1.1:2 stirs, and add by 2% of amino henpentacontane carboxylic acid weight the sulfuric acid that concentration is 45wt%, carry out esterification, esterification reaction temperature is 220 DEG C, and esterification water quantity of distillate reaches more than 90% of theoretical value for esterification terminal; Product obtains amino henpentacontane carboxylic acid glycol ester through separating-purifying;
(2) preparation of modified poly ester, comprises esterification and polycondensation reaction:
Described esterification:
Adopt mol ratio be the terephthalic acid (TPA) of 1:2.0 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 0.2MPa, and temperature is at 260 DEG C, and esterification water quantity of distillate reaches more than 90% of theoretical value for esterification terminal;
Described polycondensation reaction:
Comprise polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction low vacuum stage, the antimonous oxide of 0.05% of terephthalic acid (TPA) weight and the triphenyl phosphate of terephthalic acid (TPA) weight 0.05% is added in esterification products, polycondensation reaction is started under the condition of negative pressure, this staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, temperature controls at 270 DEG C, and the reaction time is 30 minutes;
After the described polycondensation reaction low vacuum stage terminates, add amino henpentacontane carboxylic acid glycol ester, and stir 20 minutes; Described amino henpentacontane carboxylic acid glycol ester addition is the percentage by weight of modified poly ester is 2.5%;
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction low vacuum stage, continues to vacuumize, and makes reaction pressure be down to absolute pressure and is less than 100Pa, and reaction temperature controls at 280 DEG C, 50 minutes reaction time;
Obtained modified poly ester, viscosity average molecular weigh is 30000.
(3) preparation of high dye-uptake polyester fiber FDY silk
By modified poly ester through measuring, extruding, cool, oil, stretch, HEAT SETTING and winding, obtained high dye-uptake polyester fiber FDY silk;
The described temperature extruded is 290 DEG C;
The wind-warm syndrome of described cooling is 25 DEG C;
The speed of described winding is 4600m/min;
Filament number is 1.0dtex;
Gained height dye-uptake polyester fiber FDY silk is under temperature is 130 DEG C of conditions, free volume space between fibrous inside strand increases 30v/v%, line density deviation ratio is 1.4%, fracture strength is 3.9cN/dtex, fracture strength CV value is 4.9%, and elongation at break is 31%, extension at break CV value is 9.5.0%, yarn unevenness CV is 1.90%, boiling water shrinkage 7.0%, oil content 0.90%.Dyeed by high dye-uptake polyester fiber FDY silk, 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 | 80.2 | 88.7 | 90.5 | 91.8 |
| General fibre | 28.2 | 46.3 | 78.5 | 81.7 | 90.2 | |
| Disperse blue SE-2R | Modified fibre | 52.2 | 85.3 | 92.1 | 94.4 | 93.8 |
| General fibre | 12.3 | 35.2 | 73.4 | 88.9 | 91.3 | |
| Disperse bright blue S-GL | Modified fibre | 48.5 | 74.9 | 84.6 | 86.1 | 88.1 |
| General fibre | 11.8 | 36.3 | 70.9 | 75.6 | 82.6 |
Embodiment 3
A preparation method for high dye-uptake polyester fiber FDY silk, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) add in reactor by pentacosane dicarboxylic acid and methyl alcohol with the amount of 1:1.5 mol ratio, under the catalysis of the concentrated sulfuric acid, be heated to 85 DEG C, refuxing esterification, cooling, separating-purifying obtains pentacosane dicarboxylic acid mono-methyl; The described concentrated sulfuric acid refers to that mass concentration is the sulfuric acid of 70%, and concentrated sulfuric acid addition is the 3wt% of pentacosane dicarboxylic acid;
2) described pentacosane dicarboxylic acid mono-methyl, lead tetraacetate and lithium bromide are dissolved in (mol ratio 1:1:1) in benzene, wherein pentacosane dicarboxylic acid mono-methyl concentration is 0.08mol/L, under nitrogen atmosphere, 90 DEG C of reactions, backflow, when no longer including gas and producing, adds a certain amount of dilute sulfuric acid and reacts 2.5 hours, then wash, purify and drying, obtain product bromotetradecane carboxylic acid; Described a certain amount of dilute sulfuric acid refers to that mass concentration is the sulfuric acid of 50%, and dilute sulfuric acid addition is the 3wt% of pentacosane dicarboxylic acid mono-methyl;
3) by the ammoniacal liquor of bromotetradecane carboxylic acid and 20wt% in molar ratio 1:2 join in reactor, stir, at room temperature react, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 60 DEG C, until bubble-free produces, namely stops distillation, then carry out cooling and suction filtration, filter cake deionized water is washed till without till bromide ion, adopts liquor argenti nitratis ophthalmicus to detect, and product vacuumize is obtained the amino tetradecane carboxylic acid of product;
