CN105483853B - A kind of advertising lamp box cloth polyester industrial fiber of low thermal shrinkage and preparation method thereof - Google Patents
A kind of advertising lamp box cloth polyester industrial fiber of low thermal shrinkage and preparation method thereof Download PDFInfo
- Publication number
- CN105483853B CN105483853B CN201511018037.8A CN201511018037A CN105483853B CN 105483853 B CN105483853 B CN 105483853B CN 201511018037 A CN201511018037 A CN 201511018037A CN 105483853 B CN105483853 B CN 105483853B
- Authority
- CN
- China
- Prior art keywords
- polyester
- ethylene glycol
- lamp box
- low thermal
- advertising lamp
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Classifications
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Textile Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The present invention relates to advertising lamp box cloth polyester industrial fiber of a kind of low thermal shrinkage and preparation method thereof, the advertising lamp box cloth of the low thermal shrinkage is dissolved and washed away with polyester industrial fiber by polyester, after solid-phase tack producing spinning and obtain, the advertising lamp box cloth polyester industrial fiber of the low thermal shrinkage is in temperature under 177 DEG C × 10min × 0.05cN/dtex test condition, the dry-hot shrinkage of fiber is 2.0 ± 0.5%；The advertising lamp box cloth of low thermal shrinkage polyester industrial fiber fracture strength >=7.5cN/dtex；Polycondensation catalyst is used as using ethylene glycol magnesium and antimony glycol mixture, its thermal degradation coefficient very little, oligomer is reduced in polymerization process, the reduction of thermal degradation in process, greatly reduce the impurity in polyester, the amount of nucleator in polyester is also reduced simultaneously, the probability of homogeneous nucleation is added on the basis of heterogeneous nucleation is reduced, the content that reduce further oligomer is dissolved and washed away, is conducive to growing up and crystallizing integrity optimization for crystallite dimension in the advertising lamp box cloth polyester industrial silk fiber of low thermal shrinkage.
Description
Technical field
The invention belongs to polyester industrial fiber preparing technical field, it is related to a kind of advertising lamp box cloth polyester industrial of low thermal shrinkage
Silk and preparation method thereof, particularly a kind of polycondensation catalyst is using ethylene glycol magnesium and the mixture and polyester slice of antimony glycol
Through water with dissolveing and washing away agent at 120~130 DEG C, the advertising lamp of brew, the polyester of washing and low thermal shrinkage under the conditions of 0.2~0.3MPa
Case cloth polyester industrial fiber and preparation method thereof.
Background technology
Polyethylene terephthalate (PET) is a kind of polymer of function admirable, PET so that its modulus is high, intensity is high,
Well-pressed, conformality is good, pure hygienic, barrier property is good etc., is widely used in the fields such as fiber, bottle packaging, film and sheet material,
Yield cumulative year after year, position in industry is obviously improved.
Pet Industrial Fiber is primarily referred to as mostly being applied to industry, national defence, medical treatment, environmental protection and most advanced branches of science each side
Face, is with relatively special physicalchemical structure, performance and purposes, or the chemical fibre with specific function, major embodiment
Being able to bear strong corrosion, low abrasion, high temperature resistant, radiation hardness, fire-retardant, fire-resistant, high voltage withstanding, high strength and modulus and plurality of medical work(
Energy.The PVC shelter cloths produced using high-strength low-shrinkage polyester industrial filament yarn as raw material are strong with higher peel strength and tear
Degree, makes shelter cloth be applied to various uses, flexible body advertising lamp box material, inflatable structure material, fluffy lid architectural fabrics sunshade account
Paulin etc..Obtained by main textile material of high-strength low-shrinkage industrial yarn in terms of the military supplies such as special protective garment, camouflage, covering, knapsack
To application.There is light, soft, high-strength, wear-resisting, anticorrosive, non-conductive, damping as one kind of earth working material.Make
Used time safe ready, efficiency high, and lifting object will not be damaged.The application field of Pet Industrial Fiber, which is expanded, drives application
No matter the whole competitiveness lifting in field, mitigating the weight of composite, the durability used and reduction are repaired, raise cost
Etc. all many-sides, polyesters high-performance fiber has increasingly given play to its synthetic competitive advantages.Following many decades, high-performance polyester
The development of fiber not only has considerable progress in quantity, more in the expansion of application field and carrying for industrial chain whole competitiveness
Go up the substantial effect of acquirement.
The Main way that high intensity, high-modulus, lower shrinkage, dimensional stability, functionalization develop Pet Industrial Fiber,
And influence fiber quality be polyester macromolecule collection state structure, be mainly concerned with the active force between polyester molecule, the shape of crystallization
State and structure, orientation structure etc., and the form and structure that crystallize are emphasis therein.
End carboxyl, oligomer, diethylene glycol (DEG) (DEG) content are the important quality index of polyester slice, wherein oligomer, two sweet
Alcohol is all oligomer, and they not only reflect the quality of production status, also affects the product quality of spinning processing.Therefore,
Reducing the end carboxyl in polyester slice, oligomer, diethylene glycol content just turns into the critically important link of raising polyester product quality.End
Influence of the carboxyl to polymer performance is not allowed not regard, and only control polyester content of carboxyl end group is stable in production, could stablize
Control the homogeneity of its relative molecular mass distribution.Content of the diethylene glycol (DEG) in polyester slice be in production of polyester one it is critically important
Quality index.Because it directly influences the fusing point of polyester slice, the fusing point of polyester slice can with wherein DEG content increasing
Urgent acute decline, so it not only reflects the quality of production status, directly influences the matter of post-processing-spinning technique and silk
Amount.Oligomer in polyester refers to the oligomer that the degree of polymerization is less than 10, is divided into linear oligomerization thing and cyclic oligomer, wherein with ring
Shape aggressiveness particularly cyclic trimer is in the majority, and oligomer is mainly concerned with heterogeneous nucleation, spinning processing etc., performance to polyester and
Road processing afterwards causes certain harmful effect.It is particularly significant in polyester production process to control content of the three in polyester slice
Problem.
