CN108130616A - A kind of high-strength polyester industrial fiber and preparation method thereof - Google Patents

A kind of high-strength polyester industrial fiber and preparation method thereof Download PDF

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Publication number
CN108130616A
CN108130616A CN201711342003.3A CN201711342003A CN108130616A CN 108130616 A CN108130616 A CN 108130616A CN 201711342003 A CN201711342003 A CN 201711342003A CN 108130616 A CN108130616 A CN 108130616A
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modified poly
thermal insulation
poly ester
polyester industrial
spinneret
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CN108130616B (en
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杨大矛
杨超明
赵艳丽
赵慧荣
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Jiangsu Hengli Chemical Fiber Co Ltd
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Jiangsu Hengli Chemical Fiber Co Ltd
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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
    • 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
    • C08G63/85—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
    • D—TEXTILES; PAPER
    • D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
    • D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
    • D01D10/00—Physical treatment of artificial filaments or the like during manufacture, i.e. during a continuous production process before the filaments have been collected
    • D01D10/02—Heat treatment
    • 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
    • D01D5/00—Formation of filaments, threads, or the like
    • D01D5/12—Stretch-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
    • D01D7/00—Collecting the newly-spun products

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  • Engineering & Computer Science (AREA)
  • Textile Engineering (AREA)
  • Mechanical Engineering (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Artificial Filaments (AREA)

Abstract

The present invention relates to a kind of high-strength polyester industrial fibers and preparation method thereof, modified poly ester through solid phase polycondensation is viscosified, melts, measure, squeezing out, cooling down, oiling, stretching, high-strength polyester industrial fiber is made in thermal finalization and winding, during cooling, keep longitudinal direction height constant, increase the cross-sectional area of slow cooling chamber, slow cooling chamber keeps the plate face temperature of spinneret by the way of heat preservation simultaneously, wherein it is as follows to include terephthalic acid (TPA) segment, ethylene glycol segment and branched dihydric alcohol segment, the structural formula of branched dihydric alcohol for the strand of modified poly ester：In formula, R1And R2It is each independently selected from the straight-chain alkyl-sub that carbon atom number is 1~3, R3Selected from the alkyl that carbon atom number is 1~5, R4Selected from the alkyl that carbon atom number is 2~5, fracture strength >=8.1cN/dtex of high-strength polyester industrial fiber obtained.The method of the present invention advantages of simple, industrial yarn obtained have the advantages that fracture strength is high and mechanical property is good.

Description

A kind of high-strength polyester industrial fiber and preparation method thereof
Technical field
The invention belongs to fiber preparation fields, are related to a kind of high-strength polyester industrial fiber and preparation method thereof.
Background technology
Polyethylene terephthalate (PET) fiber since the advent of the world obtains fast due to the excellent performance that it has Suddenly develop, yield has become the hat of world's synthetic fibers.Polyester fiber has fracture strength height, elasticity modulus height, returns Elasticity is moderate, thermal finalization is had excellent performance, heat-resisting light resistance is good and a series of Optimality such as acid-fast alkali-proof good corrosion resistance Can, and fabric prepared therefrom has many advantages, such as that crease-resistant and stiffness is good, so, polyester fiber is standby to be widely used in clothes With the fields such as home textile.
But during the polycondensation reaction of synthesis ethylene terephthalate, particularly when generating linear polymer, Since high-temperature oxydation degradation also association linear and cyclic oligomer, cyclic oligomer are due to macromolecular chain in polycondensation phase Hold back sting cyclisation and formed, about more than 70% is cyclic trimer in cyclic oligomer, cyclic trimer have easily aggregation, The easily characteristics such as crystallization, chemistry and heat-resistant stability height, generation cyclic trimer can there are following influences on polyester processing：(1) meeting The blocking of filament spinning component is caused, influences the service life of fondant filter and component；(2) it can be precipitated in fiber heat-setting process, It is deposited on heating roller, frictional force is caused to increase and heat irregular；(3) dyeing course can be made centered on cyclic trimer Dye aggregation is simultaneously adhered to fiber surface, and phenomena such as dyestuff color dot, spot and dyeing defect occurs in fiber surface, influences to be weaved by it The feel and coloured light of the fabric formed, the normal flow velocity of melt can be limited by being simultaneously filled with the cyclic oligomer of pipeline and valve Degree, causes stock-dye irregular, poor reproducibility；(4) fiber surface is adhered to, leads to, around yarn difficulty, broken yarn and thickness occur Phenomena such as uneven, influences the mechanical properties such as fracture strength and the elongation at break of fiber, seriously affects product quality.
Meanwhile in PET fiber production technology, slow cooling area is usually both provided with, purpose has two：One is to ensure that strand Will not be rapidly cooled after spinneret is gone out, cause it is highly oriented due to chilling outside strand, inside because of high temperature, macromolecular is also In disordered state, fiber radial direction architectural difference is big, i.e., so-called " core-skin " effect；Second, maintain spinning plate surface one higher Temperature, make wire vent smooth, aperture bulking effect is normal, be unlikely to occur " melt fracture " formation " weak silk ".To slow cooling area Mode of heating is actively to heat there are mainly two types of pattern, first, as shown in Figure 1, the heating agent using babinet is heated, is spun Silk temperature once it is determined that, generally no longer adjust, it is relatively passive, it is difficult to adapt to different application conditions；It is another as shown in Fig. 2, It is heated using electrically heated mode, set temperature can be higher than babinet heat medium temperature, can also be lower, cleverer It is living, it can be configured according to actual conditions, but high temperature can aggravate coking of the oligomer on spinneret, if reducing temperature For example cut off the power and do not heat, it, can be from case since the aluminum material that heater is usually the good quality weight of a heat-transfer effect is formed Body siphons away amount of heat, and component chambers outer surrounding heating agent is caused to condense rapidly, and heat supplement is insufficient, so as to make spinning group Part temperature declines, and melt flowability is remarkably decreased, and the problems such as a large amount of lousiness drops occurs in product, especially for odd-shaped cross section Fiber produces, and odd-shaped cross section causes aperture perimeter significantly to increase, and coking material is more in aperture accumulating amount, it is easy to strand is scratched, and There is elbow silk, the presence of this flaw generates single wire fracture in strand high-speed cruising, in cake surface with lousiness drop etc. Form shows, and the presence of lousiness is brought a great deal of trouble, and tow strength and elongation is made to be affected to post-processing unwinding, This was avoided as possible in production other than the defects of mode of heating, and slow cooling area of the prior art is also fatal scarce there are one Fall into, i.e. slow cooling area is cylindrical chamber, oligomer cannot quickly, the loss of unobstructed ground, oligomer is gathered in high-temperature field, must A large amount of cokings on spinneret are scheduled on, spinneret is caused to block, shorten the clear plate period, otherwise coking material is attached to spinneret orifice week It encloses, generates elbow silk, product appearance quality deteriorates rapidly, and broken end dramatically increases, and production efficiency declines, and labor intensity is high, It particularly shows particularly evident on production superbright light profiled fibre, has seriously affected normal production run, caused Production cost greatly wastes.
Growing with polyester fiber yield, people also increasingly improve the quality requirement of fiber, often require that fibre Dimension has excellent mechanical property, such as is used to prepare the fiber of car belt, household or clothes etc., all needs to have Higher fracture strength, but due in the fiber prepared by the prior art oligomer it is higher, make under the mechanical property of fiber Drop, causes fiber uneven, and easily fiber is made to generate lousiness.
Therefore, a kind of good high quality fiber of mechanical property is prepared as current urgent problem to be solved.
Invention content
The purpose of the invention is to overcome the problems, such as that fibrous mechanical property of the prior art is bad and quality is not high, Provide the high-strength polyester industrial fiber that a kind of mechanical property is good and quality is high.Branched binary in modified poly ester of the present invention The introducing of alcohol, reduces the cyclic oligomer generated in polyester side reaction, and the reduction of fiber surface cyclic oligomer reduces Phenomena such as fracture of wire and uneven fiber thickness, occurs for fiber, reduces fracture strength and extension at break of the cyclic oligomer to fiber The influence that the mechanical properties such as rate generate improves the quality of fiber；By the way that cylindrical slow cooling chamber is changed to rectangular cylindrical, expand Big spinning oligomer loss space, and active heated type slow cooling area is changed to non-heated heat preserving type, oligomer is reduced in height Gather quantity and hardness on warm spinneret, the profiled fibre clear plate period is significantly extended, by effectively controlling Temperature reduces the appearance of the lousiness of fiber and a phenomenon of floaing, so as to improve the quality of fiber.