4) by ethylene glycol and amino tetradecane carboxylic acid in molar ratio for 1.1:2 stirs, and add by 2% of the amino tetradecane carboxylic acid weight sulfuric acid that concentration is 50wt%, carry out esterification, esterification reaction temperature is 190 DEG C, and esterification water quantity of distillate reaches more than 90% of theoretical value for esterification terminal; Product obtains amino tetradecane carboxylic acid glycol ester through separating-purifying;
(2) preparation of modified poly ester, comprises esterification and polycondensation reaction:
Described esterification:
Adopt mol ratio be the terephthalic acid (TPA) of 1:1.6 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 0.3MPa, and temperature is at 255 DEG C, and esterification water quantity of distillate reaches more than 90% of theoretical value for esterification terminal;
Described polycondensation reaction:
Comprise polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction low vacuum stage, the antimonous oxide of 0.03% of terephthalic acid (TPA) weight and the triphenyl phosphate of terephthalic acid (TPA) weight 0.03% is added in esterification products, polycondensation reaction is started under the condition of negative pressure, this staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, temperature controls at 265 DEG C, and the reaction time is 40 minutes; After the described polycondensation reaction low vacuum stage terminates, add amino tetradecane carboxylic acid glycol ester, and stir 16 minutes; Described amino tetradecane carboxylic acid glycol ester addition is the percentage by weight of modified poly ester is 1.0%;
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction low vacuum stage, continues to vacuumize, and makes reaction pressure be down to absolute pressure and is less than 100Pa, and reaction temperature controls at 276 DEG C, 70 minutes reaction time;
Obtained modified poly ester, viscosity average molecular weigh is 22500.
(3) preparation of high dye-uptake polyester fiber FDY silk
By modified poly ester through measuring, extruding, cool, oil, stretch, HEAT SETTING and winding, obtained high dye-uptake polyester fiber FDY silk;
The described temperature extruded is 282 DEG C;
The wind-warm syndrome of described cooling is 21 DEG C;
The speed of described winding is 4100m/min;
Filament number is 0.4dtex;
Gained height dye-uptake polyester fiber FDY silk is under temperature is 100 DEG C of conditions, free volume space between fibrous inside strand increases 25v/v%, line density deviation ratio is 1.3%, fracture strength is 4.0cN/dtex, fracture strength CV value is 4.8%, and elongation at break is 33.0%, extension at break CV value is 9.6%, yarn unevenness CV is 1.80%, boiling water shrinkage 7.5%, oil content 0.8%.Dyeed by high dye-uptake polyester fiber FDY silk, its dye-uptake is as follows:
The dye uptake (%) of fiber
| Dyestuff | Temperature | 90℃ | 100℃ | 110℃ | 120℃ | 130℃ |
| Disperse Red 3B | Modified fibre | 48.6 | 80.3 | 89.8 | 90.2 | 91.4 |
| General fibre | 28.2 | 46.3 | 78.5 | 81.7 | 90.2 |
| Disperse blue SE-2R | Modified fibre | 52.5 | 85.2 | 92.3 | 93.5 | 93.8 |
| General fibre | 12.3 | 35.2 | 73.4 | 88.9 | 91.3 | |
| Disperse bright blue S-GL | Modified fibre | 48.5 | 73.3 | 85.6 | 87.1 | 88.7 |
| General fibre | 11.8 | 36.3 | 70.9 | 75.6 | 82.6 |
Embodiment 4
A preparation method for high dye-uptake polyester fiber FDY silk, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) add in reactor by eicosane dicarboxylic acids and methyl alcohol with the amount of 1:1.5 mol ratio, under the catalysis of the concentrated sulfuric acid, be heated to 85 DEG C, refuxing esterification, cooling, separating-purifying obtains eicosane mono methyl dicarboxylate; The described concentrated sulfuric acid refers to that mass concentration is the sulfuric acid of 70%, and concentrated sulfuric acid addition is the 3wt% of eicosane dicarboxylic acids;
2) described eicosane mono methyl dicarboxylate, lead tetraacetate and lithium bromide are dissolved in (mol ratio 1:1:1) in benzene, wherein eicosane mono methyl dicarboxylate concentration is 0.09mol/L, under nitrogen atmosphere, 80 DEG C of reactions, backflow, when no longer including gas and producing, adds a certain amount of dilute sulfuric acid and reacts 2.1 hours, then wash, purify and drying, obtain product bromo nonadecane carboxylic acid; Described a certain amount of dilute sulfuric acid refers to that mass concentration is the sulfuric acid of 43%, and dilute sulfuric acid addition is the 2wt% of eicosane mono methyl dicarboxylate;
3) by the ammoniacal liquor of bromo nonadecane carboxylic acid and 16wt% in molar ratio 1:2 join in reactor, stir, at room temperature react, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 69 DEG C, until bubble-free produces, namely stops distillation, then carry out cooling and suction filtration, filter cake deionized water is washed till without till bromide ion, adopts liquor argenti nitratis ophthalmicus to detect, and product vacuumize is obtained the amino nonadecane carboxylic acid of product;
