CN105648566A - Low-color-difference polyester FDY (Fully Drawn Yarn) and preparation method thereof - Google Patents
Low-color-difference polyester FDY (Fully Drawn Yarn) and preparation method thereof Download PDFInfo
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- CN105648566A CN105648566A CN201511019122.6A CN201511019122A CN105648566A CN 105648566 A CN105648566 A CN 105648566A CN 201511019122 A CN201511019122 A CN 201511019122A CN 105648566 A CN105648566 A CN 105648566A
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
- D01F6/62—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyesters
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/83—Alkali metals, alkaline earth metals, beryllium, magnesium, copper, silver, gold, zinc, cadmium, mercury, manganese, or compounds thereof
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/78—Preparation processes
- C08G63/82—Preparation processes characterised by the catalyst used
- C08G63/85—Germanium, tin, lead, arsenic, antimony, bismuth, titanium, zirconium, hafnium, vanadium, niobium, tantalum, or compounds thereof
- C08G63/86—Germanium, antimony, or compounds thereof
- C08G63/866—Antimony or compounds thereof
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
- D01D10/02—Heat treatment
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/08—Melt spinning methods
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/12—Stretch-spinning methods
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Abstract
The invention relates to low-color-difference polyester FDY (Fully Drawn Yarn) and a preparation method thereof. The low-color-difference polyester FDY is prepared through carrying out spinning on polyester and has the rupture strength not lower than 3.8cN/dtex, the breaking elongation of 33.0+/-3.0% and the color difference [delta]E smaller than 0.200. According to the low-color-difference polyester FDY and the preparation method thereof, ethylene glycol magnesium is relatively mild, has a very small thermal degradation coefficient and causes less side reactions during reaction, so that the production of oligomers during processing is reduced; the mass percent of the oligomers is lower than 0.5%, and the mass percent of diethylene glycol is lower than 0.5%. The oligomers are reduced during polymerization and are further reduced during washing, so that during the dyeing and postprocessing thermosetting of polyester fibers, the amount of the oligomers migrating to the outside of the fibers from the inside is reduced, the occurrence of color spots and streaks is reduced, and the level dyeability and rubbing fastness of the fibers are guaranteed.
Description
Technical field
The invention belongs to polyester preparing technical field, relate to a kind of low aberration polyester FDY silk and preparation method thereof, particularly a kind of polycondensation catalyst adopt the mixture of ethylene glycol magnesium and antimony glycol and polyester slice through water with dissolve and wash away agent at 120��130 DEG C, low aberration polyester FDY silk of brew, washing and preparation method thereof when 0.2��0.3MPa.
Background technology
Polyethylene terephthalate (PET) is the polymer of a kind of function admirable, PET is high with its modulus, intensity is high, well-pressed, conformality health good, pure, barrier property are good, it is widely used in the fields such as fiber, bottle packaging, thin film and sheet material, yield cumulative year after year, position in industry is obviously improved.
PET belongs to symmetric straight chain macromolecular, and strand does not contain side-chain radical, and regularity is very good, and the glass transition temperature of this structure is higher, it is necessary to dye at very high temperatures, promotes the dye molecule diffusion to fibrous inside. It addition, the strand of PET is regular, good crystallinity, strand arrangement closely, and does not have the polar group having an effect with dye molecule on strand, the colouring making polyester fiber is more difficult. Owing to not having hydrophilic group in its molecule, hygroscopicity is very poor, and this causes that the dyeing of terylene is relatively difficult. The main high-temperature and high pressure dyeing process method of terylene disperse dyeing
Oligomer in polyester fiber is a kind of low-molecular-weight ester or ether, is primarily referred to as the degree of polymerization oligomer less than 10, diethylene glycol, is produce as a by-product. Wherein oligomer is divided into linear oligomerization thing and cyclic oligomer, and wherein in the majority with ring-type aggressiveness particularly cyclic trimer, oligomer is mainly concerned with heterogeneous nucleation, spinning processing, dyeing etc., and performance and the processing of rear road to polyester cause certain harmful effect. Ethylene glycol terephthalate polymer (PET) is big containing about oligomer 3-4%, when fiber surface occurs that oligomer will make troubles to dyeing and post-treatment. Diffusing out of oligomer is easiest to occur the temperature control when dyeing to heat up and holding stage. When cooling, solubility with temperature reduction due to oligomer in water the same as dyestuff strongly reduces, therefore can crystallization, the dyestuff and the oligomer that precipitate out are attached to fiber surface and are very unlikely to wash away, thus bringing a lot of trouble to dyeing and post-treatment, in dyeing course, dyestuff and the oligomer of gathering stick to fiber surface, the phenomenons such as dyestuff color dot, spot, color flower occur.It is deposited in pipeline and the valve of staining machine, hinders liquid stream circulation, cause dyeing difficulty. Eliminate oligomer and it is critical only that elimination oligomer cyclic trimer and diethylene glycol, be the generation reducing oligomer in the course of the polymerization process on the one hand, be remove before dyeing or in dyeing on the other hand.