In order to achieve the above object, the technical solution adopted by the present invention is：
A kind of high-strength polyester industrial fiber, the material of high-strength polyester industrial fiber are modified poly ester, the molecule of modified poly ester Chain includes terephthalic acid (TPA) segment, ethylene glycol segment and branched dihydric alcohol segment, and the structural formula of branched dihydric alcohol is such as Under：
In formula, R1And R2It is each independently selected from the straight-chain alkyl-sub that carbon atom number is 1~3, R3It is 1 selected from carbon atom number ~5 alkyl, R4Selected from the alkyl that carbon atom number is 2~5, the purpose that carbon atom number limits：Due to introducing branch in dihydric alcohol Chain structure and backbone can weaken the electronegativity of alkoxy portion, and the carbon atom number of branched structure is too small, to alcoxyl The electronegativity influence of base section is small, has little significance to the generation for reducing cyclic oligomer；The carbon atom number mistake of branched structure Greatly, intermolecular entanglement can be generated, the distribution of molecular weight is had an impact；
Fracture strength >=8.1cN/dtex of high-strength polyester industrial fiber.Fiber prepared by the present invention has higher Fracture strength, uniformity is good, and full-rolling rate is high.
As preferred technical solution：
A kind of high-strength polyester industrial fiber as described above, the fiber number of the high-strength polyester industrial fiber for 275~ 1100dtex, line density deviation ratio are ± 1.5%, fracture strength CV value≤3.0%, elongation at break central value for 13.5~ 17.0%, elongation at break deviation ratio is ± 1.5%, the elongation of extension at break CV value≤8.0%, 4.0cN/dtex loads Central value be the deviation ratios of elongation of 5.7~6.5%, 4.0cN/dtex loads be ± 0.8%, 177 DEG C, 10min and Dry-hot shrinkage under the conditions of 0.05cN/dtex is 4.3~9.3%, and network is 6 ± 2/m, and oil content is 0.4~0.9%. The deviation ratio of the elongation of the 4.0cN/dtex loads of the polyester industrial fiber of the present invention is smaller, illustrates that the uniformity of product is good, fine The quality of dimension is high.
A kind of high-strength polyester industrial fiber as described above, the content of cyclic oligomer in the modified poly ester≤ 0.6wt%, the amount of cyclic oligomer is 1.5~2.1wt% in polyester made from the prior art, and the present invention is relative to existing skill Art significantly reduces the production quantity of cyclic oligomer；
The number-average molecular weight 20000~27000 of the modified poly ester, molecular weight distributing index are 1.8~2.2, modified poly- The molecular weight of ester is higher, and molecular weight distribution is relatively narrow, disclosure satisfy that the demand of spinning processing, and it is excellent to be conducive to processability Fiber；
The molar content of branched dihydric alcohol segment is terephthalic acid (TPA) segment molar content in the modified poly ester 3~5%, the molar content of branched dihydric alcohol segment is relatively low in modified poly ester, is conducive to keep the Optimality of polyester itself Energy；
The branched dihydric alcohol for 2- Ethyl-2-Methyl -1,3- propylene glycol, 2,2- diethyl -1,3- propylene glycol, 2-butyl-2-ethyl-1,3-propanediol, 3,3- diethyl -1,5- pentanediols, 4,4- diethyl -1,7- heptandiols, 4,4- bis- (1,-Methylethyl) -1,7- heptandiols, 3,3- dipropyl -1,5- pentanediols, 4,4- dipropyl -1,7- heptandiols, 4- methyl - 4- (1,1- dimethyl ethyls) -1,7- heptandiols, 3- methyl -3- amyls -1,6-HD or 3,3- diamyl -1,5- penta 2 Alcohol.
A kind of high-strength polyester industrial fiber as described above, the preparation method of the modified poly ester are：By terephthaldehyde Acid, ethylene glycol and the branched dihydric alcohol successively carry out esterification after mixing and polycondensation reaction obtains modified gather Ester；The specific preparation process of the modified poly ester is as follows：
(1) esterification；
Terephthalic acid (TPA), ethylene glycol and the branched dihydric alcohol are made into slurry, catalyst is added in and stabilizer mixes Close uniformly after, in nitrogen atmosphere pressurization carry out esterification, moulding pressure be normal pressure~0.3MPa, the temperature of esterification It is 250~260 DEG C, is esterification terminal when the water quantity of distillate in esterification reaches more than 90% theoretical value；
(2) polycondensation reaction；
After esterification, start the polycondensation reaction in low vacuum stage under condition of negative pressure, the staged pressure 30~ Absolute pressure 500Pa is steadily evacuated to by normal pressure in 50min hereinafter, reaction temperature is 260~270 DEG C, the reaction time for 30~ 50min then proceedes to vacuumize, and carries out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is made to be further reduced to absolute pressure For 100Pa hereinafter, reaction temperature is 275~285 DEG C, the reaction time is 50~90min, and modified poly ester is made.
A kind of high-strength polyester industrial fiber as described above, in step (1), terephthalic acid (TPA), ethylene glycol and the band branch The molar ratio of the dihydric alcohol of chain is 1:1.2~2.0:0.03~0.06, the addition of the catalyst is terephthalic acid (TPA) weight 0.01~0.05%, the addition of the stabilizer is the 0.01~0.05% of terephthalic acid (TPA) weight；
The catalyst is antimony oxide, antimony glycol or antimony acetate, and the stabilizer is triphenyl phosphate, phosphoric acid Trimethyl or Trimethyl phosphite.
The present invention also provides a kind of method of high-strength polyester industrial fiber as described above is prepared, by the modified poly ester It viscosifies, melt through solid phase polycondensation, measuring, squeezing out, cooling down, oiling, stretching, high-strength polyester industrial is made in thermal finalization and winding Silk；
During the cooling, keep longitudinal direction height constant, increase the cross-sectional area of slow cooling chamber, while slow cooling chamber uses The mode of heat preservation keeps the plate face temperature of spinneret.Heating agent or electrically heated side is usually used in slow cooling chamber in the prior art Formula keeps the plate face temperature of spinneret, and the present invention substitutes heating agent or electrically heated mode by the way of heat preservation, is saving energy While source, the temperature in slow cooling area is reduced, effectively reduces coking degree of the oligomer in spinning plate surface, extends clear plate week Phase, the present invention solve in traditional terylene spinning technique with the oligomer of spinning association that the coking quantity on spinneret is more, speed Soon, the problem of hard texture, spinneret temperature is being effectively ensured, is achieving the purpose that the extension clear plate period, production is super During light profiled fibre, the clear plate period extended to 34 hours or so from average 22 hours, depending on the difference of kind, clear plate week Phase extends amplitude 35~45%.
As preferred technical solution：
Method as described above, the inherent viscosity of the solid phase polycondensation thickening post-modification polyester is 1.0~1.2dL/g, special Property viscosity is a kind of characteristic manner of modified poly ester molecular weight, and the inherent viscosity of modified poly ester is excessively high, and processing temperature accordingly rises Height, the easy thermal degradation of product, the inherent viscosity of modified poly ester is too low, then is difficult to obtain the required intensity of fiber and performance；Clearly Manage the cycle stretch-out of spinneret 35~45%, replacement cycle >=40 day of filament spinning component.The replacement week of filament spinning component of the present invention Phase is long, and the stability of product is good, while reduces the cost of production, improves economic benefit.
Method as described above, the cross-sectional area of the increase slow cooling chamber refer to keeping what is connect with slow cooling chamber Under the premise of spinneret is constant, the cross section of slow cooling chamber is changed to rectangle by circle, slow cooling chamber of the prior art is circle Cylindricality, cross section are circle, and in the case where the spinneret for keeping connecting with slow cooling chamber is constant, rectangle is relative to rounded face Product increase is larger, and the volume of slow cooling chamber is caused to increase about 50%, greatly improves the loss speed of oligomer (spinning association) Degree and quantity；The slow cooling chamber is surrounded by thermal insulation board and partition, the embedded bottom for hanging on spinning manifold of thermal insulation board, is protected Hollow chamber I is opened up in warm plate, partition, which is assigned into hollow chamber I, is divided into multiple slow cooling chambers, each slow cooling chamber Inside there is one block of spinneret, by assigning partition, distinguish ingot number, and avoid spraying silicone oil during clear plate and interfere with each other；
Stainless steel plate of the thermal insulation board for the thermal insulation material of internal 400 DEG C of heatproof of filling or more, the thickness of thermal insulation board are 30~50mm, the wall thickness of stainless steel plate is 0.9~1.5mm, and under the premise of guarantee is indeformable, the wall thickness of stainless steel plate will use up Measure it is small, reduce itself caloric receptivity and babinet heating agent load；
The thermal insulation material is rock wool or ceramic fibre, and thermal insulation material is not limited to above two material, other have The material of similar functions is equally applicable to the present invention；
The thickness of the partition is 1~3mm, and the thickness of partition is thin as possible in the case of proof strength；
Polylith spinneret in the hollow chamber I is round spinneret, and the diameter of polylith spinneret is identical, center of circle position In on same straight line and close adjacent；
The cross section of the hollow chamber I is rectangle, and the side for being parallel to polylith spinneret circle center line connecting is long side, is hung down Directly in the side of long side be short side；
The length of the long side is 1.2 times of the sum of the polylith spinneret board diameter, and the length of the short side is the spray 1.7 times of filament plate diameter.