The content of the invention
It is an object of the invention to provide advertising lamp box cloth polyester industrial fiber of a kind of low thermal shrinkage and preparation method thereof, it is
A kind of polycondensation catalyst is used using the advertising lamp box cloth of the polyester and low thermal shrinkage of ethylene glycol magnesium and the mixture of antimony glycol
Polyester industrial fiber and preparation method thereof.The advertising lamp box cloth polyester industrial fiber of the low thermal shrinkage temperature be 177 DEG C ×
Under 10min × 0.05cN/dtex test condition, the dry-hot shrinkage of fiber is 2.0 ± 0.5%；The low thermal shrinkage it is wide
Accuse lamp house cloth polyester industrial fiber fracture strength >=7.5cN/dtex；The present invention is using ethylene glycol magnesium and the mixture of antimony glycol
For polycondensation catalyst, thermal degradation is reduced to minimum, and polyester slice is through water and dissolves and washes away agent at 130 DEG C, under the conditions of 0.3MPa
Brew, washing；Reduce the influence that end carboxyl, oligomer, diethylene glycol content are processed to Direct-spinning of PET Fiber.
The present invention a kind of low thermal shrinkage advertising lamp box cloth polyester industrial fiber, be the polyester be terephthalic acid (TPA) and
Ethylene glycol through esterification and ethylene glycol magnesium and antimony glycol mixture through catalytic effect under polycondensation, granulate and dissolve and wash away, solid-phase tack producing
Afterwards spinning and obtain；
In the section of the industry polyester, content of carboxyl end group is less than 15mol/t, and oligomer mass percentage content is less than
0.5%, the mass percentage content of diethylene glycol (DEG) is less than 0.5%；
The molecular formula of the ethylene glycol magnesium is Mg (OCH2CH2OH)2；
Described dissolve and wash away refers to that the section after granulation is boiled through water with dissolveing and washing away agent under the conditions of 120~130 DEG C with 0.2~0.3MPa
Bubble and
Washing.
The Main way that high intensity, high-modulus, lower shrinkage, dimensional stability, functionalization develop Pet Industrial Fiber,
And influence fiber quality be polyester macromolecule collection state structure, be mainly concerned with the active force between polyester molecule, the shape of crystallization
State and structure, orientation structure etc., and the form and structure that crystallize are emphasis therein.
Lower shrinkage, dimensional stability are to influence the principal element of high-quality polyester, macroscopical thermal contraction phenomenon of polyester fiber
It is the Entropy Changes trend because local elongation macromolecular chain, develops the internal stress produced to rolled state and spinning process is freezed
Axial internal stress in the sample, this local internal stress can be relayed to whole material by molecule web frame, when the external world provides foot
During enough heat energy, the phenomenon of generation.
Polyester fiber belongs to orientation hypocrystalline high polymer material, is made up of the different construction unit of orientation stability：(1)
The crystalline portion of high stable and high integrity degree；(2) the imperfection crystalline portion of relatively low stability；(3) knot of low stability
Transition zone between brilliant and amorphous；(4) unstable orientation amorphous phase.When polyester fiber is heated, it may occur however that following situation：
The amorphous phase of orientation occurs retraction and crystallized；The destruction of imperfection crystalline portion be recrystallized with possible：The thickening of crystal grain or
Crystal grain is melted completely.Illustrate that crystallite dimension and crystallization degree of perfection are the key factors for ensureing fiber high temperature dimensional stability.177
DEG C percent thermal shrinkage it is low be the splendid fiber of thermal dimensional stability, with two design features：Crystallite dimension is big and crystallizes perfect
Property is good.Therefore the crystallite dimension of fiber is big and crystallization integrity is good, is the guarantee of low shrinkage fibre quality.
The factor of influence crystallizing polyester mainly has：(1) structure of strand in itself.(2) selection of crystallization temperature.(3) divide
The influence of son amount.(4) application of nucleator.(5) be exactly finally process conditions influence.Wherein nucleation is that crystallization process is main
A critically important ring nucleator is that can accelerate the progress of crystallization to a certain extent in link, while to low-shrinkage polyester industrial
Silk more importantly influences the size and crystallization integrity of crystallization.
Determining terminal carboxy group in PET is high, and the heat endurance of polyester resin is poor, while polyester and gathering that carboxylic acid reactant salt is generated
The carboxylate of ester large molecule chain, consists of nucleus, polyester is accelerated heterogeneous nucleation.The oligomer containing 3-4%, more in polyester
Exist in the form of low molecular ether and ester, mainly based on cyclic trimer oligomer, diethylene glycol (DEG), product of the oligomer to polyester
Matter influence is larger, and crystallization nucleation mechanism, crystallinity, crystal habit and the crystallization of polyester are mainly influenceed in the way of nucleator
The percent thermal shrinkage of integrality etc. and then the quality, particularly polyester industrial fiber of influence polyester fiber.Pure polyester without diethylene glycol (DEG),
No matter how crystallization condition changes, all without the form for abnormal spherocrystal occur；And when containing diethylene glycol (DEG) in sample, meeting in crystalline region
There is the form that normal and abnormal spherocrystal coexists, and with the increase of diethylene glycol content, abnormal spherocrystal is in whole form
Ratio rises, thus has influence on the integrality of crystallization, and making the crystallization integrity of its polyester reduces.Cyclic trimer more than the polyester with
The mode of nucleation occurs, and nucleator is more, and crystallization rate is fast, and crystal grain quantity is big, but crystallite dimension is smaller, and then has influence on crystallization
Integrity.The increase of heterogeneous nucleation so that high stable and the crystalline portion of high integrity degree are reduced, relatively low stability it is endless
Kind transition zone between crystalline portion and the crystallization of low stability and amorphous is increased, and the thermal contraction to polyester fiber produces bad shadow
Ring.
A kind of advertising lamp box cloth polyester industrial fiber of low thermal shrinkage as described above, the advertising lamp box of the low thermal shrinkage
Line line density deviation ratio≤1.5% of cloth industrial yarn, fracture strength CV value≤2.5%, extension at break is 16.0 ± 1.5%,
Extension at break CV value≤7.0%, network 6 ± 2.