4) by ethylene glycol and amino nonadecane carboxylic acid in molar ratio for 1.1:2 stirs, and add by 2% of amino nonadecane carboxylic acid weight the sulfuric acid that concentration is 42wt%, carry out esterification, esterification reaction temperature is 160 DEG C, and esterification water quantity of distillate reaches more than 90% of theoretical value for esterification terminal; Product obtains amino nonadecane carboxylic acid glycol ester through separating-purifying;
(2) preparation of modified poly ester, comprises esterification and polycondensation reaction:
Described esterification:
Adopt mol ratio be the terephthalic acid (TPA) of 1:1.2 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 0.15MPa, and temperature is at 251 DEG C, and esterification water quantity of distillate reaches more than 90% of theoretical value for esterification terminal;
Described polycondensation reaction:
Comprise polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction low vacuum stage, the antimonous oxide of 0.02% of terephthalic acid (TPA) weight and the triphenyl phosphate of terephthalic acid (TPA) weight 0.02% is added in esterification products, polycondensation reaction is started under the condition of negative pressure, this staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, temperature controls at 262 DEG C, and the reaction time is 33 minutes;
After the described polycondensation reaction low vacuum stage terminates, add amino nonadecane carboxylic acid glycol ester, and stir 17 minutes; Described amino nonadecane carboxylic acid glycol ester addition is the percentage by weight of modified poly ester is 1.5%;
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction low vacuum stage, continues to vacuumize, and makes reaction pressure be down to absolute pressure and is less than 100Pa, and reaction temperature controls at 277 DEG C, 55 minutes reaction time;
Obtained modified poly ester, viscosity average molecular weigh is 16000.
(3) preparation of high dye-uptake polyester fiber FDY silk
By modified poly ester through measuring, extruding, cool, oil, stretch, HEAT SETTING and winding, obtained high dye-uptake polyester fiber FDY silk;
The described temperature extruded is 284 DEG C;
The wind-warm syndrome of described cooling is 22 DEG C;
The speed of described winding is 4200m/min;
Filament number is 0.5dtex;
Gained height dye-uptake polyester fiber FDY silk is under temperature is 90 DEG C of conditions, free volume space between fibrous inside strand increases 20v/v%, line density deviation ratio is 1.3%, fracture strength is 4.0cN/dtex, fracture strength CV value is 4.7%, and elongation at break is 31.0%, extension at break CV value is 10.0%, yarn unevenness CV is 1.7%, boiling water shrinkage 7.2%, oil content 0.8%.Dyeed by high dye-uptake polyester fiber FDY silk, 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 | 81.2 | 89.2 | 90.3 | 91.4 |
| General fibre | 28.2 | 46.3 | 78.5 | 81.7 | 90.2 | |
| Disperse blue SE-2R | Modified fibre | 56.5 | 84.1 | 92.1 | 93.4 | 93.8 |
| General fibre | 12.3 | 35.2 | 73.4 | 88.9 | 91.3 | |
| Disperse bright blue S-GL | Modified fibre | 48.5 | 73.4 | 84.6 | 87.3 | 88.8 |
| General fibre | 11.8 | 36.3 | 70.9 | 75.6 | 82.6 |
Embodiment 5
A preparation method for high dye-uptake polyester fiber FDY silk, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) add in reactor by melissane dicarboxylic acids and methyl alcohol with the amount of 1:1.5 mol ratio, under the catalysis of the concentrated sulfuric acid, be heated to 90 DEG C, refuxing esterification, cooling, separating-purifying obtains melissane mono methyl dicarboxylate; The described concentrated sulfuric acid refers to that mass concentration is the sulfuric acid of 70%, and concentrated sulfuric acid addition is the 3wt% of melissane dicarboxylic acids;
2) described melissane mono methyl dicarboxylate, lead tetraacetate and lithium bromide are dissolved in (mol ratio 1:1:1) in benzene, wherein melissane mono methyl dicarboxylate concentration be 0.10mol/L under nitrogen atmosphere, 85 DEG C of reactions, backflow, when no longer including gas and producing, add a certain amount of dilute sulfuric acid and react 2.3 hours, then wash, purify and drying, obtain product bromo nonacosane carboxylic acid; Described a certain amount of dilute sulfuric acid refers to that mass concentration is the sulfuric acid of 40%, and dilute sulfuric acid addition is the 3wt% of melissane mono methyl dicarboxylate;
3) by the ammoniacal liquor of bromo nonacosane carboxylic acid and 18wt% in molar ratio 1:2 join in reactor, stir, at room temperature react, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 67 DEG C, until bubble-free produces, namely stops distillation, then carry out cooling and suction filtration, filter cake deionized water is washed till without till bromide ion, adopts liquor argenti nitratis ophthalmicus to detect, and product vacuumize is obtained the amino nonacosane carboxylic acid of product;
