CN105483853A - Low-heat-shrinkage polyester industrial yarn for advertising lamp-box fabric and preparation method of polyester industrial yarn - Google Patents
Low-heat-shrinkage polyester industrial yarn for advertising lamp-box fabric and preparation method of polyester industrial yarn Download PDFInfo
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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
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of 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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- 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
- C08G63/88—Post-polymerisation treatment
- C08G63/90—Purification; Drying
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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
- D01D5/08—Melt spinning methods
- D01D5/088—Cooling filaments, threads or the like, leaving the spinnerettes
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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
- D01D7/00—Collecting the newly-spun products
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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
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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Abstract
The invention relates to a low-heat-shrinkage polyester industrial yarn for an advertising lamp-box fabric and a preparation method of the polyester industrial yarn. The low-heat-shrinkage polyester industrial yarn for the advertising lamp-box fabric is prepared by dissolving and washing polyester, and spinning after solid polymerization; the dry heat shrinkage rate of the fiber of the low-heat shrinkage polyester industrial yarn for the advertising lamp-box fabric under the test condition of 177 DEG C*10min*0.05cN/dtex is 2.0%+/-0.5%; the breaking strength of the low-heat shrinkage polyester industrial yarn for the advertising lamp-box fabric is greater than or equal to 7.5cN/dtex; with an ethylene glycol magnesium and ethylene glycol antimony mixture as a polycondensation catalyst, the thermal degradation coefficient is very small; the oligomer in the polymerization process is few; impurities in the polyester are greatly reduced by reduction of thermal degradation in the processing process; meanwhile, the amount of a nucleating agent in the polyester is also reduced; the probability of homogeneous nucleation is improved on the basis of reducing heterogeneous nucleation; the content of the oligomer is further reduced by dissolving and washing; and grain size increase in the low-heat-shrinkage polyester industrial yarn for the advertising lamp-box fabric and crystal integrity optimization are facilitated.
Description
Technical field
The invention belongs to polyester industrial fiber preparing technical field, advertising lamp box cloth polyester industrial fiber relating to a kind of low thermal shrinkage and preparation method thereof, particularly a kind of polycondensation catalyst adopts the mixture of ethylene glycol magnesium and antimony glycol and polyester slice through water and dissolves and washes away agent at 120 ~ 130 DEG C, the polyester of brew, washing under 0.2 ~ 0.3MPa condition and the advertising lamp box cloth polyester industrial fiber of low thermal shrinkage and preparation method thereof.
Background technology
Polyethylene terephthalate (PET) is a kind of polymer of function admirable, PET is high with its modulus, intensity is high, well-pressed, conformality good, pure health, barrier property are good, be widely used in the fields such as fiber, bottle packaging, film and sheet material, output cumulative year after year, position in industry significantly promotes.
Pet Industrial Fiber mainly refers to and is mostly applied to industry, national defence, medical treatment, environmental protection and most advanced branches of science each side; that there is relatively special physicalchemical structure, character and utilization; or there is the chemical fibre of specific function, be mainly reflected in be able to bear strong corrosion, low wearing and tearing, high temperature resistant, radiation hardness, fire-retardant, fire-resistant, high voltage withstanding, high strength and modulus and plurality of medical function.The PVC shelter cloth produced using high-strength low-shrinkage polyester industrial filament yarn as raw material, has higher peel strength and tearing strength, makes shelter cloth be applicable to various uses, flexible body advertising lamp box material, inflatable structure material, overcanopy architectural fabrics velaria etc.With high-strength low-shrinkage industrial yarn for main textile material is applied in the military supplies such as special protective garment, camouflage, covering, knapsack.One as earth working material has the advantages such as light, soft, high-strength, wear-resisting, anticorrosive, non-conductive, damping.Safe ready during use, efficiency are high, and can not damage lifting object.The Application Areas of Pet Industrial Fiber is expanded and is driven the whole competitiveness of Application Areas to promote, no matter alleviating the weight of composite, the durability used and minimizing are keeped in repair, are raised all many-sides such as cost, and polyesters high-performance fiber has more and more given play to its synthetic competitive advantages.Following many decades, the development of high-performance poly ester fiber not only has considerable progress in quantity, more in the expansion of Application Areas and the lifting of industrial chain whole competitiveness, obtains substantial effect.
The Main way that Pet Industrial Fiber develops by high strength, high-modulus, lower shrinkage, DIMENSIONAL STABILITY, functionalization, and what affect fiber quality is the collection state structure of polyester macromolecule, be mainly concerned with the active force between polyester molecule, the Morphology and structure, orientation structure etc. of crystallization, and the Morphology and structure of crystallization is emphasis wherein.
End carboxyl, oligomer, diethylene glycol (DEG) (DEG) content are the important quality index of polyester slice, and wherein oligomer, diethylene glycol (DEG) are all oligomer, and they not only reflect the quality of production status, also can have influence on the product quality of spinning process.Therefore, the end carboxyl in minimizing polyester slice, oligomer, diethylene glycol content just become and improve the very important link of polyester product quality.The impact of end carboxyl on polymer performance is not allowed not look, and only has control polyester content of carboxyl end group to stablize aborning, the homogeneity of its relative molecular mass distribution of control that could be stable.The content of diethylene glycol (DEG) in polyester slice is a very important quality index in production of polyester.Because it directly has influence on the fusing point of polyester slice, the fusing point of polyester slice sharply can decline with the increase of the wherein content of DEG, so it not only reflects the quality of production status, directly has influence on the quality of aft-loaded airfoil-spinning technique and silk.Oligomer in polyester refers to the oligomer that the degree of polymerization is less than 10, be divided into linear oligomerization thing and cyclic oligomer, wherein with ring-type aggressiveness, particularly cyclic trimer is in the majority, oligomer is mainly concerned with heterogeneous nucleation, spinning process etc., causes certain harmful effect to the performance of polyester and the processing of rear road.Controlling the content of three in polyester slice is problem very important in polyester production process.