A kind of advertising lamp box cloth polyester industrial fiber of low thermal shrinkage as described above, the ethylene glycol magnesium and antimony glycol
Mixture in, ethylene glycol magnesium and antimony glycol mass ratio are 2~3:1.
Present invention also offers a kind of preparation method of the advertising lamp box cloth polyester industrial fiber of low thermal shrinkage, for benzene two
Polyester is made in polycondensation through esterification and in the case where the mixture through catalytic of ethylene glycol magnesium and antimony glycol is acted on for formic acid and ethylene glycol, then through cutting
Grain obtain polyester slice, then by dissolveing and washing away, solid phase polycondensation thickening；Again through measuring, extruding, cool down, oil, stretch, thermal finalization,
Winding, is made heat-resistance polyester industrial yarn.
A kind of preparation method of the advertising lamp box cloth polyester industrial fiber of low thermal shrinkage as described above, main technique is：
(1) preparation of catalyst glycol magnesium：
Add ethylene glycol in single-cell for electrolyzation, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and negative electrode is graphite；
Logical direct current, 6~10VV of starting voltage, cathode-current density is 150~200mA, is electrolysed 10~12 hours at 50~60 DEG C, electricity
Solution takes out electrode after terminating, and obtains white suspension；It is filtered under diminished pressure, white solid is washed with absolute ethyl alcohol, second two is obtained after drying
Magnesium alkoxide；
(2) preparation of polyester, including esterification and polycondensation reaction：
The esterification：
Using terephthalic acid (TPA) and ethylene glycol as raw material, anti-ether agent is added, is made into after uniform sizing material and carries out esterification,
Obtain esterification products；Esterification is pressurizeed in nitrogen atmosphere, and Stress control is in normal pressure~0.3MPa, and temperature is 250~260
DEG C, esterification water quantity of distillate reaches that more than the 90% of theoretical value is esterification terminal；
The polycondensation reaction：
Including polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig：
The polycondensation reaction low vacuum stage, catalyst and stabilizer are added in esterification products, under conditions of negative pressure
Start polycondensation reaction, the staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, temperature control at 260~270 DEG C,
Reaction time is 30~50 minutes；The catalyst is the mixture of ethylene glycol magnesium and antimony glycol；
The polycondensation reaction high vacuum stage of Fig, after the polycondensation reaction low vacuum stage, continues to vacuumize, makes reaction pressure
Power is down to absolute pressure less than 100Pa, and reaction temperature is controlled in 275~280 DEG C, 50~90 minutes reaction time；
Polyester is made, polyester slice is obtained through pelletizing；
(3) dissolve and wash away
The polyester slice is through water and dissolves and washes away agent brew 3-5 hours under the conditions of 120~130 DEG C with 0.2~0.3MPa, after
It is scrubbed；
(4) solid phase polycondensation：
Resulting polyester slice is viscosified by solid phase polycondensation, the inherent viscosity of polyester slice is brought up to 1.0~1.2dL/
G, is high viscous section；
(5) spinning main technologic parameters：
The temperature of the extrusion is 290~320 DEG C；
The wind-warm syndrome of the cooling is 20~30 DEG C；
Described stretching, heat setting process：
450~600m/min of GR-1 speed；Temperature is normal temperature；
500~1000m/min of GR-2 speed；85~100 DEG C of temperature；
1700~2300m/min of GR-3 speed；100~150 DEG C of temperature；
2500~3300m/min of GR-4 speed；200~250 DEG C of temperature；
2500~3300m/min of GR-5 speed；200~250 DEG C of temperature；
2300~3200m/min of GR-6 speed；150~220 DEG C of temperature；
The speed of the winding is 2300~3200m/min.
A kind of preparation method of the advertising lamp box cloth polyester industrial fiber of low thermal shrinkage as described above, the ethylene glycol with
The mol ratio of the terephthalic acid (TPA) is 1.2~2.0:1.
A kind of preparation method of the advertising lamp box cloth polyester industrial fiber of low thermal shrinkage as described above, the ethylene glycol magnesium
In the mixture of antimony glycol, ethylene glycol magnesium is 2~3 with antimony glycol mass ratio:1；The catalyst amount is described right
The 0.01%~0.05% of phthalic acid quality.
Using ethylene glycol magnesium and antimony glycol mixture as polycondensation catalyst, ethylene glycol magnesium belongs to comparatively gentle one
Class, its thermal degradation coefficient very little, the side reaction triggered during the course of the reaction is less, reduces end carboxyl in process and low
The generation of polymers.The principal element for causing thermal degradation is high temperature and catalyst, and high temperature is that response intensity is too high, causes degraded to add
Speed, generates end carboxyl, while also increasing cyclic oligomer；Catalyst is then related to the degradation reaction constant of catalyst,
In polycondensation process, the effect of catalyst, which is not only in that, can be catalyzed generation main reaction, so as to influence the speed and yield of reaction, simultaneously
Thermal degradation and ehter bond generation can also be catalyzed, increases the content of diethylene glycol (DEG), so as to increase the content of end carboxyl.
A kind of preparation method of the advertising lamp box cloth polyester industrial fiber of low thermal shrinkage as described above, the stabilizer choosing
One kind from triphenyl phosphate, trimethyl phosphate and Trimethyl phosphite, stabilizing agent dosage is the terephthalic acid (TPA) weight
0.01%~0.05%.Stabilizer is main based on phosphate, and main function is catching reaction generation in the course of the polymerization process
Free radical, reduces side reaction.
A kind of preparation method of the advertising lamp box cloth polyester industrial fiber of low thermal shrinkage as described above, the water is with dissolveing and washing away
The mass ratio of agent is 100:3~4, polyester slice and water and the ratio for dissolveing and washing away agent, i.e. solid-to-liquid ratio are 1:5-10；It is described to dissolve and wash away agent
For one kind in ethylene glycol monoethyl ether, propyl cellosolve and ethylene glycol monobutyl ether (EGMBE), what addition was a small amount of in water dissolves and washes away agent, dissolves and washes away
Agent is dissolved in water, while also can dissolve most of low molecular ethers and ester, is conducive to improving the reduction of the effect washed and oligomer.