Method as described above is superimposed thermal insulation board under the thermal insulation board, and the material of thermal insulation board is identical with thermal insulation board, heat-insulated Hollow chamber II is opened up in plate, hollow chamber II is identical with the cross-sectional shape of hollow chamber I；
In the position that hollow chamber II connects with hollow chamber I, two sides of II cross section of hollow chamber respectively with it is hollow Two short sides of I cross section of chamber overlap, and the length on two sides is more than two short sides so that thermal insulation board is folded with thermal insulation board Rear hollow chamber II and hollow chamber I is added to form a step, oligomer is easier to spread, the addition of thermal insulation board in the present invention The length of zone of silence is extended, is conducive to the promotion of fiber quality, simultaneously because II inside septumless of hollow chamber, it can be most Avoid influence of the cool ambient air to the plate face temperature of spinneret to big degree；
The thickness of the thermal insulation board is 25~45mm.
Method as described above, the good high quality fiber of mechanical property, of the invention to the phase in preparation process in order to obtain It closes technological parameter to be adjusted, the spinning technology parameter of the high-strength polyester industrial fiber after adjustment is as follows：
It stretches, the technological parameter of thermal finalization is：
Invention mechanism：
In organic compound, the angle between two chemical bonds that the same atom of intramolecular is formed is known as bond angle, and bond angle leads to It commonly uses the number of degrees to represent, the electronegativity of central atom and coordination atom in organic compound molecule, the bond angle of molecule can be influenced.When During the electronegativity increase for the coordination atom being bonded with central atom, the enhancing of coordination atom electron-withdrawing ability, bond electron pair will be to Ligand direction is moved, from central atom farther out, make it is close to each other when repulsion reduces between key pair, so that bond angle also subtracts therewith It is small, on the contrary, when the electronegativity for the coordination atom being bonded with central atom reduces, the enhancing of coordination atom electron donation, bonding Electronics to will be moved to central atom direction, from central atom closer to, make to be located remotely from each other due to repulsion increases between key pair, so as to Bond angle also increases therewith.
According to Pauling Electronegativities, the electronegativity of C, H and O atom is respectively 2.55,2.20 and 3.44, and according to Valence electron balancing energy is theoretical, and the calculation formula of Group Electronegativity is shown below：
In formula, xiFor the electronegativity of i atoms neutral atom before bonding, NVe, iFor valence electron number in i atoms, niFor The number of i atoms in the molecule.Calculating step for more complicated Group Electronegativity is mainly：Simple radical is calculated first Then the electronegativity of group regards simple group as electronegativity that quasiatom calculates more complicated group again, such successive iteration, Finally obtain the electronegativity of Targeting groups.It should be noted that calculate quasiatom electronegativity when, base son (for example, Base of group-OH is O atom) in the valence electron of non-bonding regard the valence electron of quasiatom as.
C atoms can be with the O atom of hydroxyl in dihydric alcohol after the C-O keys fracture of carboxyl in terephthalic acid (TPA) in the present invention With reference to the new C-O keys formed in ester group, the C atoms key C-C formed with C atoms on phenyl ring and the change newly formed in ester group The bond angle learned between key C-O is denoted as α, and the change of bond angle α can influence annulation, and when α is less than 109 °, molecule is easy to cyclization, And with the increase of α, the probability of molecule cyclization can decline.Present invention introduces branched dihydric alcohol, structural formula such as following formula institutes Show：
In formula, R1And R2It is each independently selected from the straight-chain alkyl-sub that carbon atom number is 1~3, R3It is 1 selected from carbon atom number ~5 alkyl, R4Selected from the alkyl that carbon atom number is 2~5.The diol structure due to introducing branched structure and backbone, Can weaken the electronegativity of its alkoxy portion, by the calculation formula of Group Electronegativity can also obtain in the diol structure with The electronegativity for the group that carbonyl is connected is between 2.59~2.79 in diacid, and the base being connected in ethylene glycol with carbonyl in diacid Group-OCH2CH2Electronegativity for 3.04, thus its alkoxy is than-the OCH in ethylene glycol2CH2There is stronger electron Property, so that the bond electron pair on the chemical bond C-O keys newly formed will be moved to center C atomic orientations, from central atom Closer to making to be located remotely from each other due to repulsion increases between key pair, so that bond angle α is more than 109 °, generate the probability of linear polymer Increase, so as to reduce the generation of cyclic oligomer, the reduction of fiber surface cyclic oligomer reduces fiber and fracture of wire occurs With fiber thickness it is uneven phenomena such as, reduce cyclic oligomer to mechanical properties such as the fracture strength of fiber and elongation at breaks The influence of generation, so as to improve product quality.
The cross section of slow cooling chamber is changed to by the present invention in the case where keeping longitudinal direction height constant by current circle Rectangle increases the cross-sectional area of slow cooling chamber, expands spinning oligomer loss space, while the heat preservation side of slow cooling chamber Active heated type is changed to non-heated heat preserving type by formula, while energy consumption is reduced, reduces oligomer on high-temperature spinneret plate Gather quantity and hardness.By the improvement of these two aspects, the present invention significantly extends profiled fibre clear plate week Phase.It is also possible to hollow thermal insulation board is superimposed under thermal insulation board so that the two after thermal insulation board is superimposed with thermal insulation board Internal hollow chamber is formed into a step, is on the one hand extended the length of zone of silence, is on the other hand accelerated oligomer Diffusion velocity, while insulation can also be played the role of.The cross-sectional area of present invention increase slow cooling chamber, on the one hand causes Oligomer in fiber can be further diffused into air, improve the performance of fiber, and what is on the other hand diffused out is oligomeric The probability that object is trapped on spinneret reduces, and reduces the cleaning frequency of spinneret, and slow cooling chamber is kept by the way of warming The plate face temperature of spinneret, further reduces the generation of lousiness phenomenon, reduces cleaning frequency and the lousiness of spinneret Generation, improve the quality of product, reduce production cost.
Advantageous effect：
(1) a kind of high-strength polyester industrial fiber of the invention, preparation method advantages of simple, polyester industrial fiber obtained break Resistance to spalling is high, and mechanical property is good, has good market popularization value；
(2) preparation method of a kind of high-strength polyester industrial fiber of the invention, rectangular column is changed to by cylindrical slow cooling chamber Shape expands spinning oligomer loss space, and active heated type slow cooling area is changed to non-heated heat preserving type, reduces oligomeric Object gathers quantity and hardness on high-temperature spinneret plate, significantly extends the profiled fibre clear plate period；
(3) preparation method of a kind of high-strength polyester industrial fiber of the invention, greatly improves production efficiency, reduces Waste silk improves spinning quality, reduces labor intensity；
(4) preparation method of a kind of high-strength polyester industrial fiber of the invention, by introducing band branch in modified poly ester Dihydric alcohol, the bond angle of polyester molecule is changed, so as to significantly reduce the generation of cyclic oligomer in process of polyester synthesizing.
Description of the drawings
Fig. 1 is that the cylindrical slow cooling area of the prior art uses the schematic diagram of gas phase heating medium for heating；
Fig. 2 is that the cylindrical slow cooling area of the prior art uses electrically heated schematic diagram；
Fig. 3 is that the square frame-shaped slow cooling area of the present invention uses the schematic diagram of thermal insulation board heat preservation；
Wherein, 1- spinning manifolds, gas phase heating agent in 2- spinning manifolds, 3- hollow chamber I, 4- electric heater, 5- hollow cavities Room II, 6- thermal insulation boards, 7- thermal insulation boards.
Specific embodiment
The invention will be further elucidated with reference to specific embodiments.It should be understood that these embodiments are merely to illustrate this It invents rather than limits the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, this field Technical staff can make various changes or modifications the present invention, and such equivalent forms equally fall within the application appended claims Book limited range.
Embodiment 1
A kind of preparation method of high-strength polyester industrial fiber, is as follows：
(1) modified poly ester is prepared：
(a) esterification；It is 1 by molar ratio:1.2:0.03 terephthalic acid (TPA), ethylene glycol and 2- Ethyl-2-Methyls- 1,3-PD is made into slurry, adds in antimony oxide and triphenyl phosphate after mixing, and pressurizeing in nitrogen atmosphere carries out Esterification, moulding pressure are normal pressure, and the temperature of esterification is 250 DEG C, when the water quantity of distillate in esterification reaches theoretical Value 90% when for esterification terminal, wherein the addition of antimony oxide is the 0.01% of terephthalic acid (TPA) weight, phosphoric acid The addition of triphenylmethyl methacrylate be terephthalic acid (TPA) weight 0.05%, the structural formula of wherein 2- Ethyl-2-Methyls -1,3-PD It is as follows：
(b) polycondensation reaction；After esterification, start the polycondensation reaction in low vacuum stage under condition of negative pressure, Pressure is steadily evacuated to absolute pressure as 500Pa by normal pressure in 30min, reaction temperature is 260 DEG C, reaction time 40min, It then proceedes to vacuumize, carries out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is made to be further reduced to absolute pressure as 100Pa, Reaction temperature is 275 DEG C, reaction time 70min, and modified poly ester is made.Wherein the strand of modified poly ester is included to benzene two Formic acid segment, ethylene glycol segment and 2- ethyl -2- methyl-1s, 3-propanediol segment, the content of cyclic oligomer in modified poly ester For 0.6wt%, number-average molecular weight 20000, molecular weight distributing index 2.0,2- Ethyl-2-Methyls -1,3- third in modified poly ester The molar content of glycol segment is the 3% of terephthalic acid (TPA) segment molar content；
(2) modified poly ester viscosify, melt through solid phase polycondensation, measuring, squeezing out, cooling down, oiling, stretching, thermal finalization and winding High-strength polyester industrial fiber is made.Wherein, the inherent viscosity of solid phase polycondensation thickening post-modification polyester is 1.02dL/g；Spinning group The replacement cycle of part is 40 days, clears up the cycle stretch-out 39% of spinneret, and the maceration extracts of first bath are D- in two bath infusion processes 417, the maceration extract of the second bath is RFL.During cooling, keep longitudinal direction height constant, increase the cross-sectional area of slow cooling chamber, simultaneously Slow cooling chamber keeps the plate face temperature of spinneret by the way of heat preservation, and slow cooling chamber structure schematic diagram will be as shown in figure 3, will protect The warm embedded bottom for hanging on spinning manifold 1 of plate 6, there is gas phase heating agent 2 in spinning manifold 1, in thermal insulation board 6 in " rectangular-ambulatory-plane " Sky, inside opens up hollow chamber I 3, and the cross section of the chamber is rectangle, using be parallel to the side of polylith spinneret circle center line connecting as Long side direction, 1.2 times for the sum of polylith spinneret board diameter of the length of long side, using perpendicular to the direction of long side as short side side To the length of short side is 1.7 times of spinneret board diameter, and thickness, which is assigned into for the partition of 1mm in hollow chamber I 3, to be separated Into multiple slow cooling chambers, there is one block of round spinneret in each slow cooling chamber.The diameter of each spinneret is identical and the center of circle is located at together It is on one straight line and close adjacent.Stainless steel plate of the thermal insulation board 6 for the rock wool of internal 400 DEG C of heatproof of filling, the thickness of thermal insulation board 6 For 30mm, the wall thickness of stainless steel plate is 0.9mm.The thermal insulation board 7 that 6 times superposition thickness of thermal insulation board are 25mm, the material of thermal insulation board 7 It is identical with thermal insulation board 6, hollow chamber II 5, the cross-sectional shape of hollow chamber II 5 and hollow chamber I 3 are opened up in thermal insulation board 7 It is identical；Hollow chamber II 5 is identical with the long edge lengths of the cross section of hollow chamber I 3；In hollow chamber II 5 and hollow chamber I 3 The position of connection, two sides of II 5 cross section of hollow chamber overlap respectively with two short sides of hollow chamber I 3 cross section, and The length on two sides is more than two short sides.The rectangular cylindrical slow cooling area for wherein corresponding to single round spinneret uses thermal insulation board Heat preservation, the embedded bottom for hanging on spinning manifold of thermal insulation board, thermal insulation board is interior to be equipped with hollow chamber I, is superimposed under thermal insulation board heat-insulated Plate offers hollow chamber II in thermal insulation board, wherein in the position that hollow chamber II connects with hollow chamber I, hollow chamber II Two sides of cross section overlap respectively with two short sides of hollow chamber I cross section, and the length on two sides be more than it is two short Side, hollow chamber II and hollow chamber I form a step to accelerate oligomer diffusion after the superposition of two plates.
The spinning technology parameter of high-strength polyester industrial fiber is shown in Table 1.
Final high-strength polyester industrial fiber various performance parameters obtained are shown in Table 2.
Embodiment 2
A kind of preparation method of high-strength polyester industrial fiber, is as follows：
(1) modified poly ester is prepared：
(a) esterification；It is 1 by molar ratio:1.3:0.04 terephthalic acid (TPA), ethylene glycol and 2,2- diethyl -1,3- Propylene glycol is made into slurry, adds in antimony glycol and trimethyl phosphate after mixing, and pressurizeing in nitrogen atmosphere, it is anti-be esterified Should, moulding pressure is normal pressure, and the temperature of esterification is 260 DEG C, when the water quantity of distillate in esterification reaches theoretical value It is esterification terminal when 91%, wherein the addition of antimony glycol is the 0.02% of terephthalic acid (TPA) weight, trimethyl phosphate Addition be terephthalic acid (TPA) weight 0.03%, wherein the structural formula of 2,2- diethyl -1,3-PD is as follows：
(b) polycondensation reaction；After esterification, start the polycondensation reaction in low vacuum stage under condition of negative pressure, Pressure is steadily evacuated to absolute pressure as 490Pa by normal pressure in 35min, reaction temperature is 261 DEG C, reaction time 30min, It then proceedes to vacuumize, carries out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is made to be further reduced to absolute pressure as 100Pa, Reaction temperature is 277 DEG C, reaction time 85min, and modified poly ester is made.Wherein the strand of modified poly ester is included to benzene two Formic acid segment, ethylene glycol segment and 2,2- diethyl -1,3-PD segment, the content of cyclic oligomer is in modified poly ester 0.6wt%, number-average molecular weight 27000, molecular weight distributing index 1.8,2,2- diethyl -1,3-PD in modified poly ester The molar content of segment is the 5% of terephthalic acid (TPA) segment molar content；
(2) modified poly ester through solid phase polycondensation viscosified, melted, measured, squeezed out, cooled down, oiled, stretched, thermal finalization and volume Around obtained high-strength polyester industrial fiber.Wherein, the inherent viscosity of solid phase polycondensation thickening post-modification polyester is 1.12dL/g；Spinning The replacement cycle of component is 42 days, clears up the cycle stretch-out 40% of spinneret, and the maceration extracts of first bath are in two bath infusion processes D-417, the maceration extract of the second bath is RFL.During cooling, keep longitudinal direction height constant, increase the cross-sectional area of slow cooling chamber, together When slow cooling chamber the plate face temperature of spinneret is kept by the way of heat preservation, slow cooling chamber configuration is substantially the same manner as Example 1, Difference is septa thickness for 2mm, and filling thermal insulation material is ceramic fibre in thermal insulation board, and heat resisting temperature is 405 DEG C, heat preservation Plate thickness is 40mm, and stainless steel plate wall thickness is 1.2mm, and heat-insulated plate thickness is 35mm.
The spinning technology parameter of high-strength polyester industrial fiber is shown in Table 1.
Final high-strength polyester industrial fiber various performance parameters obtained are shown in Table 2.
Embodiment 3
A kind of preparation method of high-strength polyester industrial fiber, is as follows：
(1) modified poly ester is prepared：
(a) esterification；It is 1 by molar ratio:1.4:0.05 terephthalic acid (TPA), ethylene glycol and 2- butyl -2- ethyls - 1,3-PD is made into slurry, adds in antimony acetate and Trimethyl phosphite after mixing, the pressurization progress ester in nitrogen atmosphere Change reaction, moulding pressure 0.1MPa, the temperature of esterification is 252 DEG C, when the water quantity of distillate in esterification reaches theoretical Value 92% when for esterification terminal, wherein the addition of antimony acetate is the 0.03% of terephthalic acid (TPA) weight, phosphorous acid three The addition of methyl esters is the 0.01% of terephthalic acid (TPA) weight, and wherein the structural formula of 2- butyl -2- ethyls -1,3-PD is such as Under：
(b) polycondensation reaction；After esterification, start the polycondensation reaction in low vacuum stage under condition of negative pressure, Pressure is steadily evacuated to absolute pressure as 495Pa by normal pressure in 40min, reaction temperature is 263 DEG C, reaction time 45min, It then proceedes to vacuumize, carries out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is made to be further reduced to absolute pressure as 95Pa, Reaction temperature is 278 DEG C, reaction time 60min, and modified poly ester is made, and the wherein strand of modified poly ester is included to benzene two Formic acid segment, ethylene glycol segment and 2- butyl -2- ethyls -1,3-PD segment, the content of cyclic oligomer in modified poly ester For 0.5wt%, number-average molecular weight 21000, molecular weight distributing index 2.2,2- butyl -2- ethyls -1,3- third in modified poly ester The molar content of glycol segment is the 4% of terephthalic acid (TPA) segment molar content；
(2) modified poly ester through solid phase polycondensation viscosified, melted, measured, squeezed out, cooled down, oiled, stretched, thermal finalization and volume Around obtained high-strength polyester industrial fiber.Wherein, the inherent viscosity of solid phase polycondensation thickening post-modification polyester is 1.10dL/g；Spinning The replacement cycle of component is 48 days, clears up the cycle stretch-out 44% of spinneret, and the maceration extracts of first bath are in two bath infusion processes D-417, the maceration extract of the second bath is RFL.During cooling, keep longitudinal direction height constant, increase the cross-sectional area of slow cooling chamber, together When slow cooling chamber the plate face temperature of spinneret is kept by the way of heat preservation, slow cooling chamber configuration is substantially the same manner as Example 1, Difference is septa thickness for 3mm, and filling thermal insulation material is rock wool in thermal insulation board, and heat resisting temperature is 410 DEG C, keeps the temperature plate thickness It spends for 50mm, stainless steel plate wall thickness is 1.5mm, and heat-insulated plate thickness is 45mm.
The spinning technology parameter of high-strength polyester industrial fiber is shown in Table 1.
Final high-strength polyester industrial fiber various performance parameters obtained are shown in Table 2.
Embodiment 4
A kind of preparation method of high-strength polyester industrial fiber, is as follows：
(1) modified poly ester is prepared：
(a) 3,3- diethyl -1,5- pentanediols are prepared；At 90 DEG C, under nitrogen atmosphere, by 3,3- diethyl-propionic aldehyde, second Then aldehyde and triethylamine react 20min have concentrate addition in the hydrogenation reactor of thunder girl's Raney nickel, in 2.914MPa Hydrogen press and 100 DEG C at react, reaction finish, cooling, catalyst is precipitated, solution spent ion exchange resin processing after, decompression steam Water detaches, and purification obtains 3,3- diethyl -1,5-PD, wherein the structural formula of 3,3- diethyl -1,5-PD is such as Under：
(b) esterification；It is 1 by molar ratio:1.5:0.06 terephthalic acid (TPA), ethylene glycol and 3,3- diethyl -1,5- Pentanediol is made into slurry, adds in antimony oxide and triphenyl phosphate after mixing, pressurizes and be esterified in nitrogen atmosphere Reaction, moulding pressure 0.3MPa, the temperature of esterification is 255 DEG C, when the water quantity of distillate in esterification reaches theoretical value 95% when for esterification terminal, wherein the addition of antimony oxide is the 0.04% of terephthalic acid (TPA) weight, tricresyl phosphate The addition of phenyl ester is the 0.01% of terephthalic acid (TPA) weight；
(c) polycondensation reaction；After esterification, start the polycondensation reaction in low vacuum stage under condition of negative pressure, Pressure is steadily evacuated to absolute pressure as 400Pa by normal pressure in 50min, reaction temperature is 265 DEG C, reaction time 33min, It then proceedes to vacuumize, carries out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is made to be further reduced to absolute pressure as 90Pa, Reaction temperature is 280 DEG C, reaction time 50min, and modified poly ester is made, and the wherein strand of modified poly ester is included to benzene two Formic acid segment, ethylene glycol segment and 3,3- diethyl -1,5-PD segment, the content of cyclic oligomer is in modified poly ester 0.2wt%, number-average molecular weight 23000, molecular weight distributing index 1.9,3,3- diethyl -1,5-PD in modified poly ester The molar content of segment is the 3.5% of terephthalic acid (TPA) segment molar content；
(2) modified poly ester through solid phase polycondensation viscosified, melted, measured, squeezed out, cooled down, oiled, stretched, thermal finalization and volume Around obtained high-strength polyester industrial fiber.Wherein, the inherent viscosity of solid phase polycondensation thickening post-modification polyester is 1.18dL/g；Spinning The replacement cycle of component is 44 days, clears up the cycle stretch-out 35% of spinneret, and the maceration extracts of first bath are in two bath infusion processes D-417, the maceration extract of the second bath is RFL.During cooling, keep longitudinal direction height constant, increase the cross-sectional area of slow cooling chamber, together When slow cooling chamber the plate face temperature of spinneret is kept by the way of heat preservation, slow cooling chamber configuration is substantially the same manner as Example 1, Difference is septa thickness for 1.5mm, and filling thermal insulation material is ceramic fibre in thermal insulation board, and heat resisting temperature is 402 DEG C, is protected Warm plate thickness is 35mm, and stainless steel plate wall thickness is 1.0mm, and heat-insulated plate thickness is 30mm.
The spinning technology parameter of high-strength polyester industrial fiber is shown in Table 1.
Final high-strength polyester industrial fiber various performance parameters obtained are shown in Table 2.
Embodiment 5
A kind of preparation method of high-strength polyester industrial fiber, is as follows：
(1) modified poly ester is prepared：
(a) 4,4- diethyl -1,7- heptandiols are prepared；At 92 DEG C, under nitrogen atmosphere, by 4,4- diethyl-butyraldehyde, third Then aldehyde and triethylamine react 20min have concentrate addition in the hydrogenation reactor of thunder girl's Raney nickel, in 2.914MPa Hydrogen press and 100 DEG C at react, reaction finish, cooling, catalyst is precipitated, solution spent ion exchange resin processing after, decompression steam Water detaches, and purification obtains 4,4- diethyl -1,7- heptandiols, wherein the structural formula of 4,4- diethyl -1,7- heptandiols is such as Under：
(b) esterification；It is 1 by molar ratio:1.6:0.03 terephthalic acid (TPA), ethylene glycol and 4,4- diethyl -1,7- Heptandiol is made into slurry, adds in antimony glycol and trimethyl phosphate after mixing, and pressurizeing in nitrogen atmosphere, it is anti-be esterified Should, moulding pressure is normal pressure, and the temperature of esterification is 257 DEG C, when the water quantity of distillate in esterification reaches theoretical value It is esterification terminal when 92%, wherein the addition of antimony glycol is the 0.05% of terephthalic acid (TPA) weight, trimethyl phosphate Addition be terephthalic acid (TPA) weight 0.04%；
(c) polycondensation reaction；After esterification, start the polycondensation reaction in low vacuum stage under condition of negative pressure, Pressure is steadily evacuated to absolute pressure as 450Pa by normal pressure in 33min, reaction temperature is 270 DEG C, reaction time 30min, It then proceedes to vacuumize, carries out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is made to be further reduced to absolute pressure as 95Pa, Reaction temperature is 275 DEG C, reaction time 60min, and modified poly ester is made, and the wherein strand of modified poly ester is included to benzene two Formic acid segment, ethylene glycol segment and 4,4- diethyl -1,7- heptandiol segment, the content of cyclic oligomer is in modified poly ester 0.5wt%, number-average molecular weight 25000, molecular weight distributing index 2.1,4,4- diethyl -1,7- heptandiols in modified poly ester The molar content of segment is the 5% of terephthalic acid (TPA) segment molar content.
(2) modified poly ester through solid phase polycondensation viscosified, melted, measured, squeezed out, cooled down, oiled, stretched, thermal finalization and volume Around obtained high-strength polyester industrial fiber.Wherein, the inherent viscosity of solid phase polycondensation thickening post-modification polyester is 1.0dL/g；Spinning group The replacement cycle of part is 49 days, clears up the cycle stretch-out 36% of spinneret, and the maceration extracts of first bath are D- in two bath infusion processes 417, the maceration extract of the second bath is RFL.During cooling, keep longitudinal direction height constant, increase the cross-sectional area of slow cooling chamber, simultaneously Slow cooling chamber keeps the plate face temperature of spinneret by the way of heat preservation, and slow cooling chamber configuration is substantially the same manner as Example 1, no With being that it only has thermal insulation board, it is not superimposed thermal insulation board under thermal insulation board.
The spinning technology parameter of high-strength polyester industrial fiber is shown in Table 1.
Final high-strength polyester industrial fiber various performance parameters obtained are shown in Table 2.
Embodiment 6
A kind of preparation method of high-strength polyester industrial fiber, is as follows：
(1) modified poly ester is prepared：
(a) 4,4- bis- (1,-Methylethyl) -1,7- heptandiols are prepared；At 95 DEG C, under nitrogen atmosphere, by 4,4-, bis- (1- Methylethyl)-butyraldehyde, propionic aldehyde and triethylamine react 20min, concentrate addition then had thunder girl's Raney nickel plus hydrogen is anti- It answers in device, is reacted at 2.914MPa hydrogen pressure and 100 DEG C, reaction is finished, and catalyst is precipitated in cooling.Solution amberlite After fat processing, water is steamed in decompression, detaches, and purification obtains 4,4- bis- (1,-Methylethyl) -1,7- heptandiols, wherein 4,4- bis- The structural formula of (1,-Methylethyl) -1,7- heptandiols is as follows：
(b) esterification；It is 1 by molar ratio:1.7:0.05 terephthalic acid (TPA), ethylene glycol and 4,4- bis- (1 ,-methyl Ethyl) -1,7- heptandiols are made into slurry, and it adds in antimony acetate and Trimethyl phosphite after mixing, pressurizes in nitrogen atmosphere Esterification is carried out, moulding pressure 0.2MPa, the temperature of esterification is 253 DEG C, when the water quantity of distillate in esterification reaches To theoretical value 96% when for esterification terminal, wherein the addition of antimony acetate is the 0.01% of terephthalic acid (TPA) weight, sub- The addition of trimethyl phosphate is the 0.05% of terephthalic acid (TPA) weight；
(c) polycondensation reaction；After esterification, start the polycondensation reaction in low vacuum stage under condition of negative pressure, Pressure is steadily evacuated to absolute pressure as 480Pa by normal pressure in 38min, reaction temperature is 262 DEG C, reaction time 38min, It then proceedes to vacuumize, carries out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is made to be further reduced to absolute pressure as 98Pa, Reaction temperature is 279 DEG C, reaction time 80min, and modified poly ester is made, and the wherein strand of modified poly ester is included to benzene two Formic acid segment, ethylene glycol segment and 4,4- bis- (1,-Methylethyl) -1,7- heptandiol segments, cyclic oligomer in modified poly ester Content for 0.55wt%, number-average molecular weight 27000, molecular weight distributing index 2.2,4,4- bis- in modified poly ester (1 ,-first Base ethyl) -1,7- heptandiol segments molar content be terephthalic acid (TPA) segment molar content 4%；
(2) modified poly ester through solid phase polycondensation viscosified, melted, measured, squeezed out, cooled down, oiled, stretched, thermal finalization and volume Around obtained high-strength polyester industrial fiber.Wherein, the inherent viscosity of solid phase polycondensation thickening post-modification polyester is 1.0dL/g；Spinning group The replacement cycle of part is 40 days, clears up the cycle stretch-out 41% of spinneret, and the maceration extracts of first bath are D- in two bath infusion processes 417, the maceration extract of the second bath is RFL.During cooling, keep longitudinal direction height constant, increase the cross-sectional area of slow cooling chamber, simultaneously Slow cooling chamber keeps the plate face temperature of spinneret by the way of heat preservation, and slow cooling chamber configuration is substantially the same manner as Example 2, no With being that it only has thermal insulation board, it is not superimposed thermal insulation board under thermal insulation board.
The spinning technology parameter of high-strength polyester industrial fiber is shown in Table 1.
Final high-strength polyester industrial fiber various performance parameters obtained are shown in Table 2.
Embodiment 7
A kind of preparation method of high-strength polyester industrial fiber, is as follows：
(1) modified poly ester is prepared：
(a) 3,3- dipropyl -1,5- pentanediols are prepared；At 94 DEG C, under nitrogen atmosphere, by 3,3- dipropyl-propionic aldehyde, second Then aldehyde and triethylamine react 20min have concentrate addition in the hydrogenation reactor of thunder girl's Raney nickel, in 2.914MPa Hydrogen press and 100 DEG C at react, reaction finish, cooling, catalyst is precipitated.After the processing of solution spent ion exchange resin, decompression is steamed Water detaches, and purification obtains 3,3- dipropyl -1,5-PD, wherein the structural formula of 3,3- dipropyl -1,5-PD is such as Under：
(b) esterification；It is 1 by molar ratio:1.8:0.03 terephthalic acid (TPA), ethylene glycol and 3,3- dipropyl -1,5- Pentanediol is made into slurry, adds in antimony oxide and triphenyl phosphate after mixing, pressurizes and be esterified in nitrogen atmosphere Reaction, moulding pressure 0.3MPa, the temperature of esterification is 250 DEG C, when the water quantity of distillate in esterification reaches theoretical value 90% when for esterification terminal, wherein the addition of antimony oxide is the 0.03% of terephthalic acid (TPA) weight, tricresyl phosphate The addition of phenyl ester is the 0.02% of terephthalic acid (TPA) weight；
(c) polycondensation reaction；After esterification, start the polycondensation reaction in low vacuum stage under condition of negative pressure, Pressure is steadily evacuated to absolute pressure as 455Pa by normal pressure in 42min, reaction temperature is 264 DEG C, reaction time 45min, It then proceedes to vacuumize, carries out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is made to be further reduced to absolute pressure as 85Pa, Reaction temperature is 285 DEG C, reaction time 75min, and modified poly ester is made, and the wherein strand of modified poly ester is included to benzene two Formic acid segment, ethylene glycol segment and 3,3- dipropyl -1,5-PD segment, the content of cyclic oligomer is in modified poly ester 0.45wt%, number-average molecular weight 26500, molecular weight distributing index 2.2,3,3- dipropyl -1,5-PD in modified poly ester The molar content of segment is the 4.5% of terephthalic acid (TPA) segment molar content.
(2) modified poly ester through solid phase polycondensation viscosified, melted, measured, squeezed out, cooled down, oiled, stretched, thermal finalization and volume Around obtained high-strength polyester industrial fiber.Wherein, the inherent viscosity of solid phase polycondensation thickening post-modification polyester is 1.2dL/g；Spinning group The replacement cycle of part is 41 days, clears up the cycle stretch-out 44% of spinneret, and the maceration extracts of first bath are D- in two bath infusion processes 417, the maceration extract of the second bath is RFL.During cooling, keep longitudinal direction height constant, increase the cross-sectional area of slow cooling chamber, simultaneously Slow cooling chamber keeps the plate face temperature of spinneret by the way of heat preservation, and slow cooling chamber configuration is substantially the same manner as Example 3, no With being that it only has thermal insulation board, it is not superimposed thermal insulation board under thermal insulation board.
The spinning technology parameter of high-strength polyester industrial fiber is shown in Table 1.
Final high-strength polyester industrial fiber various performance parameters obtained are shown in Table 2.
Embodiment 8
A kind of preparation method of high-strength polyester industrial fiber, is as follows：
(1) modified poly ester is prepared：
(a) 4,4- dipropyl -1,7- heptandiols are prepared；At 92 DEG C, under nitrogen atmosphere, by 4,4- dipropyl-butyraldehyde, second Then aldehyde and triethylamine react 20min have concentrate addition in the hydrogenation reactor of thunder girl's Raney nickel, in 2.914MPa Hydrogen press and 100 DEG C at react, reaction finish, cooling, catalyst is precipitated.After the processing of solution spent ion exchange resin, decompression is steamed Water detaches, and purification obtains 4,4- dipropyl -1,7- heptandiols, wherein the structural formula of 4,4- dipropyl -1,7- heptandiols is such as Under：
(b) esterification；It is 1 by molar ratio:1.9:0.04 terephthalic acid (TPA), ethylene glycol and 4,4- dipropyl -1,7- Heptandiol is made into slurry, adds in antimony glycol and trimethyl phosphate after mixing, and pressurizeing in nitrogen atmosphere, it is anti-be esterified Should, moulding pressure 0.3MPa, the temperature of esterification is 260 DEG C, when the water quantity of distillate in esterification reaches theoretical value It is esterification terminal when 93%, wherein the addition of antimony glycol is the 0.04% of terephthalic acid (TPA) weight, trimethyl phosphate Addition be terephthalic acid (TPA) weight 0.03%；
(c) polycondensation reaction；After esterification, start the polycondensation reaction in low vacuum stage under condition of negative pressure, Pressure is steadily evacuated to absolute pressure as 475Pa by normal pressure in 45min, reaction temperature is 265 DEG C, reaction time 48min, It then proceedes to vacuumize, carries out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is made to be further reduced to absolute pressure as 88Pa, Reaction temperature is 283 DEG C, reaction time 80min, and modified poly ester is made, and the wherein strand of modified poly ester is included to benzene two Formic acid segment, ethylene glycol segment and 4,4- dipropyl -1,7- heptandiol segment, the content of cyclic oligomer is in modified poly ester 0.6wt%, number-average molecular weight 23000, molecular weight distributing index 2.0,4,4- dipropyl -1,7- heptandiols in modified poly ester The molar content of segment is the 3% of terephthalic acid (TPA) segment molar content；
(2) modified poly ester through solid phase polycondensation viscosified, melted, measured, squeezed out, cooled down, oiled, stretched, thermal finalization and volume Around obtained high-strength polyester industrial fiber.Wherein, the inherent viscosity of solid phase polycondensation thickening post-modification polyester is 1.15L/g；Spinning group The replacement cycle of part is 44 days, clears up the cycle stretch-out 45% of spinneret, and the maceration extracts of first bath are D- in two bath infusion processes 417, the maceration extract of the second bath is RFL.During cooling, keep longitudinal direction height constant, increase the cross-sectional area of slow cooling chamber, simultaneously Slow cooling chamber keeps the plate face temperature of spinneret by the way of heat preservation, and slow cooling chamber configuration is substantially the same manner as Example 4, no With being that it only has thermal insulation board, it is not superimposed thermal insulation board under thermal insulation board.
The spinning technology parameter of high-strength polyester industrial fiber is shown in Table 1.
Final high-strength polyester industrial fiber various performance parameters obtained are shown in Table 2.
Embodiment 9
A kind of preparation method of high-strength polyester industrial fiber, is as follows：
(1) modified poly ester is prepared：
(a) 4- methyl -4- (1,1- dimethyl ethyls) -1,7- heptandiols are prepared；At 92 DEG C, under nitrogen atmosphere, by 4- first Then concentrate addition is had thunder girl's nickel to urge by base -4- (1,1- dimethyl ethyl)-butyraldehyde, propionic aldehyde and triethylamine react 20min It in the hydrogenation reactor of agent, is reacted at 2.914MPa hydrogen pressure and 100 DEG C, reaction is finished, and cooling is precipitated catalyst, solution After spent ion exchange resin processing, water is steamed in decompression, detaches, and purification obtains 4- methyl -4- (1,1- dimethyl ethyl) -1,7- heptan The structural formula of glycol, wherein 4- methyl -4- (1,1- dimethyl ethyl) -1,7- heptandiols is as follows：
(b) esterification；It is 1 by molar ratio:2.0:0.05 terephthalic acid (TPA), ethylene glycol and 4- methyl -4- (1,1- Dimethyl ethyl) -1,7- heptandiols are made into slurry, antimony acetate and trimethyl phosphate are added in after mixing, in nitrogen atmosphere Pressurization carries out esterification, and moulding pressure is normal pressure MPa, and the temperature of esterification is 251 DEG C, when the water in esterification evaporates Output is esterification terminal when reaching the 96% of theoretical value, and wherein the addition of antimony acetate is terephthalic acid (TPA) weight 0.05%, the addition of trimethyl phosphate is the 0.04% of terephthalic acid (TPA) weight；
(c) polycondensation reaction；After esterification, start the polycondensation reaction in low vacuum stage under condition of negative pressure, Pressure is steadily evacuated to absolute pressure as 420Pa by normal pressure in 30min, reaction temperature is 267 DEG C, reaction time 50min, It then proceedes to vacuumize, carries out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is made to be further reduced to absolute pressure as 80Pa, Reaction temperature is 280 DEG C, reaction time 90min, and modified poly ester is made, and the wherein strand of modified poly ester is included to benzene two Formic acid segment, ethylene glycol segment and 4- methyl -4- (1,1- dimethyl ethyl) -1,7- heptandiol segments, it is cyclic annular in modified poly ester The content of oligomer is 0.25wt%, number-average molecular weight 24000, molecular weight distributing index 2.2,4- methyl in modified poly ester- The molar content of 4- (1,1- dimethyl ethyls) -1,7- heptandiol segments is the 4% of terephthalic acid (TPA) segment molar content；
(2) modified poly ester viscosify, melt through solid phase polycondensation, measuring, squeezing out, cooling down, oiling, stretching, thermal finalization and winding High-strength polyester industrial fiber is made.Wherein, the inherent viscosity of solid phase polycondensation thickening post-modification polyester is 1.09dL/g；Spinning group The replacement cycle of part is 45 days, clears up the cycle stretch-out 35% of spinneret, and the maceration extracts of first bath are D- in two bath infusion processes 417, the maceration extract of the second bath is RFL.During cooling, keep longitudinal direction height constant, increase the cross-sectional area of slow cooling chamber, simultaneously Slow cooling chamber keeps the plate face temperature of spinneret by the way of heat preservation, and slow cooling chamber configuration is substantially the same manner as Example 1, no With septa thickness is for 3mm, filling thermal insulation material is rock wool in thermal insulation board, and heat resisting temperature is 410 DEG C, keeps the temperature plate thickness For 50mm, stainless steel plate wall thickness is 1.5mm, and heat-insulated plate thickness is 45mm.
The spinning technology parameter of high-strength polyester industrial fiber is shown in Table 1.
Final high-strength polyester industrial fiber various performance parameters obtained are shown in Table 2.
Embodiment 10
A kind of preparation method of high-strength polyester industrial fiber, is as follows：
(1) modified poly ester is prepared：
(a) 3- methyl -3- amyls -1,6-HD is prepared；At 90 DEG C, under nitrogen atmosphere, by 3- methyl -3- amyls-the third Then aldehyde, propionic aldehyde and triethylamine react 20min have concentrate addition in the hydrogenation reactor of thunder girl's Raney nickel, 2.914MPa hydrogen press and 100 DEG C at react, reaction finish, cooling, catalyst is precipitated.After the processing of solution spent ion exchange resin, Water is steamed in decompression, detaches, and purification obtains 3- methyl -3- amyl -1,6- hexylene glycols, wherein 3- methyl -3- amyl -1,6- hexylene glycols Structural formula it is as follows：
(b) esterification；It is 1 by molar ratio:1.2:0.06 terephthalic acid (TPA), ethylene glycol and 3- methyl -3- amyls - 1,6- hexylene glycol is made into slurry, adds in antimony glycol and Trimethyl phosphite after mixing, and pressurizeing in nitrogen atmosphere carries out Esterification, moulding pressure 0.1MPa, the temperature of esterification is 255 DEG C, when the water quantity of distillate in esterification reaches reason By value 92% when for esterification terminal, wherein the addition of antimony glycol is the 0.01% of terephthalic acid (TPA) weight, phosphorous The addition of sour trimethyl is the 0.01% of terephthalic acid (TPA) weight；
(c) polycondensation reaction；After esterification, start the polycondensation reaction in low vacuum stage under condition of negative pressure, Pressure is steadily evacuated to absolute pressure as 490Pa by normal pressure in 50min, reaction temperature is 269 DEG C, reaction time 30min, It then proceedes to vacuumize, carries out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is made to be further reduced to absolute pressure as 100Pa, Reaction temperature is 281 DEG C, reaction time 55min, and modified poly ester is made, and the wherein strand of modified poly ester is included to benzene two Formic acid segment, ethylene glycol segment and 3- methyl -3- amyl -1,6- hexylene glycol segments, the content of cyclic oligomer in modified poly ester For 0.1wt%, number-average molecular weight 20000, molecular weight distributing index 1.9, in modified poly ester 3- methyl -3- amyls -1,6- oneself The molar content of glycol segment is the 3.5% of terephthalic acid (TPA) segment molar content；
(2) modified poly ester through solid phase polycondensation viscosified, melted, measured, squeezed out, cooled down, oiled, stretched, thermal finalization and volume Around obtained high-strength polyester industrial fiber.Wherein, the inherent viscosity of solid phase polycondensation thickening post-modification polyester is 1.1dL/g；Spinning group The replacement cycle of part is 42 days, clears up the cycle stretch-out 35% of spinneret, and the maceration extracts of first bath are D- in two bath infusion processes 417, the maceration extract of the second bath is RFL.During cooling, keep longitudinal direction height constant, increase the cross-sectional area of slow cooling chamber, simultaneously Slow cooling chamber keeps the plate face temperature of spinneret by the way of heat preservation, and slow cooling chamber configuration is substantially the same manner as Example 1, no With being that it only has thermal insulation board, it is not superimposed thermal insulation board under thermal insulation board.
The spinning technology parameter of high-strength polyester industrial fiber is shown in Table 1.
Final high-strength polyester industrial fiber various performance parameters obtained are shown in Table 2.
Embodiment 11
A kind of preparation method of high-strength polyester industrial fiber, is as follows：
(1) modified poly ester is prepared：
(a) 3,3- diamyl -1,5- pentanediols are prepared；At 95 DEG C, under nitrogen atmosphere, by 3,3- diamyl-propionic aldehyde, second Then aldehyde and triethylamine react 20min have concentrate addition in the hydrogenation reactor of thunder girl's Raney nickel, in 2.914MPa Hydrogen press and 100 DEG C at react, reaction finish, cooling, catalyst is precipitated.After the processing of solution spent ion exchange resin, decompression is steamed Water detaches, and purification obtains 3,3- diamyl -1,5-PD, wherein the structural formula of 3,3- diamyl -1,5-PD is such as Under：
(b) esterification；It is 1 by molar ratio:2.0:0.03 terephthalic acid (TPA), ethylene glycol and 3,3- diamyl -1,5- Pentanediol is made into slurry, adds in antimony acetate and Trimethyl phosphite after mixing, and pressurizeing in nitrogen atmosphere, it is anti-be esterified Should, moulding pressure 0.2MPa, the temperature of esterification is 250 DEG C, when the water quantity of distillate in esterification reaches theoretical value It is esterification terminal when 97%, wherein the addition of antimony acetate is the 0.01% of terephthalic acid (TPA) weight, Trimethyl phosphite Addition be terephthalic acid (TPA) weight 0.05%；
(c) polycondensation reaction；After esterification, start the polycondensation reaction in low vacuum stage under condition of negative pressure, Pressure is steadily evacuated to absolute pressure as 500Pa by normal pressure in 45min, reaction temperature is 260 DEG C, reaction time 40min, It then proceedes to vacuumize, carries out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is made to be further reduced to absolute pressure as 92Pa, Reaction temperature is 277 DEG C, reaction time 80min, and modified poly ester is made, and the wherein strand of modified poly ester is included to benzene two Formic acid segment, ethylene glycol segment and 3,3- diamyl -1,5-PD segment, the content of cyclic oligomer is in modified poly ester 0.35wt%, number-average molecular weight 25500, molecular weight distributing index 1.8,3,3- diamyl -1,5-PD in modified poly ester The molar content of segment is the 5% of terephthalic acid (TPA) segment molar content；
(2) modified poly ester through solid phase polycondensation viscosified, melted, measured, squeezed out, cooled down, oiled, stretched, thermal finalization and volume Around obtained high-strength polyester industrial fiber.Wherein, the inherent viscosity of solid phase polycondensation thickening post-modification polyester is 1.2dL/g；Spinning group Replacement cycle of part 47 days, clear up the cycle stretch-out 40% of spinneret, the maceration extracts of first bath are D- in two bath infusion processes 417, the maceration extract of the second bath is RFL.During cooling, keep longitudinal direction height constant, increase the cross-sectional area of slow cooling chamber, simultaneously Slow cooling chamber keeps the plate face temperature of spinneret by the way of heat preservation, and slow cooling chamber configuration is substantially the same manner as Example 2, no With being that it only has thermal insulation board, it is not superimposed thermal insulation board under thermal insulation board.
The spinning technology parameter of high-strength polyester industrial fiber is shown in Table 1.
Final high-strength polyester industrial fiber various performance parameters obtained are shown in Table 2.
Table 1
Table 2
Note：A represents the central value (%) of the elongation of 4.0cN/dtex loads in table 2, and B represents 4.0cN/dtex loads Elongation deviation ratio (%), C represents dry-hot shrinkage (%) under the conditions of 177 DEG C, 10min and 0.05cN/dtex.

Claims (10)

1. a kind of high-strength polyester industrial fiber, it is characterized in that：The material of high-strength polyester industrial fiber be modified poly ester, modified poly ester Strand include terephthalic acid (TPA) segment, ethylene glycol segment and branched dihydric alcohol segment, the knot of branched dihydric alcohol Structure formula is as follows：
In formula, R1And R2It is each independently selected from the straight-chain alkyl-sub that carbon atom number is 1~3, R3It is 1~5 selected from carbon atom number Alkyl, R4Selected from the alkyl that carbon atom number is 2~5；
Fracture strength >=8.1cN/dtex of high-strength polyester industrial fiber.
A kind of 2. high-strength polyester industrial fiber according to claim 1, which is characterized in that the high-strength polyester industrial fiber Fiber number for 275~1100dtex, line density deviation ratio is ± 1.5%, fracture strength CV value≤3.0%, in elongation at break Center value is 13.5~17.0%, and elongation at break deviation ratio is ± 1.5%, and extension at break CV values≤8.0%, 4.0cN/dtex are born The central value of the elongation of lotus is that the deviation ratio of the elongation of 5.7~6.5%, 4.0cN/dtex loads is ± 0.8%, 177 DEG C, the dry-hot shrinkage under the conditions of 10min and 0.05cN/dtex be 4.3~9.3%, network is 6 ± 2/m, and oil content is 0.4~0.9%.
A kind of 3. high-strength polyester industrial fiber according to claim 1 or 2, which is characterized in that the modified poly ester middle ring Content≤0.6wt% of shape oligomer；
The number-average molecular weight 20000~27000 of the modified poly ester, molecular weight distributing index are 1.8~2.2；
In the modified poly ester molar content of branched dihydric alcohol segment for terephthalic acid (TPA) segment molar content 3~ 5%；
The branched dihydric alcohol is 2- Ethyl-2-Methyl -1,3- propylene glycol, 2,2- diethyl -1,3- propylene glycol, 2- fourths Base -2- ethyl -1,3- propylene glycol, 3,3- diethyl -1,5- pentanediols, 4,4- diethyl -1,7- heptandiols, 4,4- bis- (1,-first Base ethyl) -1,7- heptandiols, 3,3- dipropyl -1,5- pentanediols, 4,4- dipropyl -1,7- heptandiols, 4- methyl -4- (1,1- Dimethyl ethyl) -1,7- heptandiols, 3- methyl -3- amyls -1,6-HD or 3,3- diamyl -1,5- pentanediols.
A kind of 4. high-strength polyester industrial fiber according to claim 3, which is characterized in that the preparation side of the modified poly ester Method is：Terephthalic acid (TPA), ethylene glycol and the branched dihydric alcohol are successively carried out to esterification and polycondensation after mixing Modified poly ester is obtained by the reaction；The specific preparation process of the modified poly ester is as follows：
(1) esterification；
Terephthalic acid (TPA), ethylene glycol and the branched dihydric alcohol are made into slurry, catalyst is added in and stabilizer mixing is equal After even, the pressurization progress esterification in nitrogen atmosphere, moulding pressure is normal pressure~0.3MPa, and the temperature of esterification is 250 ~260 DEG C, be esterification terminal when the water quantity of distillate in esterification reaches more than 90% theoretical value；
(2) polycondensation reaction；
After esterification, start the polycondensation reaction in low vacuum stage under condition of negative pressure, the staged pressure is in 30~50min Interior to be steadily evacuated to absolute pressure 500Pa hereinafter, reaction temperature is 260~270 DEG C by normal pressure, the reaction time is 30~50min, so After continue to vacuumize, carry out the polycondensation reaction of high vacuum stage of Fig, reaction pressure is made to be further reduced to absolute pressure 100Pa hereinafter, Reaction temperature is 275~285 DEG C, and the reaction time is 50~90min, and modified poly ester is made.
5. a kind of high-strength polyester industrial fiber according to claim 4, which is characterized in that in step (1), terephthaldehyde The molar ratio of acid, ethylene glycol and the branched dihydric alcohol is 1:1.2~2.0:0.03~0.06, the addition of the catalyst Measure 0.01~0.05% for terephthalic acid (TPA) weight, the addition of the stabilizer for terephthalic acid (TPA) weight 0.01~ 0.05%；
The catalyst is antimony oxide, antimony glycol or antimony acetate, and the stabilizer is triphenyl phosphate, trimethyl phosphate Or Trimethyl phosphite.
6. a kind of such as method of high-strength polyester industrial fiber of Claims 1 to 5 any one of them is prepared, it is characterized in that：By institute State modified poly ester viscosify, melt through solid phase polycondensation, measuring, squeezing out, cooling down, oiling, stretching, thermal finalization and winding be made high-strength Polyester industrial fiber；
It during the cooling, keeps longitudinal direction height constant, increases the cross-sectional area of slow cooling chamber, while slow cooling chamber is using heat preservation Mode keeps the plate face temperature of spinneret.
7. the according to the method described in claim 6, it is characterized in that, inherent viscosity of solid phase polycondensation thickening post-modification polyester For 1.0~1.2dL/g；Clear up the cycle stretch-out of spinneret 35~45%, replacement cycle >=40 day of filament spinning component.
8. the method according to the description of claim 7 is characterized in that the cross-sectional area of the increase slow cooling chamber refers to keeping Under the premise of the spinneret that is connect with slow cooling chamber is constant, the cross section of slow cooling chamber is changed to rectangle by circle；The slow cooling Chamber is surrounded by thermal insulation board and partition, the embedded bottom for hanging on spinning manifold of thermal insulation board, and hollow chamber is opened up in thermal insulation board I, partition, which is assigned into hollow chamber I, is divided into multiple slow cooling chambers, there is one block of spinneret in each slow cooling chamber；
Stainless steel plate of the thermal insulation board for the thermal insulation material of internal 400 DEG C of heatproof of filling or more, the thickness of thermal insulation board for 30~ 50mm, the wall thickness of stainless steel plate is 0.9~1.5mm；
The thermal insulation material is rock wool or ceramic fibre；
The thickness of the partition is 1~3mm；
Polylith spinneret in the hollow chamber I is round spinneret, the diameter of polylith spinneret is identical, the center of circle be located at it is same It is on straight line and close adjacent；
The cross section of the hollow chamber I is rectangle, and the side for being parallel to polylith spinneret circle center line connecting is long side, perpendicular to length While while be short side；
The length of the long side is 1.2 times of the sum of the polylith spinneret board diameter, and the length of the short side is the spinneret 1.7 times of diameter.
9. according to the method described in claim 8, it is characterized in that, be superimposed thermal insulation board under the thermal insulation board, the material of thermal insulation board It is identical with thermal insulation board, hollow chamber II is opened up in thermal insulation board, hollow chamber II is identical with the cross-sectional shape of hollow chamber I；
In the position that hollow chamber II connects with hollow chamber I, two sides of II cross section of hollow chamber respectively with hollow chamber I Two short sides of cross section overlap, and the length on two sides is more than two short sides；
The thickness of the thermal insulation board is 25~45mm.
10. the according to the method described in claim 8, it is characterized in that, spinning technology parameter of the high-strength polyester industrial fiber It is as follows：
It stretches, the technological parameter of thermal finalization is：
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