Summary of the invention
Advertising lamp box cloth polyester industrial fiber that the object of this invention is to provide a kind of low thermal shrinkage and preparation method thereof is the polyester of mixture and the advertising lamp box cloth polyester industrial fiber of low thermal shrinkage and preparation method thereof that a kind of polycondensation catalyst adopts ethylene glycol magnesium and antimony glycol.The advertising lamp box cloth polyester industrial fiber of described low thermal shrinkage is under the test condition of 177 DEG C × 10min × 0.05cN/dtex in temperature, and the dry-hot shrinkage of fiber is 2.0 ± 0.5%; The advertising lamp box cloth polyester industrial fiber fracture strength >=7.5cN/dtex of described low thermal shrinkage; The present invention adopts the mixture of ethylene glycol magnesium and antimony glycol to be polycondensation catalyst, and thermal degradation is reduced to minimum, and polyester slice through water with dissolve and wash away agent at 130 DEG C, brew, washing under 0.3MPa condition; The impact that minimizing end carboxyl, oligomer, diethylene glycol content are processed Direct-spinning of PET Fiber.
The advertising lamp box cloth polyester industrial fiber of a kind of low thermal shrinkage of the present invention is terephthalic acid (TPA) and ethylene glycol through polycondensation, granulation under esterification and the mixture through catalytic effect at ethylene glycol magnesium and antimony glycol for described polyester and dissolve and wash away, spinning and obtaining after solid-phase tack producing;
In the section of described industry polyester, content of carboxyl end group is less than 15mol/t, and oligomer mass percentage content is less than 0.5%, and the mass percentage content of diethylene glycol (DEG) is less than 0.5%;
The molecular formula of described ethylene glycol magnesium is Mg (OCH
2cH
2oH)
2;
Described dissolve and wash away the section after referring to granulation through water with dissolve and wash away agent 120 ~ 130 DEG C with 0.2 ~ 0.3MPa condition under brew and
Washing.
The Main way that Pet Industrial Fiber develops by high strength, high-modulus, lower shrinkage, DIMENSIONAL STABILITY, functionalization, and what affect fiber quality is the collection state structure of polyester macromolecule, be mainly concerned with the active force between polyester molecule, the Morphology and structure, orientation structure etc. of crystallization, and the Morphology and structure of crystallization is emphasis wherein.
Lower shrinkage, DIMENSIONAL STABILITY are the principal elements affecting high-quality polyester, macroscopical thermal contraction phenomenon of polyester fiber is because the Entropy Changes trend of local elongation macromolecular chain, the internal stress produced to rolled state development and spinning process process freeze axial internal stress in the sample to which, this local internal stress can be relayed to whole material by molecular network structure, when the external world provides enough heat energy, the phenomenon of generation.
Polyester fiber belongs to orientation hypocrystalline macromolecular material, and the construction unit different by orientation stability forms: the crystalline portion of (1) high stable and high integrity degree; (2) the imperfection crystalline portion of relatively low stability; (3) transition zone between the crystallization of low stability and amorphous; (4) unstable orientation amorphous phase.When polyester fiber is heated, following situation may be there is: retraction and crystallization occur the amorphous phase of orientation; The destruction of imperfection crystalline portion and recrystallization may occur: the thickening of crystal grain or the complete melting of crystal grain.Illustrate that crystallite dimension and crystallization degree of perfection are the key factors ensureing fiber high temperature DIMENSIONAL STABILITY.The fiber that what 177 DEG C of percent thermal shrinkages were low is thermal dimensional stability is splendid., there are two design features: crystallite dimension is large and crystallization integrity is good.Therefore the crystallite dimension of fiber is large and crystallization integrity is good, is the guarantee of low shrinkage fibre quality.
The factor affecting crystallizing polyester mainly contains: the structure of (1) strand itself.(2) selection of crystallization temperature.(3) impact of molecular weight.(4) application of nucleator.(5) be exactly finally the impact of process conditions.Wherein nucleation is that in the main link of crystallization process, a very important ring nucleator is to accelerate the carrying out of crystallization to a certain extent, low-shrinkage polyester industrial fiber be the more important thing is to the size and crystallization integrity that affect crystallization simultaneously.
Determining terminal carboxy group in PET is high, the poor heat stability of mylar, and polyester and carboxylate react the carboxylate of the polyester macromolecule chain generated simultaneously, consist of nucleus, makes polyester accelerate heterogeneous nucleation.Oligomer containing 3-4% in polyester, form mainly with low molecular ether and ester exists, main based on cyclic trimer oligomer, diethylene glycol (DEG), the qualitative effects of oligomer to polyester is larger, mainly with the mode of nucleator affect the crystallization nucleation mechanism of polyester, degree of crystallinity, crystal habit and crystallization integrality etc. so that affect the percent thermal shrinkage of quality, particularly polyester industrial fiber of polyester fiber.Not containing the pure polyester of diethylene glycol (DEG), no matter how crystallization condition changes, and all there will not be the form of abnormal spherocrystal; And when containing diethylene glycol (DEG) in sample, there will be the form that normal and abnormal spherocrystal coexists in crystalline region, and along with the increase of diethylene glycol content, the ratio of abnormal spherocrystal in whole form rises, thus have influence on the integrality of crystallization, the crystallization integrity of its polyester is reduced.Cyclic trimer occurs in the mode of polyester mainly with nucleation, and nucleator is many, and crystallization rate is fast, and crystal grain quantity is large, but crystallite dimension is less, and then has influence on the integrity of crystallization.The increase of heterogeneous nucleation, the crystalline portion of high stable and high integrity degree is reduced, and the imperfection crystalline portion of relatively low stability and the transition zone between the crystallization of low stability and amorphous strengthen, and produce harmful effect to the thermal contraction of polyester fiber.
The advertising lamp box cloth polyester industrial fiber of a kind of low thermal shrinkage as above, line line density deviation ratio≤1.5% of the advertising lamp box cloth industrial yarn of described low thermal shrinkage, fracture strength CV value≤2.5%, extension at break is 16.0 ± 1.5%, extension at break CV value≤7.0%, network 6 ± 2.
The advertising lamp box cloth polyester industrial fiber of a kind of low thermal shrinkage 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.
Present invention also offers a kind of preparation method of advertising lamp box cloth polyester industrial fiber of low thermal shrinkage, for the polycondensation under esterification and the mixture through catalytic effect at ethylene glycol magnesium and antimony glycol of terephthalic acid (TPA) and ethylene glycol obtains polyester, obtain polyester slice through pelletizing again, then by dissolveing and washing away, solid phase polycondensation thickening; Again through measuring, extruding, cool, oil, stretch, HEAT SETTING, winding, obtained heat-resistance polyester industrial yarn.
The preparation method of the advertising lamp box cloth polyester industrial fiber of a kind of low thermal shrinkage as above, main technique is:
(1) preparation of catalyst glycol magnesium:
In single-cell for electrolyzation, add ethylene glycol, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and negative electrode is graphite; Logical direct current, starting voltage 6 ~ 10VV, cathode-current density is 150 ~ 200mA, electrolysis 10 ~ 12 hours when 50 ~ 60 DEG C, and electrolysis terminates rear taking-up electrode, obtains white turbid liquid; Filtration under diminished pressure, white solid absolute ethanol washing, obtains ethylene glycol magnesium after drying;
(2) preparation of polyester, comprises esterification and polycondensation reaction:
Described esterification:
Adopt terephthalic acid (TPA) 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 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; 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 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 polyester, obtains polyester slice through pelletizing;
(3) dissolve and wash away
Described polyester slice is through water and dissolve and wash away agent brew 3-5 hour under 120 ~ 130 DEG C with 0.2 ~ 0.3MPa condition, by washing;
(4) solid phase polycondensation:
Institute's polyester slice that obtains, by solid phase polycondensation thickening, makes the inherent viscosity of polyester slice bring up to 1.0 ~ 1.2dL/g, is high sticky section;
(5) spinning main technologic parameters:
The described temperature extruded is 290 ~ 320 DEG C;
The wind-warm syndrome of described cooling is 20 ~ 30 DEG C;
Described stretching, heat setting process:
GR-1 speed 450 ~ 600m/min; Temperature is normal temperature;
GR-2 speed 500 ~ 1000m/min; Temperature 85 ~ 100 DEG C;
GR-3 speed 1700 ~ 2300m/min; Temperature 100 ~ 150 DEG C;
GR-4 speed 2500 ~ 3300m/min; Temperature 200 ~ 250 DEG C;
GR-5 speed 2500 ~ 3300m/min; Temperature 200 ~ 250 DEG C;
GR-6 speed 2300 ~ 3200m/min; Temperature 150 ~ 220 DEG C;
The speed of described winding is 2300 ~ 3200m/min.
The preparation method of the advertising lamp box cloth polyester industrial fiber of a kind of low thermal shrinkage as above, the mol ratio of described ethylene glycol and described terephthalic acid (TPA) is 1.2 ~ 2.0:1.
The preparation method of the advertising lamp box cloth polyester industrial fiber of a kind of low thermal shrinkage 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 0.01% ~ 0.05% of described terephthalic acid (TPA) quality.
Adopt 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 very little, and the side reaction caused in course of reaction is less, decreases the generation of end carboxyl and oligomer in process.Cause the principal element of thermal degradation to be high temperature and catalyst, high temperature is that response intensity is too high, causes degraded to be accelerated, creates end carboxyl, also make cyclic oligomer increase simultaneously; Catalyst is then relevant to the degradation reaction constant of catalyst, and in polycondensation process, the effect of catalyst is not only catalysis to generate main reaction, thus the velocity ratio and output of impact reaction, can also degrade and ehter bond generation by catalytic thermal simultaneously, increase the content of diethylene glycol (DEG), thus increase the content of end carboxyl.
The preparation method of the advertising lamp box cloth polyester industrial fiber of a kind of low thermal shrinkage 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.Stabilizing agent is mainly based on phosphate, and Main Function is the free radical of catching reaction generation in the course of the polymerization process, reduces side reaction.
The preparation method of the advertising lamp box cloth polyester industrial fiber of a kind of low thermal shrinkage as above, 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, and namely solid-to-liquid ratio is 1:5-10; It is described that to dissolve and wash away agent be one in ethylene glycol monoethyl ether, propyl cellosolve and ethylene glycol monobutyl ether (EGMBE), add in water and a small amount of dissolve and wash away agent, dissolve and wash away agent water-soluble, simultaneously also the most ofs low molecular ether of solubilized and ester, be conducive to the minimizing improving effect and the oligomer washed.