A kind of preparation method of the advertising lamp box cloth polyester industrial fiber of low thermal shrinkage as described above, the washing refers to
Then polyester slice is cleaned, Drying and cooling is standby with 70~80 DEG C of 10~15min of hot water wash with cold water after brew.
A kind of preparation method of the advertising lamp box cloth polyester industrial fiber of low thermal shrinkage as described above, the anti-ether agent is
One kind in sodium acetate and calcium acetate, anti-ether agent consumption is the 0.01%~0.05% of the terephthalic acid (TPA) weight.Anti- ether agent
The generation of ether in acid condition is reduced by adding a small amount of NaAc, so as to reduce the work that glycol reaction generates diethylene glycol (DEG)
Property.
It is an object of the invention to provide a kind of advertising lamp box cloth polyester industrial fiber of low thermal shrinkage, using relatively mild one
Class polycondensation catalyst ethylene glycol magnesium, the less side reaction triggered during the course of the reaction is less and process in less heat drop
Solution, reduces the generation of oligomer in process.Polyester slice is through water and dissolves and washes away agent at 130 DEG C, is boiled under the conditions of 0.3MPa
Bubble is conducive to improving the reduction of the effect washed and oligomer.Oligomer is reduced in polymerization process, thermal degradation in process
Reduction, greatly reduces the impurity in polyester, while also reducing the amount of nucleator in polyester, is reducing the base of heterogeneous nucleation
The probability of homogeneous nucleation is added on plinth, is conducive to crystal grain chi of the advertising lamp box cloth in polyester industrial silk fiber of low thermal shrinkage
Very little growing up and crystallize integrity optimizes.
Beneficial effect：
● using ethylene glycol magnesium with antimony glycol mixture as polycondensation catalyst, ethylene glycol magnesium belongs to comparatively gentle one
Class, its thermal degradation coefficient very little, the side reaction triggered during the course of the reaction is less, reduces end carboxyl in process and low
The generation of polymers.
● 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 two is sweet
The mass percentage content of alcohol is less than 0.5%, is conducive to further improving the quality of fiber.
● polyester slice is conducive to raising to wash through water with dissolveing and washing away agent brew under the conditions of 120~130 DEG C with 0.2~0.3MPa
The effect washed and the reduction of oligomer.
● anti-ether agent reduces the generation of ether in acid condition by adding a small amount of NaAc, so as to reduce glycol reaction
Generate the activity of diethylene glycol (DEG).
● oligomer is reduced in polymerization process, and the reduction of thermal degradation, is greatly reduced miscellaneous in polyester in process
Matter, while also reducing the amount of nucleator in polyester, the probability of homogeneous nucleation is added on the basis of heterogeneous nucleation is reduced, is had
Beneficial in the advertising lamp box cloth polyester industrial silk fiber of low thermal shrinkage crystallite dimension grow up and crystallize integrity optimization.
Embodiment
The invention will be further elucidated with reference to specific embodiments.It should be understood that these embodiments are merely to illustrate this hair
Bright rather than limitation the scope of the present invention.In addition, it is to be understood that after the content of the invention lectured has been read, art technology
Personnel can make various changes or modifications to the present invention, and these equivalent form of values equally fall within the application appended claims and limited
Fixed scope.
A kind of preparation method of the advertising lamp box cloth polyester industrial fiber of low thermal shrinkage of the present invention, terephthalic acid (TPA) and second
Through esterification and under the mixture through catalytic effect of ethylene glycol magnesium and antimony glycol, polyester is made in polycondensation to glycol, then is gathered through pelletizing
Ester is cut into slices；Then viscosified by dissolveing and washing away with solid phase polycondensation；Again through measuring, extruding, cool down, oil, stretch, thermal finalization and winding,
The advertising lamp box cloth polyester industrial fiber of low thermal shrinkage is made
Embodiment 1
A kind of preparation method of the advertising lamp box cloth polyester industrial fiber of low thermal shrinkage, main technique is：
(1) preparation of catalyst glycol magnesium：
Ethylene glycol is added in single-cell for electrolyzation, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and negative electrode is stone
Ink；Logical direct current, starting voltage 6V, cathode-current density is 150mA, is electrolysed 10 hours at 50 DEG C, and electrolysis takes out electricity after terminating
Pole, obtains white suspension；It is filtered under diminished pressure, white solid is washed with absolute ethyl alcohol, ethylene glycol magnesium is obtained after drying；
(2) preparation of polyester, including esterification and polycondensation reaction：
Esterification：
Using terephthalic acid (TPA) and ethylene glycol as raw material, the mol ratio of ethylene glycol and terephthalic acid (TPA) is 1.2:1, add
Anti- ether agent sodium acetate, sodium acetate consumption is the 0.01% of terephthalic acid (TPA) weight, is made into after uniform sizing material and carries out esterification, obtains
To esterification products；Esterification is pressurizeed in nitrogen atmosphere, and Stress control is in normal pressure, and temperature is at 250 DEG C, and esterification water quantity of distillate reaches
It is esterification terminal to the 91% of theoretical value；
Polycondensation reaction：
Including polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig：
The polycondensation reaction low vacuum stage, catalyst and stabilizer triphenyl phosphate ester, triphenyl phosphate are added in esterification products
Ester consumption is the 0.01% of terephthalic acid (TPA) weight, and catalyst amount is the 0.01% of terephthalic acid (TPA) quality, in the bar of negative pressure
Start polycondensation reaction under part, the staged pressure is steadily evacuated to absolute pressure 498Pa by normal pressure, and temperature control is at 260 DEG C, during reaction
Between be 30 minutes；Catalyst is the mixture of ethylene glycol magnesium and antimony glycol, and ethylene glycol magnesium is 2 with antimony glycol mass ratio:1；
Polycondensation reaction high vacuum stage of Fig, after the polycondensation reaction low vacuum stage, continues to vacuumize, drops reaction pressure
To absolute pressure 98Pa, reaction temperature is controlled in 275 DEG C, 50 minutes reaction time；Polyester is made, obtains polyester through pelletizing and cuts
Piece；
(3) dissolve and wash away
Polyester slice is through water and dissolves and washes away agent ethylene glycol monoethyl ether brew 3 hours under the conditions of 120 DEG C with 0.2MPa, by washing
Wash, i.e., then polyester slice is cleaned, Drying and cooling is standby with 70 DEG C of hot water wash 10min with cold water after brew, and water is with dissolveing and washing away agent
Mass ratio is 100:3, polyester slice and water and the ratio for dissolveing and washing away agent, i.e. solid-to-liquid ratio are 1:5；
(4) solid phase polycondensation：
Resulting polyester slice is viscosified by solid phase polycondensation, the inherent viscosity of polyester slice is brought up to 1.0dL/g, is
The viscous section of height；
(5) spinning main technologic parameters：
The temperature of extrusion 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；85 DEG C of temperature；
GR-3 speed 1700m/min；100 DEG C of temperature；
GR-4 speed 2500m/min；200 DEG C of temperature；
GR-5 speed 2500m/min；200 DEG C of temperature；
GR-6 speed 2300m/min；210 DEG C of temperature；
The speed of winding is 2300m/min.