Summary of the invention
It is an object of the invention to provide a kind of low aberration polyester FDY silk and preparation method thereof, be the polyester and low aberration polyester FDY silk and preparation method thereof of the mixture of a kind of polycondensation catalyst employing ethylene glycol magnesium and antimony glycol. The present invention adopts the mixture of ethylene glycol magnesium and antimony glycol to be polycondensation catalyst, reduces thermal degradation to minimum, and polyester slice through water with dissolve and wash away agent at 130 DEG C, brew, washing when 0.3MPa; Reduce what polyester FDY silk was dyeed by oligomer, diethylene glycol content impact.
The one low aberration polyester FDY silk of the present invention, for described polyester be p-phthalic acid and ethylene glycol through esterification and under the mixture through catalytic effect of ethylene glycol magnesium and antimony glycol polycondensation, pelletize and after dissolveing and washing away spinning prepare;
In the section of described polyester, oligomer mass percentage content is less than 0.5%, and the mass percentage content of diethylene glycol is less than 0.5%;
The molecular formula of described ethylene glycol magnesium is Mg (OCH2CH2OH)2;
The described section dissolved and washed away after referring to pelletize through water with dissolve and wash away agent 120��130 DEG C with 0.2��0.3MPa when brew and washing.
Described low aberration polyester FDY silk is dissolved and washed away rear spinning by polyester and obtains, the fracture strength >=3.8cN/dtex of described low aberration polyester FDY silk, and elongation at break is 33.0 �� 3.0%, and aberration �� E is less than 0.200.
In dyeing polyester fibers and post-treatment, the factor affecting surface oligomers precipitation is a lot, mainly has the factors such as temperature and time. Improving the dyeing temperature migration by aggravation oligomer, particularly when having some auxiliary agent or dyestuff to exist, migration velocity improves faster. The time of dye liquor circulation continuous is more long, and oligomer increases from fiber to the amount of external migration, frequent cold cycling and some auxiliary agents, dyestuff existence can significantly aggravation oligomer removal and deposition. Oligomer migration speed and migration amount are had a significant impact by the temperature and time of heat setting simultaneously. Synthetic fibers dyeing and finishing is processed heat setting is an extremely important operation, and its main purpose is to eliminate the dimensional stability of existing fine wrinkle and raising fabric on fabric and improve the performances such as the brute force of fabric, feel, pilling and surfacing. But, yarn dyed fabric shaping process often occurs such phenomenon, namely easily there is mottle and barriness in the fabric face after heat setting, level-dyeing property and crock fastness are also remarkably decreased, especially for Polyester Fabric of Ultra-fine Fibre under Alkali Condition, impact is particularly acute, and oligomer migration from inside to outside under heat effect is one of the main reasons. Existing technology all concentrates on dyeing link to solve the oligomer impact on dyeing, and this is that one controls calibration method, only solves to be only effect a permanent cure basic from source.
Adopting ethylene glycol magnesium and antimony glycol mixture as polycondensation catalyst, ethylene glycol magnesium belongs to a comparatively gentle class, and its thermal degradation coefficient is only small, and the side reaction caused in course of reaction is less, decreases the generation of oligomer in the course of processing. The principal element causing thermal degradation is high temperature and catalyst, and high temperature is that response strength is too high, causes that degraded is accelerated, creates end carboxyl, also makes cyclic oligomer increase simultaneously; Catalyst is then relevant to the degradation reaction constant of catalyst, in polycondensation process, the effect of catalyst is not only in that and catalysis can generate primary response, thus affecting speed and the yield of reaction, simultaneously can also catalytic thermal degraded and ehter bond generation, the content of increase cyclic oligomer and diethylene glycol.
Line density deviation ratio��0.5% of a kind of low aberration polyester FDY silk as above, 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%.
A kind of low aberration polyester FDY silk as above, in the mixture of described ethylene glycol magnesium and antimony glycol, ethylene glycol magnesium and antimony glycol mass ratio are 2��3:1.