4) by ethylene glycol and amino nonacosane carboxylic acid in molar ratio for 1.1:2 stirs, and add by 2% of amino nonacosane carboxylic acid weight the sulfuric acid that concentration is 48wt%, carry out esterification, esterification reaction temperature is 170 DEG C, and esterification water quantity of distillate reaches more than 90% of theoretical value for esterification terminal; Product obtains amino nonacosane carboxylic acid glycol ester through separating-purifying;
(2) preparation of modified poly ester, comprises esterification and polycondensation reaction:
Described esterification:
Adopt mol ratio be the terephthalic acid (TPA) of 1:1.5 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 0.3MPa, and temperature is at 254 DEG C, and esterification water quantity of distillate reaches more than 90% of theoretical value for esterification terminal;
Described polycondensation reaction:
Comprise polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction low vacuum stage, the antimony glycol of 0.01% of terephthalic acid (TPA) weight and the trimethyl phosphate of terephthalic acid (TPA) weight 0.03% is added in esterification products, polycondensation reaction is started under the condition of negative pressure, this staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, temperature controls at 266 DEG C, and the reaction time is 39 minutes;
After the described polycondensation reaction low vacuum stage terminates, add amino nonacosane carboxylic acid glycol ester, and stir 18 minutes; Described amino nonacosane carboxylic acid glycol ester addition is the percentage by weight of modified poly ester is 2.5%;
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction low vacuum stage, continues to vacuumize, and makes reaction pressure be down to absolute pressure and is less than 100Pa, and reaction temperature controls at 278 DEG C, 60 minutes reaction time;
Obtained modified poly ester, viscosity average molecular weigh is 22000.
(3) preparation of high dye-uptake polyester fiber FDY silk
By modified poly ester through measuring, extruding, cool, oil, stretch, HEAT SETTING and winding, obtained high dye-uptake polyester fiber FDY silk;
The described temperature extruded is 280 DEG C;
The wind-warm syndrome of described cooling is 23 DEG C;
The speed of described winding is 4300m/min;
Filament number is 0.6dtex;
Gained height dye-uptake polyester fiber FDY silk is under temperature is 100 DEG C of conditions, free volume space between fibrous inside strand increases 25v/v%, line density deviation ratio is 1.2%, fracture strength is 4.1cN/dtex, fracture strength CV value is 5.0%, and elongation at break is 32.0%, extension at break CV value is 9.5%, yarn unevenness CV is 1.80%, boiling water shrinkage 7.3%, oil content 1.1%.Dyeed by high dye-uptake polyester fiber FDY silk, its dye-uptake is as follows:
The dye uptake (%) of fiber
| Dyestuff | Temperature | 90℃ | 100℃ | 110℃ | 120℃ | 130℃ |
| Disperse Red 3B | Modified fibre | 48.2 | 80.3 | 88.7 | 90.9 | 91.4 |
| General fibre | 28.2 | 46.3 | 78.5 | 81.7 | 90.2 | |
| Disperse blue SE-2R | Modified fibre | 52.3 | 85.1 | 92.0 | 93.2 | 93.8 |
| General fibre | 12.3 | 35.2 | 73.4 | 88.9 | 91.3 | |
| Disperse bright blue S-GL | Modified fibre | 48.3 | 73.8 | 84.6 | 87.9 | 88.5 |
| General fibre | 11.8 | 36.3 | 70.9 | 75.6 | 82.6 |
Embodiment 6
A preparation method for high dye-uptake polyester fiber FDY silk, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) add in reactor by pentatriacontane dicarboxylic acids and methyl alcohol with the amount of 1:1.5 mol ratio, under the catalysis of the concentrated sulfuric acid, be heated to 95 DEG C, refuxing esterification, cooling, separating-purifying obtains pentatriacontane mono methyl dicarboxylate; The described concentrated sulfuric acid refers to that mass concentration is the sulfuric acid of 70%, and concentrated sulfuric acid addition is the 2wt% of pentatriacontane dicarboxylic acids;
2) described pentatriacontane mono methyl dicarboxylate, lead tetraacetate and lithium bromide are dissolved in (mol ratio 1:1:1) in benzene, wherein pentatriacontane mono methyl dicarboxylate concentration be 0.09mol/L under nitrogen atmosphere, 90 DEG C of reactions, backflow, when no longer including gas and producing, add a certain amount of dilute sulfuric acid and react 2.6 hours, then wash, purify and drying, obtain product bromo tetratriacontane carboxylic acid; Described a certain amount of dilute sulfuric acid refers to that mass concentration is the sulfuric acid of 45%, and dilute sulfuric acid addition is the 1wt% of pentatriacontane mono methyl dicarboxylate
3) by the ammoniacal liquor of bromo tetratriacontane carboxylic acid and 20wt% in molar ratio 1:2 join in reactor, stir, at room temperature react, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 69 DEG C, until bubble-free produces, namely stops distillation, then carry out cooling and suction filtration, filter cake deionized water is washed till without till bromide ion, adopts liquor argenti nitratis ophthalmicus to detect, and product vacuumize is obtained the amino tetratriacontane carboxylic acid of product;