The advertising lamp box cloth polyester industrial fiber of obtained low thermal shrinkage is 177 DEG C × 10min × 0.05cN/ in temperature
Under dtex test condition, the dry-hot shrinkage of fiber is 2.5%；The advertising lamp box cloth of low thermal shrinkage is broken with polyester industrial fiber
Intensity 7.5cN/dtex；Line line density deviation ratio 1.5%, fracture strength CV values 2.5%, extension at break is 17.5%, and fracture is stretched
Long CV values 7.0%, network 6.
Embodiment 2
A kind of preparation method of the advertising lamp box cloth polyester industrial fiber of low thermal shrinkage, main technique is：
(1) preparation of catalyst glycol magnesium：
Ethylene glycol is added in single-cell for electrolyzation, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and negative electrode is stone
Ink；Logical direct current, starting voltage 10V, cathode-current density is 200mA, is electrolysed 12 hours at 60 DEG C, and electrolysis takes out electricity after terminating
Pole, obtains white suspension；It is filtered under diminished pressure, white solid is washed with absolute ethyl alcohol, ethylene glycol magnesium is obtained after drying；
(2) preparation of polyester, including esterification and polycondensation reaction：
Esterification：
Using terephthalic acid (TPA) and ethylene glycol as raw material, the mol ratio of ethylene glycol and terephthalic acid (TPA) is 2.0:1, add
Anti- ether agent calcium acetate, calcium acetate consumption is the 0.05% of terephthalic acid (TPA) weight, is made into after uniform sizing material and carries out esterification, obtains
To esterification products；Esterification is pressurizeed in nitrogen atmosphere, and Stress control is in 0.3MPa, and temperature is in 260 DEG C, esterification water quantity of distillate
It is esterification terminal to reach the 92% of theoretical value；
Polycondensation reaction：
Including polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig：
In the polycondensation reaction low vacuum stage, catalyst and stabilizer trimethyl phosphate, tripotassium phosphate are added in esterification products
Ester consumption is the 0.02% of the terephthalic acid (TPA) weight, and catalyst amount is the 0.02% of terephthalic acid (TPA) quality, in negative pressure
Under conditions of start polycondensation reaction, the staged pressure is steadily evacuated to absolute pressure 495Pa by normal pressure, and temperature control is at 265 DEG C, instead
It is 40 minutes between seasonable；Catalyst is the mixture of ethylene glycol magnesium and antimony glycol, and ethylene glycol magnesium is with antimony glycol mass ratio
3:1；
Polycondensation reaction high vacuum stage of Fig, after the polycondensation reaction low vacuum stage, continues to vacuumize, reaction pressure is down to absolutely
To pressure 98Pa, reaction temperature is controlled in 278 DEG C, 80 minutes reaction time；Polyester is made, polyester slice is obtained through pelletizing；
(3) dissolve and wash away
Polyester slice is through water and dissolves and washes away agent propyl cellosolve brew 4 hours under the conditions of 125 DEG C with 0.25MPa, by
Washing, i.e., then polyester slice is cleaned, Drying and cooling is standby with 78 DEG C of hot water wash 12min with cold water after brew, and water is with dissolveing and washing away agent
Mass ratio be 100:4, polyester slice and water and the ratio for dissolveing and washing away agent, i.e. solid-to-liquid ratio are 1:9；
(4) solid phase polycondensation：
Resulting polyester slice is viscosified by solid phase polycondensation, the inherent viscosity of polyester slice is brought up to 1.1dL/g, is
The viscous section of height；
(5) spinning main technologic parameters：
The temperature of extrusion 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；100 DEG C of temperature；
GR-3 speed 2300m/min；150 DEG C of temperature；
GR-4 speed 3300m/min；200 DEG C of temperature；
GR-5 speed 3300m/min；200 DEG C of temperature；
GR-6 speed 3200m/min；220 DEG C of temperature；
The speed of winding is 3200m/min.
The advertising lamp box cloth polyester industrial fiber of obtained low thermal shrinkage is 177 DEG C × 10min × 0.05cN/ in temperature
Under dtex test condition, the dry-hot shrinkage of fiber is 1.5%；The advertising lamp box cloth of low thermal shrinkage is broken with polyester industrial fiber
Intensity 7.9cN/dtex；Line line density deviation ratio 1.2%, fracture strength CV values 2.1%, extension at break is 14.5%, and fracture is stretched
Long CV values 6.3%, network 8.