The preparation method that present invention also offers a kind of low aberration polyester FDY silk, a kind of preparation method of low aberration polyester FDY silk, for p-phthalic acid and ethylene glycol through esterification and under the mixture through catalytic effect of ethylene glycol magnesium and antimony glycol polycondensation prepare polyester, obtain polyester slice then through pelletizing, after then being dissolved and washed away by polyester slice, namely prepare polyester; Then through measuring, extrude, cool down, oil, stretch, thermal finalization and winding, prepare low aberration polyester fiber FDY silk; Main technique is:
(1) preparation of catalyst glycol magnesium:
Adding ethylene glycol in single-cell for electrolyzation, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and negative electrode is graphite; Logical unidirectional current, starting voltage 6��10VV, cathode-current density is 150��200mA, electrolysis 10��12 hours when 50��60 DEG C, and electrolysis takes out electrode after terminating, and obtains white suspension; Filtration under diminished pressure, white solid absolute ethanol washing, obtain ethylene glycol magnesium after drying;
(2) preparation of polyester, including esterification and polycondensation reaction:
Described esterification:
Adopt p-phthalic acid and ethylene glycol as raw material, add anti-ether agent, 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 when 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; Described catalyst is the mixture of ethylene glycol magnesium and antimony glycol;
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 less than 100Pa, and reaction temperature controls at 275��280 DEG C, 50��90 minutes response time;
Prepare polyester, obtain polyester slice through pelletizing;
(3) dissolve and wash away
Described polyester slice through water with dissolve and wash away agent 120��130 DEG C with 0.2��0.3MPa when brew 3-5 hour, by washing; Obtain polyester.
(4) spinning main technologic parameters:
The temperature of described extrusion is 280��290 DEG C;
The pathogenic wind-warm of described cooling is 20��25 DEG C;
The speed of described winding is 4000��4600m/min;
Filament number is 0.3��2.0dtex;
The mol ratio of the preparation method of a kind of low aberration polyester FDY silk as above, described ethylene glycol and described p-phthalic acid is 1.2��2.0:1.
The preparation method of a kind of low aberration polyester FDY silk as above, in the mixture of described ethylene glycol magnesium and antimony glycol, ethylene glycol magnesium and antimony glycol mass ratio are 2��3:1; Described catalyst amount is the 0.01%��0.05% of described p-phthalic acid quality.
The preparation method of a kind of low aberration polyester FDY silk as above, 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.Stabilizer is mainly based on phosphate ester, and Main Function is the free radical that catching reaction produces in the course of the polymerization process, reduces side reaction.
The preparation method of a kind of low aberration polyester FDY silk as above, described water is 100:3��4 with the mass ratio dissolveing and washing away agent, polyester slice and water and dissolve and wash away the ratio of agent, and namely solid-to-liquid ratio is 1:5-10; It is described that to dissolve and wash away agent be the one in ethylene glycol monoethyl ether, propyl cellosolve and ethylene glycol monobutyl ether (EGMBE), water adds and a small amount of dissolves and washes away agent, dissolve and wash away agent and be dissolved in water, simultaneously also the most ofs low molecular ether of solubilized and ester, be conducive to improving the minimizing of effect and the oligomer washed.
The preparation method of a kind of low aberration polyester FDY silk as above, described washing refers to 70��80 DEG C of hot water wash 10��15min of polyester slice after brew, then cleans with cold water, and Drying and cooling is standby.
The preparation method of a kind of low aberration polyester FDY silk as above, described anti-ether agent is the one in sodium acetate and calcium acetate, and anti-ether agent consumption is the 0.01%��0.05% of described p-phthalic acid weight. Anti-ether agent reduces the generation of ether in acid condition by adding a small amount of NaAc, thus reducing glycol reaction to generate the activity of diethylene glycol.
It is an object of the invention to provide a kind of low aberration polyester FDY silk, adopt a relatively mild class polycondensation catalyst ethylene glycol magnesium, course of reaction causes less side reaction is less and less thermal degradation in the course of processing, decrease the generation of oligomer in the course of processing. Polyester slice through water with dissolve and wash away agent at 130 DEG C, when 0.3MPa, brew is conducive to improving effect and the minimizing of oligomer of washing. The minimizing of oligomer so that dyeing polyester fibers and in post-treatment heat setting, oligomer reduces from fiber to the amount of external migration, decreases mottle and barriness occurs, it is ensured that fiber level-dyeing property and crock fastness.
Beneficial effect:
�� adopting ethylene glycol magnesium and antimony glycol mixture as polycondensation catalyst, ethylene glycol magnesium belongs to a comparatively gentle class, and its thermal degradation coefficient is only small, and the side reaction caused in course of reaction is less, decreases the generation of end carboxyl and oligomer in the course of processing.
�� the oligomer mass percentage content of polyester slice is less than 0.5%, and the mass percentage content of diethylene glycol, less than 0.5%, is conducive to improving further the quality of fiber.
�� polyester slice through water with dissolve and wash away agent 120��130 DEG C with 0.2��0.3MPa when brew be conducive to improving effect and the minimizing of oligomer of washing.
�� anti-ether agent reduces the generation of ether in acid condition by adding a small amount of NaAc, thus reducing glycol reaction to generate the activity of diethylene glycol.
�� the minimizing of oligomer in polymerization process, dissolveing and washing away oligomer in process to reduce further so that dyeing polyester fibers and in post-treatment heat setting, oligomer reduces from fiber to the amount of external migration, decrease mottle and barriness occurs, it is ensured that fiber level-dyeing property and crock fastness.
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 are merely to illustrate the present invention rather than 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, the present invention can be made various changes or modifications by those skilled in the art, and these equivalent form of values fall within the application appended claims limited range equally.
The one low aberration polyester FDY silk of the present invention, low aberration polyester FDY silk by polyester after dissolveing and washing away spinning and obtain, the fracture strength >=3.8cN/dtex of low aberration polyester FDY silk, elongation at break is 33.0 �� 3.0%;, aberration �� E less than 0.200, polyester be p-phthalic acid and ethylene glycol through esterification and polycondensation under the mixture through catalytic effect of ethylene glycol magnesium and antimony glycol, obtain polyester slice then through pelletizing; In the section of industry polyester, oligomer mass percentage content is less than 0.5%, and the mass percentage content of diethylene glycol is less than 0.5%; The molecular formula of ethylene glycol magnesium is Mg (OCH2CH2OH)2; Dissolve and wash away the section after referring to pelletize through water with dissolve and wash away agent 120��130 DEG C with 0.2��0.3MPa when brew and washing.
Wherein, line density deviation ratio��0.5% of low aberration polyester 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%.
Wherein, in the mixture of ethylene glycol magnesium and antimony glycol, ethylene glycol magnesium and antimony glycol mass ratio are 2��3:1.
A kind of preparation method of the low aberration polyester FDY silk of the present invention, p-phthalic acid and ethylene glycol are through being esterified and the prepared polyester of polycondensation under the mixture through catalytic effect of ethylene glycol magnesium and antimony glycol, obtain polyester slice then through pelletizing, after then being dissolved and washed away by polyester slice, namely prepare polyester; Then through measuring, extrude, cool down, oil, stretch, thermal finalization and winding, prepare low aberration polyester fiber FDY silk.
1, dyestuff:
Disperse brilliant blue 2BLN, 5% (o.w.f)
2, dyeing:
Fiber enters to contaminate insulation 10��15min, 1.0��2.0 DEG C/min of heating rate at 70��80 DEG C, 120��130 DEG C of insulation 40��60min, cooling, 70��80 DEG C of reduction cleaning 20��30min.
3, the mensuration of dye uptake
Dyeing by above-mentioned technique, and draw the front liquid of dye respectively, each 2ml of debris, in 10ml volumetric flask, adds acetone 4ml, makes dyestuff fully dissolve. With distilled water diluting to scale, then measure �� with spectrophotometricmax, time dyeing before and after the absorbance A 0 of dyestuff, A1 then:
Dye uptake (%)=(l mono-A1/A0) �� 100%
In formula: the absorbance of liquid before A0---dye
The absorbance of A1---debris
4, the mensuration of dyefastness
Test by GB3920-83, GB251-64, GB3921-83
5, the mensuration of tinctorial yield and aberration
Adopt the test of color measurement and color match instrument.
6, the mensuration of the apparent colour degree of depth (K/S)
Storehouse Bel's card Munch (kubelka-munk) function is utilized to calculate: in K/S=(1-R) 2//2R. formula, K is the absorptance of testee; S is the scattering coefficient of testee; R is reflectance during testee infinite thickness. Application SF600XDatacolor color measurement and color match instrument test, every sample is tested 5 times in zones of different, takes its mathematical mean.