The preparation method of the advertising lamp box cloth polyester industrial fiber of a kind of low thermal shrinkage as above, described washing refers to polyester slice 70 ~ 80 DEG C of hot water wash 10 ~ 15min after brew, and then clean with cold water, Drying and cooling is for subsequent use.
The preparation method of the advertising lamp box cloth polyester industrial fiber of a kind of low thermal shrinkage as above, described anti-ether agent is the one in sodium acetate and calcium acetate, and anti-ether agent consumption is 0.01% ~ 0.05% of described terephthalic acid (TPA) weight.Anti-ether agent reduces the generation of ether in acid condition by adding a small amount of NaAc, thus reduces the activity that glycol reaction generates diethylene glycol (DEG).
The object of this invention is to provide a kind of advertising lamp box cloth polyester industrial fiber of low thermal shrinkage, adopt a relatively mild class polycondensation catalyst ethylene glycol magnesium, less thermal degradation in the less and process of the less side reaction caused in course of reaction, decreases the generation of oligomer in process.Polyester slice is through water and dissolve and wash away agent at 130 DEG C, and under 0.3MPa condition, brew is conducive to improving the effect of washing and the minimizing of oligomer.In polymerization process, oligomer reduces, the reduction of thermal degradation in process, greatly reduce the impurity in polyester, also reduce the amount of nucleator in polyester simultaneously, the basis of reducing heterogeneous nucleation adds the probability of homogeneous nucleation, is conducive to growing up and the optimization of crystallization integrity of the crystallite dimension in the advertising lamp box cloth polyester industrial silk fiber of low thermal shrinkage.
Beneficial effect:
● adopt 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 very little, and the side reaction caused in course of reaction is less, decreases the generation of end carboxyl and oligomer in process.
● the content of carboxyl end group of polyester slice is less than 15mol/t, and oligomer mass percentage content is less than 0.5%, and the mass percentage content of diethylene glycol (DEG) is less than 0.5%, is conducive to the quality improving fiber further.
● polyester slice through water with dissolve and wash away agent brew under 120 ~ 130 DEG C with 0.2 ~ 0.3MPa condition and be conducive to improving the minimizing of effect and the oligomer washed.
● anti-ether agent reduces the generation of ether in acid condition by adding a small amount of NaAc, thus reduces the activity that glycol reaction generates diethylene glycol (DEG).
● in polymerization process, oligomer reduces, the reduction of thermal degradation in process, greatly reduce the impurity in polyester, also reduce the amount of nucleator in polyester simultaneously, the basis of reducing heterogeneous nucleation adds the probability of homogeneous nucleation, is conducive to growing up and the optimization of crystallization integrity of crystallite dimension in the advertising lamp box cloth polyester industrial silk fiber of low thermal shrinkage.
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.
The preparation method of the advertising lamp box cloth polyester industrial fiber of a kind of low thermal shrinkage of the present invention, the polycondensation under esterification and the mixture through catalytic effect at ethylene glycol magnesium and antimony glycol of terephthalic acid (TPA) and ethylene glycol obtains polyester, then obtains polyester slice through pelletizing; Then by dissolveing and washing away and solid phase polycondensation thickening; Again through measuring, extruding, cool, oil, stretch, HEAT SETTING and winding, the advertising lamp box cloth polyester industrial fiber of obtained low thermal shrinkage
Embodiment 1
A preparation method for the advertising lamp box cloth polyester industrial fiber of low thermal shrinkage, main technique is:
(1) preparation of catalyst glycol magnesium:
In single-cell for electrolyzation, add ethylene glycol, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and negative electrode is graphite; Logical direct current, starting voltage 6V, cathode-current density is 150mA, electrolysis 10 hours when 50 DEG C, and electrolysis terminates rear taking-up electrode, obtains white turbid liquid; Filtration under diminished pressure, white solid absolute ethanol washing, obtains ethylene glycol magnesium after drying;
(2) preparation of polyester, comprises esterification and polycondensation reaction:
Esterification:
Adopt terephthalic acid (TPA) and ethylene glycol as raw material, the mol ratio of ethylene glycol and terephthalic acid (TPA) is 1.2:1, and add anti-ether agent sodium acetate, sodium acetate consumption is 0.01% of terephthalic acid (TPA) 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 esterification water quantity of distillate reaches 91% of theoretical value for esterification terminal;
Polycondensation reaction:
Comprise polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig:
The described polycondensation reaction low vacuum stage, catalyst and stabilizing agent triphenyl phosphate ester is added in esterification products, triphenyl phosphate ester consumption is 0.01% of terephthalic acid (TPA) weight, catalyst amount is 0.01% of terephthalic acid (TPA) quality, polycondensation reaction is started under the condition of negative pressure, this staged pressure is steadily evacuated to absolute pressure 498Pa by normal pressure, and temperature controls at 260 DEG C, and the reaction 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 described polycondensation reaction low vacuum stage, continues to vacuumize, makes reaction pressure be down to absolute pressure 98Pa, and reaction temperature controls at 275 DEG C, 50 minutes reaction time; Obtained polyester, obtains polyester slice through pelletizing;
(3) dissolve and wash away
Polyester slice through water with dissolve and wash away agent ethylene glycol monoethyl ether brew 3 hours under 120 DEG C with 0.2MPa condition, by washing, i.e. polyester slice 70 DEG C of hot water wash 10min after brew, then clean with cold water, Drying and cooling is for subsequent use, water is 100:3 with the mass ratio dissolveing and washing away agent, polyester slice and water and the ratio dissolveing and washing away agent, and namely solid-to-liquid ratio is 1:5;
(4) solid phase polycondensation:
Institute's polyester slice that obtains, by solid phase polycondensation thickening, makes the inherent viscosity of polyester slice bring up to 1.0dL/g, is high sticky section;
(5) spinning main technologic parameters:
The temperature extruded is 290 DEG C;
The wind-warm syndrome of cooling is 20 DEG C;
Stretching, heat setting process:
GR-1 speed 450m/min; Temperature is normal temperature;
GR-2 speed 500m/min; Temperature 85 DEG C;
GR-3 speed 1700m/min; Temperature 100 DEG C;
GR-4 speed 2500m/min; Temperature 200 DEG C;
GR-5 speed 2500m/min; Temperature 200 DEG C;
GR-6 speed 2300m/min; Temperature 210 DEG C;
The speed of winding is 2300m/min.