Embodiment 3
A kind of preparation method of the advertising lamp box cloth polyester industrial fiber of low thermal shrinkage, main technique is：
(1) preparation of catalyst glycol magnesium：
Ethylene glycol is added in single-cell for electrolyzation, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and negative electrode is stone
Ink；Logical direct current, starting voltage 8V, cathode-current density is 160mA, is electrolysed 11 hours at 56 DEG C, and electrolysis takes out electricity after terminating
Pole, obtains white suspension；It is filtered under diminished pressure, white solid is washed with absolute ethyl alcohol, ethylene glycol magnesium is obtained after drying；
(2) preparation of polyester, including esterification and polycondensation reaction：
Esterification：
Using terephthalic acid (TPA) and ethylene glycol as raw material, the mol ratio of ethylene glycol and terephthalic acid (TPA) is 1.8:1, add
Anti- ether agent sodium acetate, sodium acetate consumption is the 0.03% of terephthalic acid (TPA) weight, is made into after uniform sizing material and carries out esterification, obtains
To esterification products；Esterification is pressurizeed in nitrogen atmosphere, and Stress control is in 0.2MPa, and temperature is in 255 DEG C, esterification water quantity of distillate
It is esterification terminal to reach the 95% of theoretical value；
Polycondensation reaction：
Including polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig：
In the polycondensation reaction low vacuum stage, catalyst and stabilizer Trimethyl phosphite, phosphorous acid are added in esterification products
Trimethyl consumption is the 0.03% of terephthalic acid (TPA) weight, and catalyst amount is the 0.04% of terephthalic acid (TPA) quality, in negative pressure
Under conditions of start polycondensation reaction, the staged pressure is steadily evacuated to absolute pressure 495Pa by normal pressure, and temperature control is at 266 DEG C, instead
It is 38 minutes between seasonable；Catalyst is the mixture of ethylene glycol magnesium and antimony glycol, and ethylene glycol magnesium is with antimony glycol mass ratio
3:1；
Polycondensation reaction high vacuum stage of Fig, after the polycondensation reaction low vacuum stage, continues to vacuumize, reaction pressure is down to absolutely
To pressure 99Pa, reaction temperature is controlled in 277 DEG C, 70 minutes reaction time；Polyester is made, polyester slice is obtained through pelletizing；
(3) dissolve and wash away
Polyester slice is through water and dissolves and washes away agent ethylene glycol monobutyl ether (EGMBE) brew 3 hours under the conditions of 128 DEG C with 0.25MPa, by
Washing, i.e., then polyester slice is cleaned, Drying and cooling is standby with 75 DEG C of hot water wash 12min with cold water after brew, and water is with dissolveing and washing away agent
Mass ratio be 100:4, polyester slice and water and the ratio for dissolveing and washing away agent, i.e. solid-to-liquid ratio are 1:8；
(4) solid phase polycondensation：
Resulting polyester slice is viscosified by solid phase polycondensation, the inherent viscosity of polyester slice is brought up to 1.2dL/g, is
The viscous section of height；
(5) spinning main technologic parameters：
The temperature of extrusion 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；95 DEG C of temperature；
GR-3 speed 1800m/min；120 DEG C of temperature；
GR-4 speed 2800m/min；220 DEG C of temperature；
GR-5 speed 2800m/min；220 DEG C of temperature；
GR-6 speed 2500m/min；220 DEG C of temperature；
The speed of winding is 2800m/min.
The advertising lamp box cloth polyester industrial fiber of obtained low thermal shrinkage is 177 DEG C × 10min × 0.05cN/ in temperature
Under dtex test condition, the dry-hot shrinkage of fiber is 2.0%；The advertising lamp box cloth of low thermal shrinkage is broken with polyester industrial fiber
Intensity 8.2cN/dtex；Line line density deviation ratio 1.2%, fracture strength CV values 2.3%, extension at break is 16.0%, and fracture is stretched
Long CV values 6.3%, network 4.
Embodiment 4
A kind of preparation method of the advertising lamp box cloth polyester industrial fiber of low thermal shrinkage, main technique is：
(1) preparation of catalyst glycol magnesium：
Ethylene glycol is added in single-cell for electrolyzation, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and negative electrode is stone
Ink；Logical direct current, starting voltage 10V, cathode-current density is 150mA, is electrolysed 12 hours at 50 DEG C, and electrolysis takes out electricity after terminating
Pole, obtains white suspension；It is filtered under diminished pressure, white solid is washed with absolute ethyl alcohol, ethylene glycol magnesium is obtained after drying；
(2) preparation of polyester, including esterification and polycondensation reaction：
Esterification：
Using terephthalic acid (TPA) and ethylene glycol as raw material, the mol ratio of ethylene glycol and terephthalic acid (TPA) is 19:1, add
Anti- ether agent sodium acetate, sodium acetate consumption is the 0.04% of terephthalic acid (TPA) weight, is made into after uniform sizing material and carries out esterification, obtains
To esterification products；Esterification is pressurizeed in nitrogen atmosphere, and Stress control is in 0.2MPa, and temperature is in 258 DEG C, esterification water quantity of distillate
It is esterification terminal to reach the 96% of theoretical value；
Polycondensation reaction：
Including polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig：
In the polycondensation reaction low vacuum stage, catalyst and stabilizer triphenyl phosphate ester are added in esterification products, triphenyl phosphate ester is used
Measure as the 0.03% of terephthalic acid (TPA) weight, catalyst amount is the 0.04% of terephthalic acid (TPA) quality, under conditions of negative pressure
Start polycondensation reaction, the staged pressure is steadily evacuated to absolute pressure 495Pa by normal pressure, temperature control is 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 is 3 with antimony glycol mass ratio:1；
Polycondensation reaction high vacuum stage of Fig, after the polycondensation reaction low vacuum stage, continues to vacuumize, reaction pressure is down to absolutely
To pressure 98Pa, reaction temperature is controlled in 277 DEG C, 70 minutes reaction time；Polyester is made, polyester slice is obtained through pelletizing；
(3) dissolve and wash away
Polyester slice is through water and dissolves and washes away agent ethylene glycol monoethyl ether brew 5 hours under the conditions of 120 DEG C with 0.3MPa, by washing
Wash, i.e., then polyester slice is cleaned, Drying and cooling is standby with 72 DEG C of hot water wash 12min with cold water after brew, and water is with dissolveing and washing away agent
Mass ratio is 100:4, polyester slice and water and the ratio for dissolveing and washing away agent, i.e. solid-to-liquid ratio are 1:8；
(4) solid phase polycondensation：
Resulting polyester slice is viscosified by solid phase polycondensation, the inherent viscosity of polyester slice is brought up to 1.2dL/g, is
The viscous section of height；
(5) spinning main technologic parameters：
The temperature of extrusion 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；100 DEG C of temperature；
GR-3 speed 1700m/min；150 DEG C of temperature；
GR-4 speed 2500m/min；200 DEG C of temperature；
GR-5 speed 3300m/min；200 DEG C of temperature；
GR-6 speed 3200m/min；220 DEG C of temperature；
The speed of winding is 2500m/min.