Embodiment 1
A kind of preparation method of low aberration polyester FDY silk, main technique includes:
(1) preparation of catalyst glycol magnesium:
Adding ethylene glycol in single-cell for electrolyzation, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and negative electrode is graphite; Logical unidirectional current, starting voltage 6V, cathode-current density is 150mA, electrolysis 10 hours when 50 DEG C, and electrolysis takes out electrode after terminating, and obtains white suspension; Filtration under diminished pressure, white solid absolute ethanol washing, obtain ethylene glycol magnesium after drying;
(2) preparation of polyester, including esterification and polycondensation reaction:
Esterification:
Adopting p-phthalic acid and ethylene glycol is 1.2:1 as the mol ratio of raw material, ethylene glycol and p-phthalic acid, adds anti-ether agent sodium acetate, and sodium acetate consumption is the 0.01% of p-phthalic acid weight, carries out esterification, obtain esterification products after being made into uniform sizing material;Esterification is pressurizeed in nitrogen atmosphere, and Stress control is at normal pressure, and temperature is at 250 DEG C, and it is esterification terminal that esterification water quantity of distillate reaches the 91% of theoretical value;
Polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
The polycondensation reaction coarse vacuum stage, esterification products adds catalyst and stabilizer triphenyl phosphate, catalyst amount is the 0.01% of p-phthalic acid quality, triphenyl phosphate consumption is the 0.01% of p-phthalic acid weight, polycondensation reaction is started when negative pressure, this staged pressure is steadily evacuated to absolute pressure 498Pa by normal pressure, and temperature controls at 260 DEG C, and the response time is 30 minutes; Catalyst is the mixture of ethylene glycol magnesium and antimony glycol, and ethylene glycol magnesium and antimony glycol mass ratio are 2:1;
Polycondensation reaction high vacuum stage of Fig, after the polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure be down to absolute pressure 96Pa, and reaction temperature controls at 275 DEG C, 50 minutes response time; Prepare polyester, obtain polyester slice through pelletizing;
(3) dissolve and wash away
Polyester slice through water with dissolve and wash away agent ethylene glycol monoethyl ether 120 DEG C with 0.2MPa when brew 3 hours, by washing, namely after brew, polyester slice is with 70 DEG C of hot water wash 10min, and then clean with cold water, Drying and cooling is standby; Gathered
Ester, water is 100:3 with the mass ratio dissolveing and washing away agent, polyester slice and water and dissolve and wash away the ratio of agent, and namely solid-to-liquid ratio is 1:5.
(4) spinning main technologic parameters:
The temperature of extrusion is 280 DEG C;
The pathogenic wind-warm of cooling is 20 DEG C;
The speed of winding is 4000m/min;
Filament number is 0.3dtex.
Preparing the fracture strength 3.8cN/dtex of low aberration polyester FDY silk, elongation at break is 30.5%, line density deviation ratio 0.4%, fracture strength CV value 3.6%, extension at break CV value 8.8%, yarn unevenness CV1.89%, boiling water shrinkage 7.8%, oil content 0.85%.
(5) dyeing
Embodiment 2
A kind of preparation method of low aberration polyester FDY silk, main technique includes:
(1) preparation of catalyst glycol magnesium:
Adding ethylene glycol in single-cell for electrolyzation, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and negative electrode is graphite; Logical unidirectional current, starting voltage 10V, cathode-current density is 200mA, electrolysis 12 hours when 60 DEG C, and electrolysis takes out electrode after terminating, and obtains white suspension; Filtration under diminished pressure, white solid absolute ethanol washing, obtain ethylene glycol magnesium after drying;
(2) preparation of polyester, including esterification and polycondensation reaction:
Esterification:
Adopting p-phthalic acid and ethylene glycol is 2.0:1 as the mol ratio of raw material, ethylene glycol and p-phthalic acid, adds anti-ether agent calcium acetate, and calcium acetate consumption is the 0.05% of p-phthalic acid weight, carries out esterification, obtain esterification products after being made into uniform sizing material; Esterification is pressurizeed in nitrogen atmosphere, and Stress control is at 0.3MPa, and temperature is at 260 DEG C, and it is esterification terminal that esterification water quantity of distillate reaches the 92% of theoretical value;
Polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
The polycondensation reaction coarse vacuum stage, esterification products adds catalyst and stabilizer trimethyl phosphate, catalyst amount is the 0.05% of p-phthalic acid quality, trimethyl phosphate consumption is the 0.05% of p-phthalic acid weight, polycondensation reaction is started when negative pressure, this staged pressure is steadily evacuated to absolute pressure 496Pa by normal pressure, and temperature controls at 270 DEG C, and the response time is 50 minutes;Catalyst is the mixture of ethylene glycol magnesium and antimony glycol, and ethylene glycol magnesium and antimony glycol mass ratio are 3:1;
Polycondensation reaction high vacuum stage of Fig, after the polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure be down to absolute pressure 95Pa, and reaction temperature controls at 280 DEG C, 90 minutes response time; Prepare polyester, obtain polyester slice through pelletizing;
(3) dissolve and wash away
Polyester slice through water with dissolve and wash away agent propyl cellosolve 130 DEG C with 0.3MPa when brew 5 hours, by washing, namely after brew, polyester slice is with 80 DEG C of hot water wash 15min, and then clean with cold water, Drying and cooling is standby; Obtaining polyester, water is 100:4 with the mass ratio dissolveing and washing away agent, polyester slice and water and dissolve and wash away the ratio of agent, and namely solid-to-liquid ratio is 1:10.
(4) spinning main technologic parameters:
The temperature of extrusion is 290 DEG C;
The pathogenic wind-warm of cooling is 25 DEG C;
The speed of winding is 4600m/min;
Filament number is 0.3dtex.
Preparing the fracture strength 4.6cN/dtex of low aberration polyester FDY silk, elongation at break is 34.0%, line density deviation ratio 0.3%, fracture strength CV value 3.6%, extension at break CV value 9.2%, yarn unevenness CV1.8%, boiling water shrinkage 6.8%, oil content 0.85%.
(5) dyeing
Embodiment 3
A kind of preparation method of low aberration polyester FDY silk, main technique includes:
(1) preparation of catalyst glycol magnesium:
Adding ethylene glycol in single-cell for electrolyzation, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and negative electrode is graphite; Logical unidirectional current, starting voltage 7V, cathode-current density is 160mA, electrolysis 11 hours when 55 DEG C, and electrolysis takes out electrode after terminating, and obtains white suspension; Filtration under diminished pressure, white solid absolute ethanol washing, obtain ethylene glycol magnesium after drying;
(2) preparation of polyester, including esterification and polycondensation reaction:
Esterification:
Adopting p-phthalic acid and ethylene glycol is 1.5:1 as the mol ratio of raw material, ethylene glycol and p-phthalic acid, adds anti-ether agent sodium acetate, and sodium acetate consumption is the 0.02% of p-phthalic acid weight, carries out esterification, obtain esterification products after being made into uniform sizing material; Esterification is pressurizeed in nitrogen atmosphere, and Stress control is at 0.2MPa, and temperature is at 255 DEG C, and it is esterification terminal that esterification water quantity of distillate reaches the 92% of theoretical value;
Polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
The polycondensation reaction coarse vacuum stage, esterification products adds catalyst and stabilizer NSC 6513, catalyst amount is the 0.02% of p-phthalic acid quality, NSC 6513 consumption is the 0.02% of p-phthalic acid weight, polycondensation reaction is started when negative pressure, this staged pressure is steadily evacuated to absolute pressure 496Pa by normal pressure, and temperature controls at 265 DEG C, and the response time is 35 minutes; Catalyst is the mixture of ethylene glycol magnesium and antimony glycol, and ethylene glycol magnesium and antimony glycol mass ratio are 3:1;
Polycondensation reaction high vacuum stage of Fig, after the polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure be down to absolute pressure 98Pa, and reaction temperature controls at 277 DEG C, 60 minutes response time; Prepare polyester, obtain polyester slice through pelletizing;
(3) dissolve and wash away
Polyester slice through water with dissolve and wash away agent ethylene glycol monobutyl ether (EGMBE) 125 DEG C with 0.2MPa when brew 3 hours, by washing, namely after brew, polyester slice is with 70 DEG C of hot water wash 15min, and then clean with cold water, Drying and cooling is standby;Obtaining polyester, water is 100:4 with the mass ratio dissolveing and washing away agent, polyester slice and water and dissolve and wash away the ratio of agent, and namely solid-to-liquid ratio is 1:10.
(4) spinning main technologic parameters:
The temperature of extrusion is 285 DEG C;
The pathogenic wind-warm of cooling is 24 DEG C;
The speed of winding is 4600m/min;
Filament number is 0.3dtex.