The advertising lamp box cloth polyester industrial fiber of obtained low thermal shrinkage is under the test condition of 177 DEG C × 10min × 0.05cN/dtex in temperature, and the dry-hot shrinkage of fiber is 2.5%; The advertising lamp box cloth polyester industrial fiber fracture strength 7.5cN/dtex of low thermal shrinkage; Line line density deviation ratio 1.5%, fracture strength CV value 2.5%, extension at break is 17.5%, extension at break CV value 7.0%, network 6.
Embodiment 2
A preparation method for the advertising lamp box cloth polyester industrial fiber of low thermal shrinkage, main technique is:
(1) preparation of catalyst glycol magnesium:
In single-cell for electrolyzation, add ethylene glycol, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and negative electrode is graphite; Logical direct current, starting voltage 10V, cathode-current density is 200mA, electrolysis 12 hours when 60 DEG C, and electrolysis terminates rear taking-up electrode, obtains white turbid liquid; Filtration under diminished pressure, white solid absolute ethanol washing, obtains ethylene glycol magnesium after drying;
(2) preparation of polyester, comprises esterification and polycondensation reaction:
Esterification:
Adopt terephthalic acid (TPA) and ethylene glycol as raw material, the mol ratio of ethylene glycol and terephthalic acid (TPA) is 2.0:1, and add anti-ether agent calcium acetate, calcium acetate consumption is 0.05% of terephthalic acid (TPA) 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 esterification water quantity of distillate reaches 92% of theoretical value for esterification terminal;
Polycondensation reaction:
Comprise polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig:
The polycondensation reaction low vacuum stage, catalyst and stabilizing agent trimethyl phosphate is added in esterification products, trimethyl phosphate consumption is 0.02% of described terephthalic acid (TPA) weight, catalyst amount is 0.02% of terephthalic acid (TPA) quality, polycondensation reaction is started under the condition of negative pressure, this staged pressure is steadily evacuated to absolute pressure 495Pa by normal pressure, and temperature controls at 265 DEG C, and the reaction time is 40 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 low vacuum stage, continues to vacuumize, makes reaction pressure be down to absolute pressure 98Pa, and reaction temperature controls at 278 DEG C, 80 minutes reaction time; Obtained polyester, obtains polyester slice through pelletizing;
(3) dissolve and wash away
Polyester slice through water with dissolve and wash away agent propyl cellosolve brew 4 hours under 125 DEG C with 0.25MPa condition, by washing, i.e. polyester slice 78 DEG C of hot water wash 12min after brew, then clean with cold water, Drying and cooling is for subsequent use, water is 100:4 with the mass ratio dissolveing and washing away agent, polyester slice and water and the ratio dissolveing and washing away agent, and namely solid-to-liquid ratio is 1:9;
(4) solid phase polycondensation:
Institute's polyester slice that obtains, by solid phase polycondensation thickening, makes the inherent viscosity of polyester slice bring up to 1.1dL/g, is high sticky section;
(5) spinning main technologic parameters:
The temperature extruded is 320 DEG C;
The wind-warm syndrome of cooling is 30 DEG C;
Stretching, heat setting process:
GR-1 speed 600m/min; Temperature is normal temperature;
GR-2 speed 1000m/min; Temperature 100 DEG C;
GR-3 speed 2300m/min; Temperature 150 DEG C;
GR-4 speed 3300m/min; Temperature 200 DEG C;
GR-5 speed 3300m/min; Temperature 200 DEG C;
GR-6 speed 3200m/min; Temperature 220 DEG C;
The speed of winding is 3200m/min.
The advertising lamp box cloth polyester industrial fiber of obtained low thermal shrinkage is under the test condition of 177 DEG C × 10min × 0.05cN/dtex in temperature, and the dry-hot shrinkage of fiber is 1.5%; The advertising lamp box cloth polyester industrial fiber fracture strength 7.9cN/dtex of low thermal shrinkage; Line line density deviation ratio 1.2%, fracture strength CV value 2.1%, extension at break is 14.5%, extension at break CV value 6.3%, network 8.
Embodiment 3
A preparation method for the advertising lamp box cloth polyester industrial fiber of low thermal shrinkage, main technique is:
(1) preparation of catalyst glycol magnesium:
In single-cell for electrolyzation, add ethylene glycol, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and negative electrode is graphite; Logical direct current, starting voltage 8V, cathode-current density is 160mA, electrolysis 11 hours when 56 DEG C, and electrolysis terminates rear taking-up electrode, obtains white turbid liquid; Filtration under diminished pressure, white solid absolute ethanol washing, obtains ethylene glycol magnesium after drying;
(2) preparation of polyester, comprises esterification and polycondensation reaction:
Esterification:
Adopt terephthalic acid (TPA) and ethylene glycol as raw material, the mol ratio of ethylene glycol and terephthalic acid (TPA) is 1.8:1, and add anti-ether agent sodium acetate, sodium acetate consumption is 0.03% of terephthalic acid (TPA) 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 esterification water quantity of distillate reaches 95% of theoretical value for esterification terminal;
Polycondensation reaction:
Comprise polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig:
The polycondensation reaction low vacuum stage, catalyst and stabilizing agent Trimethyl phosphite is added in esterification products, Trimethyl phosphite consumption is 0.03% of terephthalic acid (TPA) weight, catalyst amount is 0.04% of terephthalic acid (TPA) quality, polycondensation reaction is started under the condition of negative pressure, this staged pressure is steadily evacuated to absolute pressure 495Pa by normal pressure, and temperature controls at 266 DEG C, and the reaction 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 low vacuum stage, continues to vacuumize, makes reaction pressure be down to absolute pressure 99Pa, and reaction temperature controls at 277 DEG C, 70 minutes reaction time; Obtained polyester, obtains polyester slice through pelletizing;
(3) dissolve and wash away
Polyester slice through water with dissolve and wash away agent ethylene glycol monobutyl ether (EGMBE) brew 3 hours under 128 DEG C with 0.25MPa condition, by washing, i.e. polyester slice 75 DEG C of hot water wash 12min after brew, then clean with cold water, Drying and cooling is for subsequent use, water is 100:4 with the mass ratio dissolveing and washing away agent, polyester slice and water and the ratio dissolveing and washing away agent, and namely solid-to-liquid ratio is 1:8;
(4) solid phase polycondensation:
Institute's polyester slice that obtains, by solid phase polycondensation thickening, makes the inherent viscosity of polyester slice bring up to 1.2dL/g, is high sticky section;
(5) spinning main technologic parameters:
The temperature extruded is 300 DEG C;
The wind-warm syndrome of cooling is 22 DEG C;
Stretching, heat setting process:
GR-1 speed 480m/min; Temperature is normal temperature;
GR-2 speed 600m/min; Temperature 95 DEG C;
GR-3 speed 1800m/min; Temperature 120 DEG C;
GR-4 speed 2800m/min; Temperature 220 DEG C;
GR-5 speed 2800m/min; Temperature 220 DEG C;
GR-6 speed 2500m/min; Temperature 220 DEG C;
The speed of winding is 2800m/min.
The advertising lamp box cloth polyester industrial fiber of obtained low thermal shrinkage is under the test condition of 177 DEG C × 10min × 0.05cN/dtex in temperature, and the dry-hot shrinkage of fiber is 2.0%; The advertising lamp box cloth polyester industrial fiber fracture strength 8.2cN/dtex of low thermal shrinkage; Line line density deviation ratio 1.2%, fracture strength CV value 2.3%, extension at break is 16.0%, extension at break CV value 6.3%, network 4.
Embodiment 4
A preparation method for the advertising lamp box cloth polyester industrial fiber of low thermal shrinkage, main technique is:
(1) preparation of catalyst glycol magnesium:
In single-cell for electrolyzation, add ethylene glycol, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and negative electrode is graphite; Logical direct current, starting voltage 10V, cathode-current density is 150mA, electrolysis 12 hours when 50 DEG C, and electrolysis terminates rear taking-up electrode, obtains white turbid liquid; Filtration under diminished pressure, white solid absolute ethanol washing, obtains ethylene glycol magnesium after drying;
(2) preparation of polyester, comprises esterification and polycondensation reaction:
Esterification:
Adopt terephthalic acid (TPA) and ethylene glycol as raw material, the mol ratio of ethylene glycol and terephthalic acid (TPA) is 19:1, and add anti-ether agent sodium acetate, sodium acetate consumption is 0.04% of terephthalic acid (TPA) 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 258 DEG C, and esterification water quantity of distillate reaches 96% of theoretical value for esterification terminal;
Polycondensation reaction:
Comprise polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig:
The polycondensation reaction low vacuum stage, catalyst and stabilizing agent triphenyl phosphate ester is added in esterification products, triphenyl phosphate ester consumption is 0.03% of terephthalic acid (TPA) weight, catalyst amount is 0.04% of terephthalic acid (TPA) quality, polycondensation reaction is started under the condition of negative pressure, this staged pressure is steadily evacuated to absolute pressure 495Pa by normal pressure, and temperature controls at 265 DEG C, and the reaction 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 3:1;
Polycondensation reaction high vacuum stage of Fig, after the polycondensation reaction low vacuum stage, continues to vacuumize, makes reaction pressure be down to absolute pressure 98Pa, and reaction temperature controls at 277 DEG C, 70 minutes reaction time; Obtained polyester, obtains polyester slice through pelletizing;
(3) dissolve and wash away
Polyester slice through water with dissolve and wash away agent ethylene glycol monoethyl ether brew 5 hours under 120 DEG C with 0.3MPa condition, by washing, i.e. polyester slice 72 DEG C of hot water wash 12min after brew, then clean with cold water, Drying and cooling is for subsequent use, water is 100:4 with the mass ratio dissolveing and washing away agent, polyester slice and water and the ratio dissolveing and washing away agent, and namely solid-to-liquid ratio is 1:8;
(4) solid phase polycondensation:
Institute's polyester slice that obtains, by solid phase polycondensation thickening, makes the inherent viscosity of polyester slice bring up to 1.2dL/g, is high sticky section;
(5) spinning main technologic parameters:
The temperature extruded is 295 DEG C;
The wind-warm syndrome of cooling is 28 DEG C;
Stretching, heat setting process:
GR-1 speed 600m/min; Temperature is normal temperature;
GR-2 speed 500m/min; Temperature 100 DEG C;
GR-3 speed 1700m/min; Temperature 150 DEG C;
GR-4 speed 2500m/min; Temperature 200 DEG C;
GR-5 speed 3300m/min; Temperature 200 DEG C;
GR-6 speed 3200m/min; Temperature 220 DEG C;
The speed of winding is 2500m/min.
The advertising lamp box cloth polyester industrial fiber of obtained low thermal shrinkage is under the test condition of 177 DEG C × 10min × 0.05cN/dtex in temperature, and the dry-hot shrinkage of fiber is 1.8%; The advertising lamp box cloth polyester industrial fiber fracture strength 8.2cN/dtex of low thermal shrinkage; Line line density deviation ratio 1.3%, fracture strength CV value 1.9%, extension at break is 16.0%, extension at break CV value 6.3%, network 4.
Claims (10)
1. the advertising lamp box cloth polyester industrial fiber of a low thermal shrinkage, it is characterized in that: the advertising lamp box cloth polyester industrial fiber of described low thermal shrinkage by polyester through dissolve and wash away with solid-phase tack producing after spinning and obtaining, the advertising lamp box cloth polyester industrial fiber of described low thermal shrinkage is under the test condition of 177 DEG C × 10min × 0.05cN/dtex in temperature, and the dry-hot shrinkage of fiber is 2.0 ± 0.5%; The advertising lamp box cloth polyester industrial fiber fracture strength >=7.5cN/dtex of described low thermal shrinkage; The polycondensation that is terephthalic acid (TPA) and ethylene glycol under esterification and the mixture through catalytic effect at ethylene glycol magnesium and antimony glycol of described polyester is also obtained after granulation;
In the section of described polyester, content of carboxyl end group is less than 15mol/t, and oligomer mass percentage content is less than 0.5%, and the mass percentage content of diethylene glycol (DEG) is less than 0.5%;
The molecular formula of described ethylene glycol magnesium is Mg (OCH
2cH
2oH)
2;
Described dissolve and wash away the section after referring to granulation through water with dissolve and wash away agent 120 ~ 130 DEG C with 0.2 ~ 0.3MPa condition under brew and washing.
2. the advertising lamp box cloth polyester industrial fiber of a kind of low thermal shrinkage according to claim 1, it is characterized in that, line line density deviation ratio≤1.5% of the advertising lamp box cloth industrial yarn of described low thermal shrinkage, fracture strength CV value≤2.5%, extension at break is 16.0 ± 1.5%, extension at break CV value≤7.0%, network 6 ± 2.
3. the advertising lamp box cloth polyester industrial fiber of a kind of low thermal shrinkage according to claim 1, is characterized 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 the advertising lamp box cloth polyester industrial fiber of a kind of low thermal shrinkage according to any one of claims 1 to 3, it is characterized in that: the polycondensation under esterification and the mixture through catalytic effect at ethylene glycol magnesium and antimony glycol of terephthalic acid (TPA) and ethylene glycol obtains polyester, then obtains polyester slice through pelletizing; Then by dissolveing and washing away and solid phase polycondensation thickening; Again through measuring, extruding, cool, oil, stretch, HEAT SETTING and winding, the advertising lamp box cloth polyester industrial fiber of obtained low thermal shrinkage.
5. the preparation method of the advertising lamp box cloth polyester industrial fiber of a kind of low thermal shrinkage according to claim 4, is characterized in that: main technique is:
(1) preparation of catalyst glycol magnesium:
In single-cell for electrolyzation, add ethylene glycol, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and negative electrode is graphite; Logical direct current, starting voltage 6 ~ 10V, cathode-current density is 150 ~ 200mA, electrolysis 10 ~ 12 hours when 50 ~ 60 DEG C, and electrolysis terminates rear taking-up electrode, obtains white turbid liquid; Filtration under diminished pressure, white solid absolute ethanol washing, obtains ethylene glycol magnesium after drying;
(2) preparation of polyester, comprises esterification and polycondensation reaction:
Described esterification:
Adopt terephthalic acid (TPA) 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 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; 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 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 polyester, obtains polyester slice through pelletizing;
(3) dissolve and wash away
Described polyester slice is through water and dissolve and wash away agent brew 3-5 hour under 120 ~ 130 DEG C with 0.2 ~ 0.3MPa condition, by washing;
(4) solid phase polycondensation:
Institute's polyester slice that obtains, by solid phase polycondensation thickening, makes the inherent viscosity of polyester slice bring up to 1.0 ~ 1.2dL/g, is high sticky section;
(5) spinning main technologic parameters:
The described temperature extruded is 290 ~ 320 DEG C;
The wind-warm syndrome of described cooling is 20 ~ 30 DEG C;
Described stretching, heat setting process:
GR-1 speed 450 ~ 600m/min; Temperature is normal temperature;
GR-2 speed 500 ~ 1000m/min; Temperature 85 ~ 100 DEG C;
GR-3 speed 1700 ~ 2300m/min; Temperature 100 ~ 150 DEG C;
GR-4 speed 2500 ~ 3300m/min; Temperature 200 ~ 250 DEG C;
GR-5 speed 2500 ~ 3300m/min; Temperature 200 ~ 250 DEG C;
GR-6 speed 2300 ~ 3200m/min; Temperature 150 ~ 220 DEG C;
The speed of described winding is 2300 ~ 3200m/min.
6. the preparation method of the advertising lamp box cloth polyester industrial fiber of a kind of low thermal shrinkage according to claim 4 or 5, is characterized in that, the mol ratio of described ethylene glycol and described terephthalic acid (TPA) is 1.2 ~ 2.0:1.
7. the preparation method of the advertising lamp box cloth polyester industrial fiber of a kind of low thermal shrinkage according to claim 5, is characterized 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 0.01% ~ 0.05% of described terephthalic acid (TPA) quality; 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 the advertising lamp box cloth polyester industrial fiber of a kind of low thermal shrinkage according to claim 5, it is characterized 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, and namely solid-to-liquid ratio is 1:5 ~ 10; It is described that to dissolve and wash away agent be one in ethylene glycol monoethyl ether, propyl cellosolve and ethylene glycol monobutyl ether (EGMBE).
9. the preparation method of the advertising lamp box cloth polyester industrial fiber of a kind of low thermal shrinkage according to claim 5, it is characterized in that, described washing refers to polyester slice 70 ~ 80 DEG C of hot water wash 10 ~ 15min after brew, and then clean with cold water, Drying and cooling is for subsequent use.
10. the preparation method of the advertising lamp box cloth polyester industrial fiber of a kind of low thermal shrinkage according to claim 5, it is characterized in that, described anti-ether agent is the one in sodium acetate and calcium acetate, and anti-ether agent consumption is 0.01% ~ 0.05% of described terephthalic acid (TPA) weight.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017113955A1 (en) * | 2015-12-29 | 2017-07-06 | 江苏恒力化纤股份有限公司 | Ultra-low shrinkage polyester industrial yarn and preparation method thereof |
| WO2017113622A1 (en) * | 2015-12-29 | 2017-07-06 | 江苏恒力化纤股份有限公司 | High-modulus low-shrinkage polyester industrial yarn and preparation method therefor |
| CN108822499A (en) * | 2018-05-25 | 2018-11-16 | 合肥大麦灯箱器材有限公司 | A kind of PVC material and preparation method thereof for lamp house cloth production |
| CN109750380A (en) * | 2018-12-27 | 2019-05-14 | 江苏恒力化纤股份有限公司 | The preparation method of terylene lamp box advertisement cloth |
Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594660A (en) * | 2004-07-05 | 2005-03-16 | 苏州大学 | Process for synthesizing glycol antimony |
| CN102797055A (en) * | 2012-09-03 | 2012-11-28 | 江苏恒力化纤股份有限公司 | Manufacturing method for low-shrinkage high-strength PET industrial yarn |
| CN102797056A (en) * | 2012-09-03 | 2012-11-28 | 江苏恒力化纤股份有限公司 | Manufacturing method for superlow shrinkage type PET industrial yarn |
| CN102797057A (en) * | 2012-09-03 | 2012-11-28 | 江苏恒力化纤股份有限公司 | Manufacturing method for high-modulus low-shrinkage PET industrial yarn |
| CN103556285A (en) * | 2013-10-14 | 2014-02-05 | 江苏恒力化纤股份有限公司 | Creep-resistant polyester ultralow-shrinkage industrial yarn and its preparation method |
-
2015
- 2015-12-29 CN CN201511018037.8A patent/CN105483853B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1594660A (en) * | 2004-07-05 | 2005-03-16 | 苏州大学 | Process for synthesizing glycol antimony |
| CN102797055A (en) * | 2012-09-03 | 2012-11-28 | 江苏恒力化纤股份有限公司 | Manufacturing method for low-shrinkage high-strength PET industrial yarn |
| CN102797056A (en) * | 2012-09-03 | 2012-11-28 | 江苏恒力化纤股份有限公司 | Manufacturing method for superlow shrinkage type PET industrial yarn |
| CN102797057A (en) * | 2012-09-03 | 2012-11-28 | 江苏恒力化纤股份有限公司 | Manufacturing method for high-modulus low-shrinkage PET industrial yarn |
| CN103556285A (en) * | 2013-10-14 | 2014-02-05 | 江苏恒力化纤股份有限公司 | Creep-resistant polyester ultralow-shrinkage industrial yarn and its preparation method |
Non-Patent Citations (2)
| Title |
|---|
| 聚酯中齐聚物的表征及控制方法研究: "魏文良", 《中国博士学位论文全文数据库（电子期刊） 工程科技I辑》 * |
| 魏家瑞: "《热塑性聚酯及其应用》", 31 January 2012, 化学工业出版社 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017113955A1 (en) * | 2015-12-29 | 2017-07-06 | 江苏恒力化纤股份有限公司 | Ultra-low shrinkage polyester industrial yarn and preparation method thereof |
| WO2017113622A1 (en) * | 2015-12-29 | 2017-07-06 | 江苏恒力化纤股份有限公司 | High-modulus low-shrinkage polyester industrial yarn and preparation method therefor |
| US10041192B1 (en) | 2015-12-29 | 2018-08-07 | Jiangsu Hengli Chemical Fibre Co., Ltd. | Ultra-low shrinkage polyester industrial yarn and its preparation method |
| CN108822499A (en) * | 2018-05-25 | 2018-11-16 | 合肥大麦灯箱器材有限公司 | A kind of PVC material and preparation method thereof for lamp house cloth production |
| CN109750380A (en) * | 2018-12-27 | 2019-05-14 | 江苏恒力化纤股份有限公司 | The preparation method of terylene lamp box advertisement cloth |
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