4) by ethylene glycol and amino tetratriacontane carboxylic acid in molar ratio for 1.1:2 stirs, and add by 1% of amino tetratriacontane carboxylic acid weight the sulfuric acid that concentration is 50wt%, carry out esterification, esterification reaction temperature is 180 DEG C, and esterification water quantity of distillate reaches more than 90% of theoretical value for esterification terminal; Product obtains amino tetratriacontane carboxylic acid glycol ester through separating-purifying;
(2) preparation of modified poly ester, comprises esterification and polycondensation reaction:
Described esterification:
Adopt mol ratio be the terephthalic acid (TPA) of 1:1.6 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 0.4MPa, and temperature is at 256 DEG C, and esterification water quantity of distillate reaches more than 90% of theoretical value for esterification terminal;
Described polycondensation reaction:
Comprise polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction low vacuum stage, the antimony acetate of 0.04% of terephthalic acid (TPA) weight and the Trimethyl phosphite of terephthalic acid (TPA) weight 0.02% is added in esterification products, polycondensation reaction is started under the condition of negative pressure, this staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, temperature controls at 267 DEG C, and the reaction time is 40 minutes; After the described polycondensation reaction low vacuum stage terminates, add amino tetratriacontane carboxylic acid glycol ester, and stir 18 minutes; Described amino tetratriacontane carboxylic acid glycol ester addition is the percentage by weight of modified poly ester is 2.0%;
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction low vacuum stage, continues to vacuumize, and makes reaction pressure be down to absolute pressure and is less than 100Pa, and reaction temperature controls at 275 DEG C, 70 minutes reaction time;
Obtained modified poly ester, viscosity average molecular weigh is 24000.
(3) preparation of high dye-uptake polyester fiber FDY silk
By modified poly ester through measuring, extruding, cool, oil, stretch, HEAT SETTING and winding, obtained high dye-uptake polyester fiber FDY silk;
The described temperature extruded is 288 DEG C;
The wind-warm syndrome of described cooling is 24 DEG C;
The speed of described winding is 4400m/min;
Filament number is 0.7dtex
Gained height dye-uptake polyester fiber FDY silk is under temperature is 110 DEG C of conditions, free volume space between fibrous inside strand increases 30v/v%, line density deviation ratio is 1.5%, fracture strength is 3.9cN/dtex, fracture strength CV value is 5.0%, and elongation at break is 36%, extension at break CV value is 10.0%, yarn unevenness CV is 1.80%, boiling water shrinkage 8.0%, oil content 1.0%.Dyeed by high dye-uptake polyester fiber FDY silk, 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 | 80.1 | 89.7 | 90.5 | 91.7 |
| General fibre | 28.2 | 46.3 | 78.5 | 81.7 | 90.2 | |
| Disperse blue SE-2R | Modified fibre | 52.9 | 85.1 | 92.5 | 94.4 | 93.4 |
| General fibre | 12.3 | 35.2 | 73.4 | 88.9 | 91.3 | |
| Disperse bright blue S-GL | Modified fibre | 48.5 | 73.4 | 84.6 | 87.7 | 87.7 |
| General fibre | 11.8 | 36.3 | 70.9 | 75.6 | 82.6 |
Embodiment 7
A preparation method for high dye-uptake polyester fiber FDY silk, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) add in reactor by tetracontane dicarboxylic acids and methyl alcohol with the amount of 1:1.5 mol ratio, under the catalysis of the concentrated sulfuric acid, be heated to 100 DEG C, refuxing esterification, cooling, separating-purifying obtains tetracontane mono methyl dicarboxylate; The described concentrated sulfuric acid refers to that mass concentration is the sulfuric acid of 70%, and concentrated sulfuric acid addition is the 3wt% of tetracontane dicarboxylic acids;
2) described tetracontane mono methyl dicarboxylate, lead tetraacetate and lithium bromide are dissolved in (mol ratio 1:1:1) in benzene, wherein tetracontane mono methyl dicarboxylate concentration be 0.06mol/L under nitrogen atmosphere, 80 DEG C of reactions, backflow, when no longer including gas and producing, add a certain amount of dilute sulfuric acid and react 2.7 hours, then wash, purify and drying, obtain product bromo nonatriacontane carboxylic acid; Described a certain amount of dilute sulfuric acid refers to that mass concentration is the sulfuric acid of 48%, and dilute sulfuric acid addition is the 2wt% of tetracontane mono methyl dicarboxylate;
3) by the ammoniacal liquor of bromo nonatriacontane carboxylic acid and 22wt% in molar ratio 1:2 join in reactor, stir, at room temperature react, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is 60 DEG C, until bubble-free produces, namely stops distillation, then carry out cooling and suction filtration, filter cake deionized water is washed till without till bromide ion, adopts liquor argenti nitratis ophthalmicus to detect, and product vacuumize is obtained the amino nonatriacontane carboxylic acid of product;
4) by ethylene glycol and amino nonatriacontane carboxylic acid in molar ratio for 1.1:2 stirs, and add by 2% of amino nonatriacontane carboxylic acid weight the sulfuric acid that concentration is 46wt%, carry out esterification, esterification reaction temperature is 190 DEG C, and esterification water quantity of distillate reaches more than 90% of theoretical value for esterification terminal; Product obtains amino nonatriacontane carboxylic acid glycol ester through separating-purifying;
(2) preparation of modified poly ester, comprises esterification and polycondensation reaction:
Described esterification:
Adopt mol ratio be the terephthalic acid (TPA) of 1:1.8 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 0.2MPa, and temperature is at 258 DEG C, and esterification water quantity of distillate reaches more than 90% of theoretical value for esterification terminal;
Described polycondensation reaction:
Comprise polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction low vacuum stage, the antimony acetate of 0.05% of terephthalic acid (TPA) weight and the trimethyl phosphate of terephthalic acid (TPA) weight 0.03% is added in esterification products, polycondensation reaction is started under the condition of negative pressure, this staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, temperature controls at 268 DEG C, and the reaction time is 45 minutes;
After the described polycondensation reaction low vacuum stage terminates, add amino nonatriacontane carboxylic acid glycol ester, and stir 16 minutes; Described amino nonatriacontane carboxylic acid glycol ester addition is the percentage by weight of modified poly ester is 1.5%;
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction low vacuum stage, continues to vacuumize, and makes reaction pressure be down to absolute pressure and is less than 100Pa, and reaction temperature controls at 275 DEG C, 75 minutes reaction time;
Obtained modified poly ester, viscosity average molecular weigh is 25000.
(3) preparation of high dye-uptake polyester fiber FDY silk
By modified poly ester through measuring, extruding, cool, oil, stretch, HEAT SETTING and winding, obtained high dye-uptake polyester fiber FDY silk;
The described temperature extruded is 290 DEG C;
The wind-warm syndrome of described cooling is 24 DEG C;
The speed of described winding is 4500m/min;
Filament number is 0.8dtex;
Gained height dye-uptake polyester fiber FDY silk is under temperature is 120 DEG C of conditions, free volume space between fibrous inside strand increases 30v/v%, line density deviation ratio is 1.5%, fracture strength is 4.0cN/dtex, fracture strength CV value is 4.8%, and elongation at break is 36.0%, extension at break CV value is 9.6%, yarn unevenness CV is 2.00%, boiling water shrinkage 7.7%, oil content 0.90%.Dyeed by high dye-uptake polyester fiber FDY silk, its dye-uptake is as follows:
The dye uptake (%) of fiber
| Dyestuff | Temperature | 90℃ | 100℃ | 110℃ | 120℃ | 130℃ |
| Disperse Red 3B | Modified fibre | 49.3 | 80.1 | 89.7 | 91.5 | 91.4 |
| General fibre | 28.2 | 46.3 | 78.5 | 81.7 | 90.2 | |
| Disperse blue SE-2R | Modified fibre | 52.5 | 85.1 | 92.3 | 93.4 | 93.8 |
| 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 | 88.1 | 88.7 |
| General fibre | 11.8 | 36.3 | 70.9 | 75.6 | 82.6 |
Embodiment 8
A preparation method for high dye-uptake polyester fiber FDY silk, comprises the following steps:
(1) preparation of amino ethylene glycol fatty acid:
1) add in reactor by pentatetracontane dicarboxylic acids and methyl alcohol with the amount of 1:1.5 mol ratio, under the catalysis of the concentrated sulfuric acid, be heated to 110 DEG C, refuxing esterification, cooling, separating-purifying obtains pentatetracontane mono methyl dicarboxylate; The described concentrated sulfuric acid refers to that mass concentration is the sulfuric acid of 70%, and concentrated sulfuric acid addition is the 2wt% of pentatetracontane dicarboxylic acids;
2) described pentatetracontane mono methyl dicarboxylate, lead tetraacetate and lithium bromide are dissolved in (mol ratio 1:1:1) in benzene, wherein pentatetracontane mono methyl dicarboxylate concentration is 0.07mol/L, under nitrogen atmosphere, 88 DEG C of reactions, backflow, when no longer including gas and producing, adds a certain amount of dilute sulfuric acid and reacts 2.3 hours, then wash, purify and drying, obtain product bromo tetratetracontane carboxylic acid; Described a certain amount of dilute sulfuric acid refers to that mass concentration is the sulfuric acid of 45%, and dilute sulfuric acid addition is the 2wt% of pentatetracontane mono methyl dicarboxylate;
3) by the ammoniacal liquor of bromo tetratetracontane carboxylic acid and 25wt% in molar ratio 1:2 join in reactor, stir, at room temperature react, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is no more than 70 DEG C, until bubble-free produces, namely stops distillation, then carry out cooling and suction filtration, filter cake deionized water is washed till without till bromide ion, adopts liquor argenti nitratis ophthalmicus to detect, and product vacuumize is obtained the amino tetratetracontane carboxylic acid of product;
4) by ethylene glycol and amino tetratetracontane carboxylic acid in molar ratio for 1.1:2 stirs, and add by 1% of amino tetratetracontane carboxylic acid weight the sulfuric acid that concentration is 50wt%, carry out esterification, esterification reaction temperature is 210 DEG C, and esterification water quantity of distillate reaches more than 90% of theoretical value for esterification terminal; Product obtains amino tetratetracontane carboxylic acid glycol ester through separating-purifying;
(2) preparation of modified poly ester, comprises esterification and polycondensation reaction:
Described esterification:
Adopt mol ratio be the terephthalic acid (TPA) of 1:2.0 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 0.3MPa, and temperature is at 260 DEG C, and esterification water quantity of distillate reaches more than 90% of theoretical value for esterification terminal;
Described polycondensation reaction:
Comprise polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction low vacuum stage, the antimony glycol of 0.02% of terephthalic acid (TPA) weight and the trimethyl phosphate of terephthalic acid (TPA) weight 0.05% is added in esterification products, polycondensation reaction is started under the condition of negative pressure, this staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, temperature controls at 270 DEG C, and the reaction time is 50 minutes;
After the described polycondensation reaction low vacuum stage terminates, add amino tetratetracontane carboxylic acid glycol ester, and stir 20 minutes; Described amino tetratetracontane carboxylic acid glycol ester addition is the percentage by weight of modified poly ester is 2.0%;
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction low vacuum stage, continues to vacuumize, and makes reaction pressure be down to absolute pressure and is less than 100Pa, and reaction temperature controls at 280 DEG C, 85 minutes reaction time;
Obtained modified poly ester, viscosity average molecular weigh is 30000.
(3) preparation of high dye-uptake polyester fiber FDY silk
By modified poly ester through measuring, extruding, cool, oil, stretch, HEAT SETTING and winding, obtained high dye-uptake polyester fiber FDY silk;
The described temperature extruded is 285 DEG C;
The wind-warm syndrome of described cooling is 23 DEG C;
The speed of described winding is 4500m/min;
Filament number is 1.0dtex;
Gained height dye-uptake polyester fiber FDY silk is under temperature is 130 DEG C of conditions, free volume space between fibrous inside strand increases 30v/v%, line density deviation ratio is 1.2%, fracture strength is 4.0cN/dtex, fracture strength CV value is 5.0%, and elongation at break is 35.0%, extension at break CV value is 10.0%, yarn unevenness CV is 2.00%, boiling water shrinkage 7.8%, oil content 0.8%.Dyeed by high dye-uptake polyester fiber FDY silk, 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 | 81.1 | 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 | 91.4 | 93.4 | 93.1 |
| General fibre | 12.3 | 35.2 | 73.4 | 88.9 | 91.3 | |
| Disperse bright blue S-GL | Modified fibre | 48.9 | 73.8 | 84.6 | 86.1 | 88.7 |
| General fibre | 11.8 | 36.3 | 70.9 | 75.6 | 82.6 |
Claims (10)
1. one kind high dye-uptake polyester fiber FDY silk, it is characterized in that: the material of described high dye-uptake polyester fiber FDY silk is modified poly ester, described high dye-uptake polyester fiber FDY silk is under temperature is 90 ~ 130 DEG C of conditions, and the free volume space between fibrous inside strand increases 20 ~ 30v/v%; Fracture strength >=the 3.8cN/dtex of described high dye-uptake polyester fiber FDY silk, elongation at break is 33.0 ± 3.0%; Described modified poly ester is made up of polyester and amino ethylene glycol fatty acid, described amino ethylene glycol fatty acid is dispersed between the strand of described polyester, and have hydrogen bond action between the strand of described amino ethylene glycol fatty acid and described polyester, the relative position of the strand of described amino ethylene glycol fatty acid and described polyester is fixed;
The molecular structure of described amino ethylene glycol fatty acid is:
H
2N(CH
2)
nCOOCH
2CH
2OOC(CH
2)
nNH
2；
Wherein, n=10-50.
2. one according to claim 1 high dye-uptake polyester fiber FDY silk, it is characterized in that, line density deviation ratio≤0.5% of described high dye-uptake polyester fiber FDY silk, fracture strength CV value≤5.0%, extension at break CV value≤10.0%, yarn unevenness CV≤2.00%, boiling water shrinkage 7.5 ± 0.5%, oil content 0.90 ± 0.20%.
3. one according to claim 1 high dye-uptake polyester fiber FDY silk, is characterized in that, the percentage by weight that described amino ethylene glycol fatty acid accounts for described high dye-uptake polyester fiber FDY silk is 0.5 ~ 2.5%.
4. the preparation method of a kind of high dye-uptake polyester fiber FDY silk as claimed in claim 1, to is characterized in that modified poly ester through measuring, extruding, cool, oil, stretch, HEAT SETTING and winding, obtained high dye-uptake polyester fiber FDY silk;
The described temperature extruded is 280 ~ 290 DEG C;
The wind-warm syndrome of described cooling is 20 ~ 25 DEG C;
The speed of described winding is 4000 ~ 4600m/min;
Filament number is 0.3 ~ 1.0dtex;
The preparation process of described modified poly ester comprises:
(1) preparation of amino ethylene glycol fatty acid:
1) add in reactor by binary of fatty acids and methyl alcohol with the amount of 1:1.5 mol ratio, under the catalysis of the concentrated sulfuric 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 that dodecanedicarboxylic acid is to the one in dopentacontane dicarboxylic acids;
2) by described binary of fatty acids mono-methyl, lead tetraacetate and lithium bromide in molar ratio 1:1:1 be dissolved in benzene, wherein the concentration of binary of fatty acids mono-methyl is 0.05 ~ 0.1mol/L, under nitrogen atmosphere, 100 DEG C of reactions, backflow, when no longer including gas and producing, adds a certain amount of dilute sulfuric acid reaction 2 ~ 3 hours, then wash, purify and drying, obtain product bromo aliphatic acid;
3) by the ammoniacal liquor of bromo aliphatic acid and 15 ~ 25wt% in molar ratio 1:2 join in reactor, stir, at room temperature react, then product is added thermal distillation, and absorb ammonia with cold water, the temperature adding thermal distillation is no more than 70 DEG C, until bubble-free produces, namely stop distillation, then carry out cooling and suction filtration, filter cake deionized water is washed till without till bromide ion, product vacuumize is obtained the amino aliphatic acid of product;
4) by ethylene glycol and amino aliphatic acid in molar ratio for 1.1:2 stirs, and add by 1 ~ 3% of amino fatty acid wt the sulfuric acid that concentration is 40 ~ 50wt%, carry out esterification, esterification reaction temperature is 160 ~ 220 DEG C, and esterification water quantity of distillate reaches more than 90% of theoretical value for esterification terminal; Product obtains amino ethylene glycol fatty acid through separating-purifying;
(2) preparation of modified poly ester, comprises esterification and polycondensation reaction:
Described esterification:
Adopt terephthalic acid (TPA) 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 esterification water quantity of distillate reaches more than 90% of theoretical value for esterification terminal;
Described polycondensation reaction:
Comprise polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction low vacuum stage, in esterification products, add catalyst and stabilizing agent, under the condition of negative pressure, start polycondensation reaction, this staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, temperature controls at 260 ~ 270 DEG C, and the reaction time is 30 ~ 50 minutes;
After the described polycondensation reaction low vacuum stage terminates, add amino ethylene glycol fatty acid, and stir;
Described polycondensation reaction high vacuum stage of Fig, after the described polycondensation reaction low vacuum stage, continues to vacuumize, and makes reaction pressure be down to absolute pressure and is less than 100Pa, and reaction temperature controls at 275 ~ 280 DEG C, 50 ~ 90 minutes reaction time;
Obtained modified poly ester.
5. the preparation method of a kind of high dye-uptake polyester fiber FDY silk according to claim 4, it is characterized in that, the mol ratio of described ethylene glycol and described terephthalic acid (TPA) is 1.2 ~ 2.0:1.
6. the preparation method of a kind of high dye-uptake polyester fiber FDY silk according to claim 4, it is characterized in that, described catalyst is selected from the one in antimonous oxide, antimony glycol and antimony acetate, and catalyst amount is 0.01% ~ 0.05% of described terephthalic acid (TPA) weight.
7. the preparation method of a kind of high dye-uptake polyester fiber FDY silk according to claim 4, it is characterized in that, described stabilizing agent is selected from the one in triphenyl phosphate, trimethyl phosphate and Trimethyl phosphite, and stabilizing agent dosage is 0.01% ~ 0.05% of described terephthalic acid (TPA) weight.
8. the preparation method of a kind of high dye-uptake polyester fiber FDY silk according to claim 4, it is characterized in that, add the stirring after amino ethylene glycol fatty acid, the time is 15 ~ 20 minutes.
9. the preparation method of a kind of high dye-uptake polyester fiber FDY silk according to claim 4, is characterized in that, being washed till without adopting liquor argenti nitratis ophthalmicus to detect till bromide ion with deionized water.
10. the preparation method of a kind of high dye-uptake polyester fiber FDY silk according to claim 4, it is characterized in that, the described concentrated sulfuric acid refers to that mass concentration is the sulfuric acid of 70 ~ 80%, and concentrated sulfuric acid addition is 1 ~ 3wt% of binary of fatty acids; Described a certain amount of dilute sulfuric acid refers to that mass concentration is the sulfuric acid of 40 ~ 50%, and dilute sulfuric acid addition is 1 ~ 3wt% of binary of fatty acids mono-methyl.
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