Preparing the fracture strength 4.1cN/dtex of low aberration polyester FDY silk, elongation at break is 35.2%, line density deviation ratio 0.45%, fracture strength CV value 5.0%, extension at break CV value 8.9%, yarn unevenness CV1.95%, boiling water shrinkage 7.8%, oil content 0.75%.
(5) dyeing
Embodiment 4
A kind of preparation method of low aberration polyester FDY silk, main technique includes:
(1) preparation of catalyst glycol magnesium:
Adding ethylene glycol in single-cell for electrolyzation, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and negative electrode is graphite; Logical unidirectional current, starting voltage 7V, cathode-current density is 170mA, electrolysis 11 hours when 58 DEG C, and electrolysis takes out electrode after terminating, and obtains white suspension; Filtration under diminished pressure, white solid absolute ethanol washing, obtain ethylene glycol magnesium after drying;
(2) preparation of polyester, including esterification and polycondensation reaction:
Esterification:
Adopt p-phthalic acid and ethylene glycol as raw material, the mol ratio of ethylene glycol and described p-phthalic acid is 1.8:1, adds anti-ether agent sodium acetate, and sodium acetate consumption is the 0.02% of p-phthalic acid weight, 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 250 DEG C, and it is esterification terminal that esterification water quantity of distillate reaches the 98% of theoretical value;
Polycondensation reaction:
Including polycondensation reaction coarse vacuum stage and polycondensation reaction high vacuum stage of Fig:
The polycondensation reaction coarse vacuum stage, esterification products adds catalyst and stabilizer triphenyl phosphate, catalyst amount is the 0.01% of described p-phthalic acid quality, triphenyl phosphate consumption is the 0.02% of p-phthalic acid weight, polycondensation reaction is started when negative pressure, this staged pressure is steadily evacuated to absolute pressure 496Pa by normal pressure, and temperature controls at 264 DEG C, and the response time is 38 minutes; Catalyst is the mixture of ethylene glycol magnesium and antimony glycol, and ethylene glycol magnesium and antimony glycol mass ratio are 3:1;
Polycondensation reaction high vacuum stage of Fig, after the polycondensation reaction coarse vacuum stage, continues evacuation, makes reaction pressure be down to absolute pressure 99Pa, and reaction temperature controls at 280 DEG C, 90 minutes response time; Prepare polyester, obtain polyester slice through pelletizing;
(3) dissolve and wash away
Polyester slice through water with dissolve and wash away agent ethylene glycol monoethyl ether 120 DEG C with 0.3MPa when brew 3 hours, by washing, namely after brew, polyester slice is with 70 DEG C of hot water wash 15min, and then clean with cold water, Drying and cooling is standby; Obtaining polyester, water is 100:4 with the mass ratio dissolveing and washing away agent, polyester slice and water and dissolve and wash away the ratio of agent, and namely solid-to-liquid ratio is 1:8.
(4) spinning main technologic parameters:
The temperature of extrusion is 285 DEG C;
The pathogenic wind-warm of cooling is 25 DEG C;
The speed of winding is 4500m/min;
Filament number is 0.3dtex.
Preparing the fracture strength 3.9cN/dtex of low aberration polyester FDY silk, elongation at break is 36%, line density deviation ratio 0.3%, fracture strength CV value 4.5%, extension at break CV value 9.5%, yarn unevenness CV1.99%, boiling water shrinkage 7.8%, oil content 1.05%.
(5) dyeing
Claims (10)
1. a low aberration polyester FDY silk, is characterized in that: described low aberration polyester FDY silk by polyester after dissolveing and washing away spinning and obtain,
Fracture strength >=the 3.8cN/dtex of described low aberration polyester FDY silk, elongation at break is 33.0 �� 3.0%; Aberration �� E less than 0.200, described polyester be p-phthalic acid and ethylene glycol through esterification and polycondensation under the mixture through catalytic effect of ethylene glycol magnesium and antimony glycol, obtain polyester slice then through pelletizing;
In the section of described industry polyester, oligomer mass percentage content is less than 0.5%, and the mass percentage content of diethylene glycol is less than 0.5%;
The molecular formula of described ethylene glycol magnesium is Mg (OCH2CH2OH)2;
The described section dissolved and washed away after referring to pelletize through water with dissolve and wash away agent 120��130 DEG C with 0.2��0.3MPa when brew and washing.
2. one according to claim 1 low aberration polyester FDY silk, it is characterized in that, line density deviation ratio��0.5% of described low aberration polyester 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 low aberration polyester FDY silk, it is characterised in that in the mixture of described ethylene glycol magnesium and antimony glycol, ethylene glycol magnesium and antimony glycol mass ratio are 2��3:1.
4. the preparation method of a kind of low aberration polyester FDY silk as according to any one of claims 1 to 3, it is characterized in that: p-phthalic acid and ethylene glycol are through being esterified and the prepared polyester of polycondensation under the mixture through catalytic effect of ethylene glycol magnesium and antimony glycol, obtain polyester slice then through pelletizing, after then being dissolved and washed away by polyester slice, namely prepare polyester; Then through measuring, extrude, cool down, oil, stretch, thermal finalization and winding, prepare low aberration polyester fiber FDY silk.
5. the preparation method of a kind of low aberration polyester FDY silk according to claim 4, it is characterised in that main technique includes:
(1) preparation of catalyst glycol magnesium:
Adding ethylene glycol in single-cell for electrolyzation, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and negative electrode is graphite; Logical unidirectional current, starting voltage 6��10V, cathode-current density is 150��200mA, electrolysis 10��12 hours when 50��60 DEG C, and electrolysis takes out electrode after terminating, and obtains white suspension; Filtration under diminished pressure, white solid absolute ethanol washing, obtain ethylene glycol magnesium after drying;
(2) preparation of polyester, including esterification and polycondensation reaction:
Described esterification:
Adopt p-phthalic acid and ethylene glycol as raw material, add anti-ether agent, 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 when 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; Described catalyst is the mixture of ethylene glycol magnesium and antimony glycol;
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 less than 100Pa, and reaction temperature controls at 275��280 DEG C, 50��90 minutes response time;
Prepare polyester, obtain polyester slice through pelletizing;
(3) dissolve and wash away
Described polyester slice through water with dissolve and wash away agent 120��130 DEG C with 0.2��0.3MPa when brew 3-5 hour, by washing; Obtain polyester.
(4) spinning main technologic parameters:
The temperature of described extrusion is 280��290 DEG C;
The pathogenic wind-warm of described cooling is 20��25 DEG C;
The speed of described winding is 4000��4600m/min;
Filament number is 0.3��2.0dtex.
6. the preparation method of a kind of low aberration polyester FDY silk according to claim 4 or 5, it is characterised in that the mol ratio of described ethylene glycol and described p-phthalic acid is 1.2��2.0:1.
7. the preparation method of a kind of low aberration polyester FDY silk according to claim 5, it is characterised in that in the mixture of described ethylene glycol magnesium and antimony glycol, ethylene glycol magnesium and antimony glycol mass ratio are 2��3:1; Described catalyst amount is the 0.01%��0.05% of described p-phthalic acid quality; 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.
8. the preparation method of a kind of low aberration polyester FDY silk according to claim 5, it is characterised in that described water is 100:3��4 with the mass ratio dissolveing and washing away agent, polyester slice and water and the ratio dissolveing and washing away agent, namely solid-to-liquid ratio is 1:5��10; It is described that to dissolve and wash away agent be the one in ethylene glycol monoethyl ether, propyl cellosolve and ethylene glycol monobutyl ether (EGMBE).
9. the preparation method of a kind of low aberration polyester FDY silk according to claim 5, it is characterised in that described washing refers to 70��80 DEG C of hot water wash 10��15min of polyester slice after brew, then cleans with cold water, and Drying and cooling is standby.
10. the preparation method of a kind of low aberration polyester FDY silk according to claim 5, it is characterised in that described anti-ether agent is the one in sodium acetate and calcium acetate, and anti-ether agent consumption is the 0.01%��0.05% of described p-phthalic acid weight.
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| CN104499082A (en) * | 2014-12-31 | 2015-04-08 | 江苏恒力化纤股份有限公司 | Polyester fiber DTY (draw textured yarn) with high dyeing rate and preparation method thereof |
| CN105155007A (en) * | 2015-07-31 | 2015-12-16 | 江苏恒科新材料有限公司 | Threeleaf heteromorphic FDY fiber and preparation method for same |
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| CN1594660A (en) * | 2004-07-05 | 2005-03-16 | 苏州大学 | Process for synthesizing glycol antimony |
| CN104499082A (en) * | 2014-12-31 | 2015-04-08 | 江苏恒力化纤股份有限公司 | Polyester fiber DTY (draw textured yarn) with high dyeing rate and preparation method thereof |
| CN105155007A (en) * | 2015-07-31 | 2015-12-16 | 江苏恒科新材料有限公司 | Threeleaf heteromorphic FDY fiber and preparation method for same |
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