The advertising lamp box cloth polyester industrial fiber of obtained low thermal shrinkage is 177 DEG C × 10min × 0.05cN/ in temperature
Under dtex test condition, the dry-hot shrinkage of fiber is 1.8%；The advertising lamp box cloth of low thermal shrinkage is broken with polyester industrial fiber
Intensity 8.2cN/dtex；Line line density deviation ratio 1.3%, fracture strength CV values 1.9%, extension at break is 16.0%, and fracture is stretched
Long CV values 6.3%, network 4.
Claims (9)
1. a kind of advertising lamp box cloth polyester industrial fiber of low thermal shrinkage, it is characterized in that：The advertising lamp box cloth of the low thermal shrinkage
Obtained, the advertising lamp box cloth polyester work of the low thermal shrinkage with spinning after solid-phase tack producing by polyester through dissolveing and washing away with polyester industrial fiber
Industry silk in temperature under 177 DEG C × 10min × 0.05cN/dtex test condition, the dry-hot shrinkage of fiber for 2.0 ±
0.5%；The advertising lamp box cloth of low thermal shrinkage polyester industrial fiber fracture strength >=7.5cN/dtex；The polyester is to benzene
Dioctyl phthalate and ethylene glycol polycondensation and the system after granulation through esterification and in the case where the mixture through catalytic of ethylene glycol magnesium and antimony glycol is acted on
；
In the section of the polyester, content of carboxyl end group is less than 15mol/t, and oligomer mass percentage content is less than 0.5%, and two is sweet
The mass percentage content of alcohol is less than 0.5%；
The molecular formula of the ethylene glycol magnesium is Mg (OCH2CH2OH)2；
In the mixture of the ethylene glycol magnesium and antimony glycol, ethylene glycol magnesium is 2~3 with antimony glycol mass ratio:1；
It is described dissolve and wash away refer to granulation after section through water and dissolve and wash away agent 120~130 DEG C with 0.2~0.3MPa under the conditions of 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 characterised in that described
Line line density deviation ratio≤1.5% of the advertising lamp box cloth industrial yarn of low thermal shrinkage, fracture strength CV value≤2.5%, fracture
Extend for 16.0 ± 1.5%, extension at break CV value≤7.0%, network 6 ± 2.
3. a kind of prepare such as a kind of advertising lamp box cloth polyester industrial of low thermal shrinkage according to any one of claims 1 to 2
The method of silk, it is characterized in that：Terephthalic acid (TPA) and ethylene glycol are through esterification and in ethylene glycol magnesium and the mixture through catalytic of antimony glycol
Polyester is made in the lower polycondensation of effect, then obtains polyester slice through pelletizing；Then viscosified by dissolveing and washing away with solid phase polycondensation；Again through metering,
Extrude, cool down, oiling, stretching, thermal finalization and winding, the advertising lamp box cloth polyester industrial fiber of low thermal shrinkage is made.
4. method according to claim 3, it is characterised in that：Main technique is：
(1) preparation of catalyst glycol magnesium：
Ethylene glycol is added in single-cell for electrolyzation, supporting electrolyte is magnesium chloride, and metal MAG block is anode, and negative electrode is graphite；It is logical
Direct current, 6~10V of starting voltage, cathode-current density is 150~200mA, is electrolysed 10~12 hours at 50~60 DEG C, electrolysis
Electrode is taken out after end, white suspension is obtained；It is filtered under diminished pressure, white solid is washed with absolute ethyl alcohol, ethylene glycol is obtained after drying
Magnesium；
(2) preparation of polyester, including esterification and polycondensation reaction：
The esterification：
Using terephthalic acid (TPA) and ethylene glycol as raw material, anti-ether agent is added, is made into after uniform sizing material and carries out esterification, obtain
Esterification products；Esterification is pressurizeed in nitrogen atmosphere, and Stress control is in normal pressure~0.3MPa, and temperature is in 250~260 DEG C, ester
Change water quantity of distillate and reach that more than the 90% of theoretical value is esterification terminal；
The polycondensation reaction：
Including polycondensation reaction low vacuum stage and polycondensation reaction high vacuum stage of Fig：
The polycondensation reaction low vacuum stage, catalyst and stabilizer are added in esterification products, started under conditions of negative pressure
Polycondensation reaction, the staged pressure is steadily evacuated to below absolute pressure 500Pa by normal pressure, and temperature control is at 260~270 DEG C, reaction
Time is 30~50 minutes；The catalyst is the mixture of ethylene glycol magnesium and antimony glycol；
The polycondensation reaction high vacuum stage of Fig, after the polycondensation reaction low vacuum stage, continues to vacuumize, drops reaction pressure
It is less than 100Pa to absolute pressure, reaction temperature is controlled in 275~280 DEG C, 50~90 minutes reaction time；
Polyester is made, polyester slice is obtained through pelletizing；
(3) dissolve and wash away
The polyester slice is through water and dissolves and washes away agent brew 3-5 hours under the conditions of 120~130 DEG C with 0.2~0.3MPa, by washing
Wash；
(4) solid phase polycondensation：
Resulting polyester slice is viscosified by solid phase polycondensation, the inherent viscosity of polyester slice is brought up to 1.0~1.2dL/g, i.e.,
For the viscous section of height；
(5) spinning main technologic parameters：
The temperature of the extrusion is 290~320 DEG C；
The wind-warm syndrome of the cooling is 20~30 DEG C；
Described stretching, heat setting process：
450~600m/min of GR-1 speed；Temperature is normal temperature；
500~1000m/min of GR-2 speed；85~100 DEG C of temperature；
1700~2300m/min of GR-3 speed；100~150 DEG C of temperature；
2500~3300m/min of GR-4 speed；200~250 DEG C of temperature；
2500~3300m/min of GR-5 speed；200~250 DEG C of temperature；
2300~3200m/min of GR-6 speed；150~220 DEG C of temperature；
The speed of the winding is 2300~3200m/min.
5. the method according to claim 3 or 4, it is characterised in that mole of the ethylene glycol and the terephthalic acid (TPA)
Than for 1.2~2.0:1.
6. method according to claim 4, it is characterised in that in the mixture of the ethylene glycol magnesium and antimony glycol, second
Two magnesium alkoxides are 2~3 with antimony glycol mass ratio:1；The catalyst amount for the terephthalic acid (TPA) quality 0.01%~
0.05%；The one kind of the stabilizer in triphenyl phosphate, trimethyl phosphate and Trimethyl phosphite, stabilizing agent dosage is
The 0.01%~0.05% of the terephthalic acid (TPA) weight.
7. method according to claim 4, it is characterised in that the water is 100 with the mass ratio for dissolveing and washing away agent:3~4,
Polyester slice and water and the ratio for dissolveing and washing away agent, i.e. solid-to-liquid ratio are 1:5~10；It is described to dissolve and wash away agent for ethylene glycol monoethyl ether, ethylene glycol
One kind in one propyl ether and ethylene glycol monobutyl ether (EGMBE).
8. method according to claim 4, it is characterised in that the washing refers to that polyester slice is with 70~80 DEG C after brew
10~15min of hot water wash, is then cleaned, Drying and cooling is standby with cold water.
9. method according to claim 4, it is characterised in that the anti-ether agent is one kind in sodium acetate and calcium acetate,
Anti- ether agent consumption is the 0.01%~0.05% of the terephthalic acid (TPA) weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511018037.8A CN105483853B (en) | 2015-12-29 | 2015-12-29 | A kind of advertising lamp box cloth polyester industrial fiber of low thermal shrinkage and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201511018037.8A CN105483853B (en) | 2015-12-29 | 2015-12-29 | A kind of advertising lamp box cloth polyester industrial fiber of low thermal shrinkage and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN105483853A CN105483853A (en) | 2016-04-13 |
| CN105483853B true CN105483853B (en) | 2017-10-17 |
Family
ID=55671111
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201511018037.8A Active CN105483853B (en) | 2015-12-29 | 2015-12-29 | A kind of advertising lamp box cloth polyester industrial fiber of low thermal shrinkage and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN105483853B (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105504241B (en) * | 2015-12-29 | 2018-06-12 | 江苏恒力化纤股份有限公司 | A kind of high mode and low mode polyester industrial fiber and preparation method thereof |
| CN105646858B (en) | 2015-12-29 | 2018-07-27 | 江苏恒力化纤股份有限公司 | A kind of ultralow contractive polyester industrial yarn and preparation method thereof |
| 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 |
| CN109750380B (en) * | 2018-12-27 | 2020-10-16 | 江苏恒力化纤股份有限公司 | Preparation method of polyester lamp box advertisement cloth |
Family Cites Families (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1279214C (en) * | 2004-07-05 | 2006-10-11 | 苏州大学 | Process for synthesizing glycol antimony |
| CN102797055B (en) * | 2012-09-03 | 2014-08-20 | 江苏恒力化纤股份有限公司 | Manufacturing method for low-shrinkage high-strength PET industrial yarn |
| CN102797057B (en) * | 2012-09-03 | 2015-04-01 | 江苏恒力化纤股份有限公司 | Manufacturing method for high-modulus low-shrinkage PET industrial yarn |
| CN102797056B (en) * | 2012-09-03 | 2014-10-01 | 江苏恒力化纤股份有限公司 | Manufacturing method for superlow shrinkage type PET industrial yarn |
| CN103556285B (en) * | 2013-10-14 | 2016-01-13 | 江苏恒力化纤股份有限公司 | Super low shrinkage industrial yarn of a kind of creep resistant polyester and preparation method thereof |
-
2015
- 2015-12-29 CN CN201511018037.8A patent/CN105483853B/en active Active
Also Published As
| Publication number | Publication date |
|---|---|
| CN105483853A (en) | 2016-04-13 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105504242B (en) | A kind of low shrinkage polyester industrial filament and preparation method thereof | |
| CN105506773B (en) | A kind of high-strength middle contracting polyester industrial fiber and preparation method thereof | |
| CN105504241B (en) | A kind of high mode and low mode polyester industrial fiber and preparation method thereof | |
| CN105463608B (en) | A kind of high-strength safety belt polyester industrial fiber and preparation method thereof | |
| CN105504244B (en) | A kind of superelevation strong type polyester industrial fiber and preparation method thereof | |
| CN105504239B (en) | A kind of high-strength flatness polyester industrial fiber and preparation method thereof | |
| CN105483853B (en) | A kind of advertising lamp box cloth polyester industrial fiber of low thermal shrinkage and preparation method thereof | |
| CN105646858B (en) | A kind of ultralow contractive polyester industrial yarn and preparation method thereof | |
| CN105646856B (en) | A kind of low-shrinkage high-strength polyester industrial silk and preparation method thereof | |
| TW201000700A (en) | Polyethylene naphthalate fiber and process for producing the polyethylene naphthalate fiber | |
| CN105461911B (en) | A kind of industry polyester and preparation method thereof | |
| CN105603559B (en) | A kind of high-strength car mould polyester industrial fiber and preparation method thereof | |
| CN105603562B (en) | A kind of heat-resistance polyester industrial yarn and preparation method thereof | |
| CN105603563B (en) | A kind of corrosion-resistant polyester industrial fiber and preparation method thereof | |
| CN105504240B (en) | A kind of heat resistance high-strength polyester industrial silk and preparation method thereof | |
| CN105601899B (en) | A kind of polyester for bottle and preparation method thereof | |
| JP2011162892A (en) | Hollow polyester multifilament | |
| JPH04268327A (en) | Polyester having terminal carboxyl group capped with polycarbonate, fibrous material made from this polyester, and preparation of this polyester | |
| JPH0118167B2 (en) |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |