CN109735936A - The preparation method of polyester industrial yarn for heavy-duty hoisting band - Google Patents
The preparation method of polyester industrial yarn for heavy-duty hoisting band Download PDFInfo
- Publication number
- CN109735936A CN109735936A CN201811614105.0A CN201811614105A CN109735936A CN 109735936 A CN109735936 A CN 109735936A CN 201811614105 A CN201811614105 A CN 201811614105A CN 109735936 A CN109735936 A CN 109735936A
- Authority
- CN
- China
- Prior art keywords
- polyester
- heavy
- preparation
- industrial yarn
- polyester industrial
- 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.)
- Granted
Links
Landscapes
- Artificial Filaments (AREA)
- Polyesters Or Polycarbonates (AREA)
Abstract
The present invention relates to a kind of preparation methods of polyester industrial yarn for heavy-duty hoisting band, the preparation method comprises the following steps: by polyester fondant carry out solid phase polycondensation thickening, melting, metering, extrusion, cooling, oil, combine, stretch, twist, thermal finalization, heat treatment without tension and winding are made and are used for the polyester industrial yarn of heavy-duty hoisting band；Solid phase polycondensation viscosify before polyester the preparation method comprises the following steps: by the Sb of terephthalic acid (TPA), ethylene glycol and doping vario-property2O3Powder successively carries out esterification and polycondensation reaction after mixing；Heat treatment without tension refers to the space by polyester tow in the state that the over feed rate(OFR) of winding is 3.0~5.0% by 200~240 DEG C.The present invention passes through the mutual cooperation of heat treatment temperature and higher over feed rate(OFR), improves the integrality of fiber crystallization, reduces the thermal contraction in its application process, while reducing the additive amount of antimony-based catalyst, simple process and low cost, and application prospect is good.
Description
Technical field
The invention belongs to polyester fiber technical fields, are related to a kind of preparation side of polyester industrial yarn for heavy-duty hoisting band
Method.
Background technique
Wirerope is a kind of traditional lifting device, since it is easy to cause a degree of damage and destruction to article,
Hanging belt came into being since the last century 50's, gradually instead of wirerope, and was widely used in such as ship, port
Mouth, metallurgy, steel, machinery, construction site, mine, petroleum, chemical industry, power station, harbour, harbour, electric power, electronics, warehouse, fortune
The fields such as defeated, military.
Since hanging belt is required to bear biggish pulling force and its operating environment is more severe, this proposes its material
Certain requirement.Polyester industrial fiber has the advantages that modulus is high, elongation is low, heat-resist, acid resistance is strong and endurance etc., at
For the common material of hanging belt.Hanging belt made of polyester industrial fiber also has the following characteristics that 1) matter other than the above advantage
Ground is soft, therefore the use of hanging belt can be reduced to the surface damage received vulnerable to operation, especially be reduced to lacquered surface
Damage；2) light and fast, the weight of hanging belt are the 25% of same pulling force metallic ropes tool, thus it is easy to carry, carry and
Storage, while being also very easy to operate；3) securely and reliably, for the tensile properties of hanging belt close to wirerope, safety coefficient is high.
But heavy-duty hoisting band load-bearing is larger, is easy to be heated after long working, polyester industrial fiber can occur after heated
Irreversible thermal contraction, by repeatedly after-contraction will become apparent from repeatedly.If heavy-duty hoisting band is in this state for a long time, hold
It is easily broken, influences using safe.Therefore the pet copolyester industrial yarn of heavy-duty hoisting band is to the more demanding of percent thermal shrinkage, so
And the percent thermal shrinkage of polyester industrial fiber is often higher at present, is difficult to meet the requirement of heavy-duty hoisting band.
In addition, synthetic method used in PET polyester material production at present is broadly divided into ester-interchange method (DMT method) and straight contracting
(PTA method), and the catalyst used in process of polyester synthesizing, mainly use antimony-based catalyst in the market.With society
Continue to develop, the requirement in terms of environmental protection is just being gradually increased in people, environmental protection production be modern industrial production must
Right trend.Metallic antimony can all bring harm to man and nature, contain the metals such as antimony currently for PET material to body nocuousness
Environmental issue caused the extensive concern of people, but due to compared with other catalyst, the catalysis of the antimony such as antimony oxide system
The advantages that agent is active placed in the middle, cheap and lower to side reaction promotion, therefore, currently, antimony-based catalyst is on the market
Still it is widely applied, market use ratio reaches 90%, and antimony-based catalyst is also difficult to be substituted comprehensively by other catalyst.And mesh
Preceding common antimony-based catalyst such as Sb on the market2O3Additive amount in process of polyester synthesizing is larger, the additive amount of antimony-based catalyst
The larger influence generated to environment is also larger, is unfavorable for the environmental protection production of polyester, the small antimony-based catalyst of additive amount can not be to ginseng
It is catalyzed with the reacting for all raw materials of polyester synthesis, is unable to satisfy the needs of production of polyester.
Therefore, the terylene industrial for heavy-duty hoisting band that a kind of percent thermal shrinkage is small and antimony-based catalyst additive amount is small is developed
The great realistic meaning of preparation method of silk.
Summary of the invention
The purpose of the present invention is overcoming prior art percent thermal shrinkage larger and the biggish defect of antimony-based catalyst dosage, provide
A kind of preparation method for the polyester industrial yarn for heavy-duty hoisting band that percent thermal shrinkage is small and antimony-based catalyst additive amount is small.
In order to achieve the above objectives, The technical solution adopted by the invention is as follows:
The preparation method of polyester industrial yarn for heavy-duty hoisting band, by polyester fondant carry out solid phase polycondensation thickening, melting,
It measures, squeezes out, cool down, oil, combining, stretching, twisting, thermal finalization, heat treatment without tension and winding are made for heavy-duty hoisting band
Polyester industrial yarn；
Polyester the preparation method comprises the following steps: by terephthalic acid (TPA), ethylene glycol and doping vario-property before the solid phase polycondensation viscosifies
Sb2O3Powder successively carries out esterification and polycondensation reaction after mixing；
Sb2O3The process of doping vario-property are as follows: first by metal ion Mx+Solution with contain Sb3+Solution be uniformly mixed,
Then the pH value that precipitating reagent is added dropwise to mixed liquor is 9~10, finally calcines precipitated product and crushes；Metal ions Mx+For Mg2+、
Ca2+、Ba2+And Zn2+One or more of；
The heat treatment without tension refers to the space by polyester tow in relaxed state appropriate Jing Guo certain temperature；
The relaxed state appropriate refers to that the over feed rate(OFR) of winding is 3.0~5.0%；
The certain temperature refers to 200~240 DEG C.
The present invention reduces the shrinking percentage of polyester industrial fiber by the mutual cooperation of heat treatment temperature and over feed rate(OFR), and fiber exists
When heat treatment, macromolecular chain folded chain easy to form in amorphous area is conducive to the further growth of crystal grain, at this time crystallinity
It increases, along with the raising of crystallinity, fiber can generate a certain amount of contraction, on the one hand the present invention is disappeared by improving over feed rate(OFR)
On the other hand influence in addition to high elastic deformation to winding eliminates the influence of the contraction of fiber during crystallinity improves.
The present invention is also by by metal ion Mx+Solution with contain Sb3+Solution first be uniformly mixed reprecipitation finally forge
It burns to realize the doping and blending of metal oxide and antimony oxide with certain catalytic activity, metal oxide is
After one or more of MgO, CaO, BaO and ZnO, metal oxide of the invention and antimony oxide doping, metal oxide
By inhibit antimony oxide crystallization and cubic crystal antimony oxide crystal grain grow up and same order elements antimony enters antimony
Lattice position makes antimony oxide crystal generate defect, and crystal habit generates variation, and crystallite dimension becomes smaller, and improves three oxidations two
The specific surface area S of antimony catalystg, while metal can also be enriched in part antimony oxide plane of crystal, make antimony oxide list
Active r on bit surface areasIncrease, specific surface area SgWith the active r in per surface areasBigger, the catalytic activity of catalyst is cured
Height is allowed the invention in low Sb2O3Catalyzing and synthesizing for polyester is realized under additive amount, is good for the environment production.
As a preferred technical scheme:
The preparation method of polyester industrial yarn as described above for heavy-duty hoisting band, the terylene work for heavy-duty hoisting band
The filament number of industry silk is 8.0~9.0dtex, and breaking strength >=8.2N, line density is 3300~4400dtex, line density deviation
Rate is ± 2.0%, and elongation at break is 6.5~9.5%, the processing and mechanicalness of ultralow shrinkage type polyester industrial fiber of the invention
Can be suitable with the low shrinkage polyester industrial filament performance of the prior art, it is dry under the conditions of 177 DEG C × 10min × 0.05cN/dtex
Percent thermal shrinkage is 7.0~10.0%, and internet pricing is 6~14/m, and the lower shrinkage type polyester industrial fiber of the prior art is in the test
Under the conditions of dry-hot shrinkage be 10.0~13.0%, comparison is as can be seen that present invention significantly reduces the heat of polyester industrial fiber
Shrinking percentage.
The preparation method of polyester industrial yarn as described above for heavy-duty hoisting band, the metal ion Mx+Solution
Concentration be 0.5~1.0mol%, solvent is water, the anion in solution be NO3 -；It is described to contain Sb3+Solution be concentration 5~
The Sb of 10mol%2O3Solution, solvent is oxalic acid；The precipitating reagent is the ammonium hydroxide of concentration 2mol/L；When precipitating starts, mix molten
Metal ions M in liquidx+With Sb3+Molar ratio be 1~3:100, Sb2O3It is the highest polyester catalyst of current cost performance, this hair
It is bright to pass through infiltration metal oxide (i.e. M2OX) inhibit antimony oxide (Sb2O3) crystallization and cubic crystal antimony oxide crystal grain
Grow up, while metal ions Mx+The lattice position of antimony and entrance antimony can be replaced, so that antimony oxide crystal generates defect, to mention
The catalytic activity of high antimony oxide.If blended metal oxide amount is very few (molar ratio is too low), to antimony oxide crystal grain shadow
Sound is relatively low, and excessive (molar ratio is excessively high) can make the main body Sb of catalyst3+Fall is bigger than normal, to raising antimony oxide
Catalytic activity is unfavorable；
Precipitated product is washed and is dried before the calcining, dry temperature be 105~110 DEG C, the time be 2~
3h；The process of the calcining are as follows: keep the temperature 2~3h after being warming up to 400 DEG C first, 1~2h is kept the temperature after then heating to 900 DEG C, most
It cools down in air afterwards；
Sb2O3It is crushed to obtain powder of the average grain diameter less than 0.5 micron after doping vario-property.
The preparation method of polyester industrial yarn as described above for heavy-duty hoisting band, polyester before the solid phase polycondensation viscosifies
Preparation step it is as follows:
(1) esterification；
Terephthalic acid (TPA) and ethylene glycol are made into slurry, the Sb of doping vario-property is added2O3Powder, delustering agent and stabilizer are mixed
After closing uniformly, pressurization carries out esterification in nitrogen atmosphere, and 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 90% or more of theoretical value；
(2) polycondensation reaction；
After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, the staged pressure 30~
Absolute pressure 500Pa being steadily evacuated to by normal pressure in 50min hereinafter, reaction temperature is 250~260 DEG C, the reaction time is 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 270~282 DEG C, the reaction time is 50~90min.
The preparation method of polyester industrial yarn as described above for heavy-duty hoisting band, the terephthalic acid (TPA) and ethylene glycol
Molar ratio be 1:1.2~2.0, the Sb of the doping vario-property2O3The additional amount of powder, delustering agent and stabilizer is respectively to benzene
0.012~0.015wt%, 0.20~0.25wt% and the 0.01~0.05wt% of dioctyl phthalate additional amount.Polyester in the prior art
Sb in synthesis process2O3Additional amount be usually terephthalic acid (TPA) additional amount 0.02~0.04wt%, the addition of antimony-based catalyst
Amount is high, and this is mainly due to undoped Sb2O3Active r in per surface areasLow and specific surface area SgIt is small, therefore Sb2O3It is whole
The catalytic activity of body is lower, and the present invention passes through to Sb2O3It is doped modification, improves Sb2O3Activity, therefore significantly reduce
Sb in process of polyester synthesizing2O3Additive amount.
The preparation method of polyester industrial yarn as described above for heavy-duty hoisting band, the delustering agent are titanium dioxide,
The stabilizer is triphenyl phosphate, trimethyl phosphate or Trimethyl phosphite.
The preparation method of polyester industrial yarn as described above for heavy-duty hoisting band, polyester after the solid phase polycondensation viscosifies
Inherent viscosity be 1.0~1.2dL/g.
The preparation method of polyester industrial yarn as described above for heavy-duty hoisting band, the space of the certain temperature refers to
Space between a pair of arranged in parallel and non-coplanar hot plate, hot plate are located at last group of setting roller and winding in FDY equipment
Between roller；Along the traffic direction of polyester tow, the length of two hot plates is 3.0~4.0m, and the both ends of two hot plates flush；Polyester tow
When passing through among from two hot plates, the distance between two hot plates are 5~10mm.The present invention passes through control hot plate temperature (i.e. institute
State certain temperature) guarantee that macromolecular rearrangement can obtain energy, the length of hot plate is controlled to guarantee enough crystallization times, controls silk
Beam guarantees the efficiency of heat treatment at a distance from hot plate, and the mutual coordinated of three improves the integrality of fiber crystallization, and then subtracts
Thermal contraction during few fiber applications, wherein hot plate temperature is too low, it is difficult to guarantee that macromolecular rearrangement can obtain enough energy
Amount；Hot plate temperature is excessively high to destroy former established structure；Hot plate length is too short, and crystallization time is too short, influences fiber crystallization
Integrality influences fiber percent thermal shrinkage；The too long efficiency decline manufacturing apparatus waste of hot plate length；Tow too small appearance at a distance from hot plate
It easily causes and is contacted with the direct of tow；Tow excessive thermal efficiency at a distance from hot plate reduces
The preparation method of polyester industrial yarn as described above for heavy-duty hoisting band, last group of setting roller and winding
Spacing between roller is 300~400mm；Spacing between two hot plates and last group of setting roller is 200~300mm.
The preparation method of polyester industrial yarn as described above for heavy-duty hoisting band, the washing for heavy-duty hoisting band
The spinning technology parameter of synthetic fibre industrial yarn is as follows:
It stretches, the technological parameter of thermal finalization are as follows:
The process flow of the plying are as follows: creel → sensor → pressure tensioner → godet roller → guide rod or Network device →
Sensor → linear speed inductor → pulley → traverse filar guide → winding paper tube；
The technological parameter of the plying are as follows: number of share of stock 10~20,400~500m/min of speed.
Preparation process of the invention is not limited to that, only enumerates a kind of feasible technical solution herein.Concrete technology ginseng
Number is also not limited to this, can be adjusted according to actual needs.
Invention mechanism:
Fiber is in post-processing stretching process, and due to the effect of mechanical stress, fiber orientation degree is significantly increased and has
Certain crystallinity, to make elongate fiber and total deformation work reduce, during stretching, although the big portion of fibrogenic deformation
Dividing is expendable plastic deformation under room temperature, and often because crystallization is fixed, however some can be in room temperature
It is lower to restore because of the relaxation of tensile stress, or reply can be shunk in subsequent heat-treated, in the application process of fiber
In this shrink that reply be that the shrinking percentage of fiber will be largely affected by performance (such as security performance, endurance quality of fiber
Deng), it is assumed that the fiber is used as tire cord, and in use, cord fabric thread is stretched repeatedly, compressed, is bent tire, causes
Tire is heated, leads to curtain linear shrinkage creep, but when curtain linear shrinkage is excessive may knife cord fabric delamination, and then lead to tire
Disintegrate, this carrys out greatly hidden danger to using of seat belts for tire.
It is the shrinking percentage for reducing polyester industrial fiber as much as possible at present during the spin-drawing of polyester industrial fiber,
It generally requires to carry out nervous thermal finalization (carrying out shaping fiber under some tension using setting roller) after carrying out multiple tracks stretching,
To overfeeding of the over feed rate(OFR) for 1~2% is wound with after nervous thermal finalization, by carrying out nervous thermal finalization to fiber, in certain temperature
Under conditions of degree and some tension, the mobility of molecule segment is improved, so that intermolecular combination obtains even closer, raising fiber
Average grain size and crystallinity, to drop low-fiber shrinking percentage, but since fiber has certain height during stretching
Deformation is played, elastic recovery can be generated in the case where tension reduces, therefore, it is fixed that the speed of winding head has to be lower than last group heat
The speed of type roller needs certain over feed rate(OFR), is shunk, is expired with guaranteeing that the silk after stretching obtains a degree of low-tension
The final product quality of meaning and package prevent package from causing turned-down edge because of overtension, over feed rate(OFR) need to control in a certain range (1~
2%) it, crosses conference and adverse effect is generated to final product quality and package.Although can be to a certain extent by nervous thermal finalization+overfeeding
Reduce shrinking percentage, but in nervous heat-setting process, due to the length of fiber be fixed it is immutable, it is suppressed that macromolecular chain
Folding, thus the rate of grain growth is restricted, and causes to crystallize existing defects (crystallinity increases less), and only pass through
Control overfeeding can not reduce crystal defect, when this will lead to fiber obtained and is heat-treated in application process, fiber it is big
Strand and segment have higher activity, are easy to produce deorientation, cause fiber that a certain amount of shrink occurs and (shrink
Rate is larger).
In fact, the thermal finalization mode of fiber is not only nervous thermal finalization, further includes relaxation heat setting.Relaxation heat setting is again
Referred to as free shrink thermal finalization is fiber under complete no-station pole canopy or the lesser situation of tension, by certain temperature to fiber
Be heat-treated, under the conditions of relaxation heat setting, fiber can free shrink, the macromolecular chain folding easy to form in amorphous area
Chain is conducive to the further growth of crystal grain, in addition more abundant heat treatment time, therefore after heat treatment without tension, the knot of fiber
Brilliant degree increases more (compared to nervous thermal finalization), to make that fibrous inside high elastic deformation is restored while internal stress is filled
Divide relaxation, so that fibrogenic contraction reply is smaller when being heat-treated in application process.Current relaxation heat is fixed
Type be mainly used for polyester staple fiber carry out thermal finalization processing, heat treatment temperature is lower (130 DEG C or so), heat treatment time compared with
It is long, it is difficult to be suitable for long filament and produce.
The present invention by the way that the over feed rate(OFR) that polyester tow is wound is promoted to 3~5% in the process of polyester industrial fiber,
Hot plate arranged in parallel above and below a pair of is set between one of setting roller last in FDY equipment and take-up roll simultaneously, by polyester
Tow passes through among two hot plates, improves the crystallinity of polyester tow, has restored the high elastic deformation inside polyester tow, so that
Polyester tow internal stress obtains a certain amount of relaxation, and then reduces polyester industrial fiber when being heat-treated in application process and send out
Raw contraction is replied.The present invention reduces the receipts of polyester industrial fiber by the mutual cooperation of heat treatment temperature and higher over feed rate(OFR)
Shrinkage, fiber is in heat treatment, and macromolecular chain folded chain easy to form in amorphous area is conducive to the further life of crystal grain
Long, crystallinity increases at this time, and along with the raising of crystallinity, fiber can generate a certain amount of contraction, and the present invention is super by improving
The rate of feeding, on the one hand eliminates influence of the high elastic deformation to winding, on the other hand eliminates the receipts of fiber during crystallinity improves
The influence of contracting.In addition, the present invention is by the mutual cooperation of heat treatment temperature, hot plate length and tow and hot plate apart from three, one
Aspect overcomes the defect that prior art heat treatment without tension is not suitable for long filament production, on the other hand, improves fiber crystallization
Integrality improves the stability of fiber size, reduces the thermal contraction in its application process.
The mechanism that the present invention reduces antimony-based catalyst dosage is as follows:
Polyester catalyst mainly based on antimonial, such as antimony oxide, antimony glycol and antimony acetate, industrially gathers
The additional amount of antimony is greater than 200ppm in Lipase absobed, and since antimony is heavy metal, the progress in epoch is more next for the restriction of antimony catalyst
It is tighter, it, still can not be in the short time due to color and activity control etc. are various although the catalysis of titanium system is applied
Interior substitution antimony system.
The catalytic activity of catalyst and the specific surface area S of catalystg, in utilization rate of inner surface f and per surface area
Active rsDirectly proportional, certain for component catalyst, catalytic activity depend on the specific surface area S of the catalystgAnd inner surface
Utilization rate f, the active r in catalyst per surface areasOne timing, specific surface area is bigger, and catalytic activity is higher.
The present invention is co-precipitated to calcine again again by first solution blending realizes the gold with certain catalyzed polycondensation reactivity
Belong to the doping and blending of oxide and antimony oxide, one or more of metal oxide MgO, CaO, BaO and ZnO, valence
Position and the price of antimony have a certain difference, and there is also certain difference, these differences can change for ionic radius and antimony
The crystal plane structure of antimony oxide, to influence correlated performance.In addition, MgO, CaO, BaO, ZnO are white crystal, as poly-
Ester catalyst will not bring the variation on color.
Influence of the metal oxide to antimony oxide is mainly reflected in: on the one hand, metal oxide can inhibit three oxidations
The crystallization of two antimony and growing up for cubic crystal antimony oxide crystal grain make the specific surface area S of antimony oxide catalystgIt improves, mentions
The high catalytic activity of antimony oxide；On the other hand, metal understands the lattice position of same order elements antimony and entrance antimony, makes three oxidations two
Antimony crystal generates defect, and crystal habit generates variation, and crystallite dimension becomes smaller, specific surface area SgIncrease, while in partial crystals table
Face makes metal enrichment, makes the active r in its per surface areasIt improves, improves the catalytic activity of antimony oxide.As will be only had
There is the metal oxide of certain catalyzed polycondensation reactivity to be blended with antimony oxide simple physical, the catalysis of antimony oxide is living
Property will not significantly improve because simple physical be blended, crystal defect will not be generated, crystal habit does not generate variation, crystal grain
Size remains unchanged, and the total surface area of crystal is constant, will not have an impact to catalytic activity.
The present invention improves the catalytic activity of antimony trioxide, three oxygen by being doped to antimony trioxide in a degree
The catalytic activity for changing antimony, which improves, advantageously reduces the usage amount of antimony trioxide, in process of polyester synthesizing, protects in polycondensating process condition
It holds in the case that constant and polyester reaches identical index, after being doped using metal oxide to antimony trioxide, three oxidations
The usage amount of antimony can reduce 30% or more, efficiently solve the problems, such as that additive amount existing for current antimony trioxide is big, while can
Meet the needs of production of polyester.
The utility model has the advantages that
(1) preparation method of a kind of polyester industrial yarn for heavy-duty hoisting band of the invention, by heat treatment temperature with
The mutual cooperation of higher over feed rate(OFR) improves the integrality of fiber crystallization, reduces the thermal contraction in its application process；
(2) preparation method of a kind of polyester industrial yarn for heavy-duty hoisting band of the invention, by having certain catalysis
Active metal oxide improves antimony oxide specific surface area S to the doping vario-property of antimony oxidegAnd per surface area
On active rs, to improve the catalytic activity of antimony oxide, improve polymerization efficiency；And then polyester life can met
The additive amount for producing antimony-based catalyst when reducing synthesis polyester while needs effectively reduces the antimony discharge that fiber is made thereafter,
It is advantageously implemented environmentally friendly production.
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 hair
It is bright rather than limit the scope of the invention.In addition, it should also be understood that, after reading the content taught by the present invention, art technology
Personnel can make various changes or modifications the present invention, and such equivalent forms equally fall within the application the appended claims and limited
Fixed range.
Embodiment 1
A kind of preparation method of the polyester industrial yarn for heavy-duty hoisting band, the specific steps are as follows:
(1) polyester is prepared；
(1.1) Sb of doping vario-property is prepared2O3；
Mg (the NO that concentration is 0.8mol% by (1.1.1)3)2The Sb that aqueous solution and concentration are 8mol%2O3Solution mixing
Uniformly, Sb2O3The solvent of solution be oxalic acid, Mg in mixed liquor2+With Sb3+Molar ratio be 2:100；
The pH value that ammonium hydroxide to mixed liquor that concentration is 2mol/L is added dropwise in (1.1.2) is 9 to obtain precipitated product, then to precipitating
Product is washed and is dried, and dry temperature is 105 DEG C, time 2.5h；
(1.1.3) keeps the temperature 2.5h after the product after drying is warming up to 400 DEG C first, keeps the temperature after then heating to 900 DEG C
1.5h is crushed after finally cooling down in air and is obtained the Sb for the doping vario-property that average grain diameter is 0.4 micron2O3Powder；
(1.2) esterification；
Terephthalic acid (TPA) and ethylene glycol that molar ratio is 1:1.2 are made into slurry, the Sb of doping vario-property is added2O3Powder, two
After mixing, pressurization carries out esterification, moulding pressure 0.1MPa, ester in nitrogen atmosphere for titanium oxide and triphenyl phosphate
The temperature for changing reaction is 250 DEG C, is esterification terminal when the water quantity of distillate in esterification reaches the 93% of theoretical value, mixes
The Sb of miscellaneous modification2O3The additional amount of powder, titanium dioxide and triphenyl phosphate is respectively terephthalic acid (TPA) additional amount
0.012wt%, 0.20wt% and 0.02wt%；
(1.3) polycondensation reaction；
After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, the staged pressure is in 30min
The interior absolute pressure that is steadily evacuated to by normal pressure is 480Pa, and reaction temperature is 250 DEG C, reaction time 31min, then proceedes to take out true
Sky carries out the polycondensation reaction of high vacuum stage of Fig, and reaction pressure is made to be further reduced to absolute pressure 100Pa, reaction temperature 270
DEG C, polyester is made in reaction time 50min；
(1.4) solid phase polycondensation is carried out to polyester to viscosify to obtain the polyester fondant that inherent viscosity is 1.0dL/g；
(2) polyester fondant melted, measured, being squeezed out, being cooled down, being oiled, being combineeed, being stretched, being twisted, thermal finalization, relaxation
The polyester industrial yarn for heavy-duty hoisting band is made in heat treatment and winding；
The polyester tow that it is 4.9% by the over feed rate(OFR) of winding that heat treatment without tension, which refers to, is by a pair of arranged in parallel and non-co-planar
Temperature is the space between 200 DEG C of hot plate simultaneously, hot plate be located in FDY equipment last group of setting roller and take-up roll it
Between, along the traffic direction of polyester tow, the length of two hot plates is 3.0m, and the both ends of two hot plates flush, and polyester tow is from two hot plates
When centre passes through, the distance between two hot plates are 5mm, and the spacing between last group of setting roller and take-up roll is
300mm, the spacing between two hot plates and last group of setting roller are 200mm；
Spinning technology parameter is as follows:
It stretches, the technological parameter of thermal finalization are as follows:
The process flow of plying are as follows: creel → sensor → pressure tensioner → godet roller → guide rod or Network device → sensing
Device → linear speed inductor → pulley → traverse filar guide → winding paper tube, the technological parameter of plying are as follows: number of share of stock 10, speed 400m/
min。
The filament number of the final polyester industrial yarn obtained for heavy-duty hoisting band is 9.0dtex, and breaking strength is
8.4N, line density 4400dtex, line density deviation ratio be 0.5%, elongation at break 9.5%, 177 DEG C × 10min ×
Dry-hot shrinkage under the conditions of 0.05cN/dtex is 9.5%, and internet pricing is 14/m.
Comparative example 1
A kind of preparation method of polyester industrial yarn, step is substantially the same manner as Example 1, and difference is to adopt in step (1)
With conventional Sb2O3Replace the Sb of doping vario-property2O3Powder, conventional Sb2O3Additive amount be terephthalic acid (TPA) additional amount
0.03wt%, step (2) is without heat treatment without tension process, and winding speed is 2680m/min, and the over feed rate(OFR) of winding is
1.47%.The filament number of polyester industrial yarn obtained is 9.0dtex, breaking strength 8.3N, line density 4400dtex, line
Density variation rate is 0.5%, elongation at break 9.5%, xeothermic receipts under the conditions of 177 DEG C × 10min × 0.05cN/dtex
Shrinkage is 11.5%, and internet pricing is 14/m.
Comparative example 2
A kind of preparation method of polyester industrial yarn, step is substantially the same manner as Example 1, and difference is to adopt in step (1)
With conventional Sb2O3Replace the Sb of doping vario-property2O3Powder, conventional Sb2O3Additive amount be terephthalic acid (TPA) additional amount
0.03wt%.The filament number of polyester industrial yarn obtained be 9.0dtex, breaking strength 8.4N, line density 4400dtex,
Line density deviation ratio is 0.5%, and elongation at break 9.3% is xeothermic under the conditions of 177 DEG C × 10min × 0.05cN/dtex
Shrinking percentage is 9.2%, and internet pricing is 14/m.
Comparative example 3
A kind of preparation method of polyester industrial yarn, step is substantially the same manner as Example 1, difference be step (2) without
Heat treatment without tension process is crossed, and winding speed is 2680m/min, the over feed rate(OFR) of winding is 1.47%.Polyester industrial yarn obtained
Filament number be 9.0dtex, breaking strength 8.2N, line density 4400dtex, line density deviation ratio be 0.5%, fracture
Elongation is 10.5%, and dry-hot shrinkage under the conditions of 177 DEG C × 10min × 0.05cN/dtex is 12.5%, and internet pricing is
14/m.
Comprehensive analysis embodiment 1 and comparative example 1~3 are it can be found that the present invention uses the Sb of doping vario-property2O3Powder replacement
Conventional Sb2O3The additional amount of catalyst is significantly reduced while ensure that same catalytic activity, has been reached and has been reduced antimony discharge
Purpose.The present invention also significantly reduces the dry-hot shrinkage of polyester industrial fiber by adding heat treatment without tension process.
Embodiment 2
A kind of preparation method of the polyester industrial yarn for heavy-duty hoisting band, the specific steps are as follows:
(1) polyester is prepared；
(1.1) Sb of doping vario-property is prepared2O3；
Ca (the NO that concentration is 0.5mol% by (1.1.1)3)2The Sb that aqueous solution and concentration are 5mol%2O3Solution mixing
Uniformly, Sb2O3The solvent of solution be oxalic acid, Ca in mixed liquor2+With Sb3+Molar ratio be 1:100；
The pH value that ammonium hydroxide to mixed liquor that concentration is 2mol/L is added dropwise in (1.1.2) is 10 to obtain precipitated product, then to heavy
Shallow lake product is washed and is dried, and dry temperature is 110 DEG C, time 2h；
(1.1.3) keeps the temperature 2h after the product after drying is warming up to 400 DEG C first, keeps the temperature 1h after then heating to 900 DEG C,
It is crushed after finally cooling down in air and obtains the Sb for the doping vario-property that average grain diameter is 0.4 micron2O3Powder；
(1.2) esterification；
Terephthalic acid (TPA) and ethylene glycol that molar ratio is 1:1.5 are made into slurry, the Sb of doping vario-property is added2O3Powder, two
After mixing, pressurization carries out esterification in nitrogen atmosphere, and moulding pressure is normal pressure for titanium oxide and trimethyl phosphate, esterification
The temperature of reaction is 251 DEG C, is esterification terminal, doping when the water quantity of distillate in esterification reaches the 92% of theoretical value
Modified Sb2O3The additional amount of powder, titanium dioxide and trimethyl phosphate be respectively terephthalic acid (TPA) additional amount 0.014wt%,
0.22wt% and 0.01wt%；
(1.3) polycondensation reaction；
After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, the staged pressure is in 30min
The interior absolute pressure that is steadily evacuated to by normal pressure is 500Pa, and reaction temperature is 252 DEG C, reaction time 30min, then proceedes to take out true
Sky carries out the polycondensation reaction of high vacuum stage of Fig, and reaction pressure is made to be further reduced to absolute pressure 100Pa, reaction temperature 271
DEG C, polyester is made in reaction time 55min；
(1.4) solid phase polycondensation is carried out to polyester to viscosify to obtain the polyester fondant that inherent viscosity is 1.0dL/g；
(2) polyester fondant melted, measured, being squeezed out, being cooled down, being oiled, being combineeed, being stretched, being twisted, thermal finalization, relaxation
The polyester industrial yarn for heavy-duty hoisting band is made in heat treatment and winding；
The polyester tow that it is 4.2% by the over feed rate(OFR) of winding that heat treatment without tension, which refers to, is by a pair of arranged in parallel and non-co-planar
Temperature is the space between 207 DEG C of hot plate simultaneously, hot plate be located in FDY equipment last group of setting roller and take-up roll it
Between, along the traffic direction of polyester tow, the length of two hot plates is 3.2m, and the both ends of two hot plates flush, and polyester tow is from two hot plates
When centre passes through, the distance between two hot plates are 6mm, and the spacing between last group of setting roller and take-up roll is
311mm, the spacing between two hot plates and last group of setting roller are 220mm；
Spinning technology parameter is as follows:
It stretches, the technological parameter of thermal finalization are as follows:
The process flow of plying are as follows: creel → sensor → pressure tensioner → godet roller → guide rod or Network device → sensing
Device → linear speed inductor → pulley → traverse filar guide → winding paper tube, the technological parameter of plying are as follows: number of share of stock 20, speed 500m/
min。
The filament number of the final polyester industrial yarn obtained for heavy-duty hoisting band is 8.5dtex, and breaking strength is
8.4N, line density 3600dtex, line density deviation ratio be -1.0%, elongation at break 8.0%, 177 DEG C × 10min ×
Dry-hot shrinkage under the conditions of 0.05cN/dtex is 8.8%, and internet pricing is 7/m.
Embodiment 3
A kind of preparation method of the polyester industrial yarn for heavy-duty hoisting band, the specific steps are as follows:
(1) polyester is prepared；
(1.1) Sb of doping vario-property is prepared2O3；
Ba (the NO that concentration is 1.0mol% by (1.1.1)3)2The Sb that aqueous solution and concentration are 10mol%2O3Solution it is mixed
It closes uniformly, Sb2O3The solvent of solution be oxalic acid, Ba in mixed liquor2+With Sb3+Molar ratio be 3:100；
The pH value that ammonium hydroxide to mixed liquor that concentration is 2mol/L is added dropwise in (1.1.2) is 9.5 to obtain precipitated product, then to heavy
Shallow lake product is washed and is dried, and dry temperature is 105 DEG C, time 3h；
(1.1.3) keeps the temperature 3h after the product after drying is warming up to 400 DEG C first, keeps the temperature 2h after then heating to 900 DEG C,
It is crushed after finally cooling down in air and obtains the Sb for the doping vario-property that average grain diameter is 0.5 micron2O3Powder；
(1.2) esterification；
Terephthalic acid (TPA) and ethylene glycol that molar ratio is 1:1.8 are made into slurry, the Sb of doping vario-property is added2O3Powder, two
After mixing, pressurization carries out esterification in nitrogen atmosphere, and moulding pressure is normal pressure, ester for titanium oxide and Trimethyl phosphite
The temperature for changing reaction is 252 DEG C, is esterification terminal when the water quantity of distillate in esterification reaches the 90% of theoretical value, mixes
The Sb of miscellaneous modification2O3The additional amount of powder, titanium dioxide and Trimethyl phosphite is respectively terephthalic acid (TPA) additional amount
0.013wt%, 0.23wt% and 0.03wt%；
(1.3) polycondensation reaction；
After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, the staged pressure is in 35min
The interior absolute pressure that is steadily evacuated to by normal pressure is 450Pa, and reaction temperature is 253 DEG C, reaction time 35min, then proceedes to take out true
Sky carries out the polycondensation reaction of high vacuum stage of Fig, and reaction pressure is made to be further reduced to absolute pressure 90Pa, reaction temperature 274
DEG C, polyester is made in reaction time 60min；
(1.4) solid phase polycondensation is carried out to polyester to viscosify to obtain the polyester fondant that inherent viscosity is 1.1dL/g；
(2) polyester fondant melted, measured, being squeezed out, being cooled down, being oiled, being combineeed, being stretched, being twisted, thermal finalization, relaxation
The polyester industrial yarn for heavy-duty hoisting band is made in heat treatment and winding；
The polyester tow that it is 3% by the over feed rate(OFR) of winding that heat treatment without tension, which refers to, is by a pair of arranged in parallel and non-co-planar same
The space between hot plate that Shi Wendu is 215 DEG C, hot plate are located in FDY equipment between last group of setting roller and take-up roll,
Along the traffic direction of polyester tow, the length of two hot plates is 3.3m, and the both ends of two hot plates flush, and polyester tow is among two hot plates
Across when, the distance between two hot plates are 7mm, and spacing between last group of setting roller and take-up roll is 335mm, two
Spacing between hot plate and last group of setting roller is 235mm；
Spinning technology parameter is as follows:
It stretches, the technological parameter of thermal finalization are as follows:
The process flow of plying are as follows: creel → sensor → pressure tensioner → godet roller → guide rod or Network device → sensing
Device → linear speed inductor → pulley → traverse filar guide → winding paper tube, the technological parameter of plying are as follows: number of share of stock 15, speed 450m/
min。
The filament number of the final polyester industrial yarn obtained for heavy-duty hoisting band is 8.5dtex, and breaking strength is
8.6N, line density 3800dtex, line density deviation ratio be 0.7%, elongation at break 8.0%, 177 DEG C × 10min ×
Dry-hot shrinkage under the conditions of 0.05cN/dtex is 7.0%, and internet pricing is 6/m.
Embodiment 4
A kind of preparation method of the polyester industrial yarn for heavy-duty hoisting band, the specific steps are as follows:
(1) polyester is prepared；
(1.1) Sb of doping vario-property is prepared2O3；
Zn (the NO that concentration is 0.6mol% by (1.1.1)3)2The Sb that aqueous solution and concentration are 6mol%2O3Solution mixing
Uniformly, Sb2O3The solvent of solution be oxalic acid, Zn in mixed liquor2+With Sb3+Molar ratio be 1.2:100；
The pH value that ammonium hydroxide to mixed liquor that concentration is 2mol/L is added dropwise in (1.1.2) is 10 to obtain precipitated product, then to heavy
Shallow lake product is washed and is dried, and dry temperature is 110 DEG C, time 2.5h；
(1.1.3) keeps the temperature 2.5h after the product after drying is warming up to 400 DEG C first, keeps the temperature after then heating to 900 DEG C
1h is crushed after finally cooling down in air and is obtained the Sb for the doping vario-property that average grain diameter is 0.4 micron2O3Powder；
(1.2) esterification；
Terephthalic acid (TPA) and ethylene glycol that molar ratio is 1:1.9 are made into slurry, the Sb of doping vario-property is added2O3Powder, two
After mixing, pressurization carries out esterification, moulding pressure 0.3MPa, ester in nitrogen atmosphere for titanium oxide and triphenyl phosphate
The temperature for changing reaction is 254 DEG C, is esterification terminal when the water quantity of distillate in esterification reaches the 96% of theoretical value, mixes
The Sb of miscellaneous modification2O3The additional amount of powder, titanium dioxide and triphenyl phosphate is respectively terephthalic acid (TPA) additional amount
0.012wt%, 0.25wt% and 0.05wt%；
(1.3) polycondensation reaction；
After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, the staged pressure is in 40min
The interior absolute pressure that is steadily evacuated to by normal pressure is 410Pa, and reaction temperature is 255 DEG C, reaction time 32min, then proceedes to take out true
Sky carries out the polycondensation reaction of high vacuum stage of Fig, and reaction pressure is made to be further reduced to absolute pressure 95Pa, reaction temperature 275
DEG C, polyester is made in reaction time 70min；
(1.4) solid phase polycondensation is carried out to polyester to viscosify to obtain the polyester fondant that inherent viscosity is 1.2dL/g；
(2) polyester fondant melted, measured, being squeezed out, being cooled down, being oiled, being combineeed, being stretched, being twisted, thermal finalization, relaxation
The polyester industrial yarn for heavy-duty hoisting band is made in heat treatment and winding；
The polyester tow that it is 4.8% by the over feed rate(OFR) of winding that heat treatment without tension, which refers to, is by a pair of arranged in parallel and non-co-planar
Temperature is the space between 222 DEG C of hot plate simultaneously, hot plate be located in FDY equipment last group of setting roller and take-up roll it
Between, along the traffic direction of polyester tow, the length of two hot plates is 3.4m, and the both ends of two hot plates flush, and polyester tow is from two hot plates
When centre passes through, the distance between two hot plates are 8mm, and the spacing between last group of setting roller and take-up roll is
346mm, the spacing between two hot plates and last group of setting roller are 250mm；
Spinning technology parameter is as follows:
It stretches, the technological parameter of thermal finalization are as follows:
The process flow of plying are as follows: creel → sensor → pressure tensioner → godet roller → guide rod or Network device → sensing
Device → linear speed inductor → pulley → traverse filar guide → winding paper tube, the technological parameter of plying are as follows: number of share of stock 20, speed 400m/
min。
The filament number of the final polyester industrial yarn obtained for heavy-duty hoisting band is 8.2dtex, and breaking strength is
8.4N, line density 3500dtex, line density deviation ratio be -0.6%, elongation at break 7.2%, 177 DEG C × 10min ×
Dry-hot shrinkage under the conditions of 0.05cN/dtex is 9.0%, and internet pricing is 10/m.
Embodiment 5
A kind of preparation method of the polyester industrial yarn for heavy-duty hoisting band, the specific steps are as follows:
(1) polyester is prepared；
(1.1) Sb of doping vario-property is prepared2O3；
Mg (the NO that concentration is 0.7mol% by (1.1.1)3)2The Sb that aqueous solution and concentration are 8mol%2O3Solution mixing
Uniformly, Sb2O3The solvent of solution be oxalic acid, Mg in mixed liquor2+With Sb3+Molar ratio be 2:100；
The pH value that ammonium hydroxide to mixed liquor that concentration is 2mol/L is added dropwise in (1.1.2) is 10 to obtain precipitated product, then to heavy
Shallow lake product is washed and is dried, and dry temperature is 110 DEG C, time 2.5h；
(1.1.3) keeps the temperature 2.5h after the product after drying is warming up to 400 DEG C first, keeps the temperature after then heating to 900 DEG C
2h is crushed after finally cooling down in air and is obtained the Sb for the doping vario-property that average grain diameter is 0.5 micron2O3Powder；
(1.2) esterification；
Terephthalic acid (TPA) and ethylene glycol that molar ratio is 1:2.0 are made into slurry, the Sb of doping vario-property is added2O3Powder, two
Titanium oxide and Trimethyl phosphite after mixing, pressurize in nitrogen atmosphere and carry out esterification, moulding pressure 0.2MPa,
The temperature of esterification is 256 DEG C, is esterification terminal when the water quantity of distillate in esterification reaches the 99% of theoretical value,
The Sb of doping vario-property2O3The additional amount of powder, titanium dioxide and Trimethyl phosphite is respectively terephthalic acid (TPA) additional amount
0.012wt%, 0.20wt% and 0.04wt%；
(1.3) polycondensation reaction；
After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, the staged pressure is in 45min
The interior absolute pressure that is steadily evacuated to by normal pressure is 490Pa, and reaction temperature is 257 DEG C, reaction time 40min, then proceedes to take out true
Sky carries out the polycondensation reaction of high vacuum stage of Fig, and reaction pressure is made to be further reduced to absolute pressure 90Pa, reaction temperature 277
DEG C, polyester is made in reaction time 75min；
(1.4) solid phase polycondensation is carried out to polyester to viscosify to obtain the polyester fondant that inherent viscosity is 1.05dL/g；
(2) polyester fondant melted, measured, being squeezed out, being cooled down, being oiled, being combineeed, being stretched, being twisted, thermal finalization, relaxation
The polyester industrial yarn for heavy-duty hoisting band is made in heat treatment and winding；
The polyester tow that it is 4.0% by the over feed rate(OFR) of winding that heat treatment without tension, which refers to, is by a pair of arranged in parallel and non-co-planar
Temperature is the space between 232 DEG C of hot plate simultaneously, hot plate be located in FDY equipment last group of setting roller and take-up roll it
Between, along the traffic direction of polyester tow, the length of two hot plates is 3.6m, and the both ends of two hot plates flush, and polyester tow is from two hot plates
When centre passes through, the distance between two hot plates are 8.5mm, and the spacing between last group of setting roller and take-up roll is
368mm, the spacing between two hot plates and last group of setting roller are 260mm；
Spinning technology parameter is as follows:
It stretches, the technological parameter of thermal finalization are as follows:
The process flow of plying are as follows: creel → sensor → pressure tensioner → godet roller → guide rod or Network device → sensing
Device → linear speed inductor → pulley → traverse filar guide → winding paper tube, the technological parameter of plying are as follows: number of share of stock 12, speed 420m/
min。
The filament number of the final polyester industrial yarn obtained for heavy-duty hoisting band is 8.8dtex, and breaking strength is
8.5N, line density 4000dtex, line density deviation ratio be 2.0%, elongation at break 8.1%, 177 DEG C × 10min ×
Dry-hot shrinkage under the conditions of 0.05cN/dtex is 8.3%, and internet pricing is 10/m.
Embodiment 6
A kind of preparation method of the polyester industrial yarn for heavy-duty hoisting band, the specific steps are as follows:
(1) polyester is prepared；
(1.1) Sb of doping vario-property is prepared2O3；
Concentration is the Mg (NO of 0.8mol% by (1.1.1)3)2Aqueous solution and Ca (NO3)21:1 is mixed by volume for aqueous solution
Conjunction obtains metal ion Mx+Aqueous solution, metal ion Mx+Aqueous solution and concentration be 8mol% Sb2O3Solution it is mixed
It closes uniformly, Sb2O3The solvent of solution be oxalic acid, M in mixed liquorx+With Sb3+Molar ratio be 2.5:100；
The pH value that ammonium hydroxide to mixed liquor that concentration is 2mol/L is added dropwise in (1.1.2) is 10 to obtain precipitated product, then to heavy
Shallow lake product is washed and is dried, and dry temperature is 105 DEG C, time 3h；
(1.1.3) keeps the temperature 3h after the product after drying is warming up to 400 DEG C first, keeps the temperature after then heating to 900 DEG C
1.5h is crushed after finally cooling down in air and is obtained the Sb for the doping vario-property that average grain diameter is 0.4 micron2O3Powder；
(1.2) esterification；
Terephthalic acid (TPA) and ethylene glycol that molar ratio is 1:1.2 are made into slurry, the Sb of doping vario-property is added2O3Powder, two
After mixing, pressurization carries out esterification, moulding pressure 0.2MPa, ester in nitrogen atmosphere for titanium oxide and trimethyl phosphate
The temperature for changing reaction is 258 DEG C, is esterification terminal when the water quantity of distillate in esterification reaches the 95% of theoretical value, mixes
The Sb of miscellaneous modification2O3The additional amount of powder, titanium dioxide and trimethyl phosphate is respectively terephthalic acid (TPA) additional amount
0.0135wt%, 0.23wt% and 0.01wt%；
(1.3) polycondensation reaction；
After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, the staged pressure is in 35min
The interior absolute pressure that is steadily evacuated to by normal pressure is 430Pa, and reaction temperature is 258 DEG C, reaction time 40min, then proceedes to take out true
Sky carries out the polycondensation reaction of high vacuum stage of Fig, and reaction pressure is made to be further reduced to absolute pressure 94Pa, reaction temperature 280
DEG C, polyester is made in reaction time 80min；
(1.4) solid phase polycondensation is carried out to polyester to viscosify to obtain the polyester fondant that inherent viscosity is 1.1dL/g；
(2) polyester fondant melted, measured, being squeezed out, being cooled down, being oiled, being combineeed, being stretched, being twisted, thermal finalization, relaxation
The polyester industrial yarn for heavy-duty hoisting band is made in heat treatment and winding；
The polyester tow that it is 3.0% by the over feed rate(OFR) of winding that heat treatment without tension, which refers to, is by a pair of arranged in parallel and non-co-planar
Temperature is the space between 235 DEG C of hot plate simultaneously, hot plate be located in FDY equipment last group of setting roller and take-up roll it
Between, along the traffic direction of polyester tow, the length of two hot plates is 3.8m, and the both ends of two hot plates flush, and polyester tow is from two hot plates
When centre passes through, the distance between two hot plates are 9mm, and the spacing between last group of setting roller and take-up roll is
384mm, the spacing between two hot plates and last group of setting roller are 280mm；
Spinning technology parameter is as follows:
It stretches, the technological parameter of thermal finalization are as follows:
The process flow of plying are as follows: creel → sensor → pressure tensioner → godet roller → guide rod or Network device → sensing
Device → linear speed inductor → pulley → traverse filar guide → winding paper tube, the technological parameter of plying are as follows: number of share of stock 18, speed 480m/
min。
The filament number of the final polyester industrial yarn obtained for heavy-duty hoisting band is 8.0dtex, and breaking strength is
8.2N, line density 3300dtex, line density deviation ratio be 1.2%, elongation at break 9.5%, 177 DEG C × 10min ×
Dry-hot shrinkage under the conditions of 0.05cN/dtex is 7.0%, and internet pricing is 6/m.
Embodiment 7
A kind of preparation method of the polyester industrial yarn for heavy-duty hoisting band, the specific steps are as follows:
(1) polyester is prepared；
(1.1) Sb of doping vario-property is prepared2O3；
Concentration is the Mg (NO of 0.5mol% by (1.1.1)3)2Aqueous solution, Ba (NO3)2Aqueous solution and Ca (NO3)2It is water-soluble
1:1:1 is mixed to get metal ion M to liquid by volumex+Aqueous solution, metal ion Mx+Aqueous solution be with concentration
The Sb of 10mol%2O3Solution be uniformly mixed, Sb2O3The solvent of solution be oxalic acid, metal ions M in mixed liquorx+With Sb3+'s
Molar ratio is 2:100；
The pH value that ammonium hydroxide to mixed liquor that concentration is 2mol/L is added dropwise in (1.1.2) is 9 to obtain precipitated product, then to precipitating
Product is washed and is dried, and dry temperature is 108 DEG C, time 2.5h；
(1.1.3) keeps the temperature 2.5h after the product after drying is warming up to 400 DEG C first, keeps the temperature after then heating to 900 DEG C
2h is crushed after finally cooling down in air and is obtained the Sb for the doping vario-property that average grain diameter is 0.4 micron2O3Powder；
(1.2) esterification；
Terephthalic acid (TPA) and ethylene glycol that molar ratio is 1:2.0 are made into slurry, the Sb of doping vario-property is added2O3Powder, two
After mixing, pressurization carries out esterification, moulding pressure 0.3MPa, ester in nitrogen atmosphere for titanium oxide and triphenyl phosphate
The temperature for changing reaction is 260 DEG C, is esterification terminal when the water quantity of distillate in esterification reaches the 91% of theoretical value, mixes
The Sb of miscellaneous modification2O3The additional amount of powder, titanium dioxide and triphenyl phosphate is respectively terephthalic acid (TPA) additional amount
0.015wt%, 0.25wt% and 0.05wt%；
(1.3) polycondensation reaction；
After esterification, start the polycondensation reaction of low vacuum stage under condition of negative pressure, the staged pressure is in 50min
The interior absolute pressure that is steadily evacuated to by normal pressure is 400Pa, and reaction temperature is 260 DEG C, reaction time 50min, then proceedes to take out true
Sky carries out the polycondensation reaction of high vacuum stage of Fig, and reaction pressure is made to be further reduced to absolute pressure 88Pa, reaction temperature 282
DEG C, polyester is made in reaction time 90min；
(1.4) solid phase polycondensation is carried out to polyester to viscosify to obtain the polyester fondant that inherent viscosity is 1.15dL/g；
(2) polyester fondant melted, measured, being squeezed out, being cooled down, being oiled, being combineeed, being stretched, being twisted, thermal finalization, relaxation
The polyester industrial yarn for heavy-duty hoisting band is made in heat treatment and winding；
The polyester tow that it is 5.0% by the over feed rate(OFR) of winding that heat treatment without tension, which refers to, is by a pair of arranged in parallel and non-co-planar
Temperature is the space between 240 DEG C of hot plate simultaneously, hot plate be located in FDY equipment last group of setting roller and take-up roll it
Between, along the traffic direction of polyester tow, the length of two hot plates is 4.0m, and the both ends of two hot plates flush, and polyester tow is from two hot plates
When centre passes through, the distance between two hot plates are 10mm, and the spacing between last group of setting roller and take-up roll is
400mm, the spacing between two hot plates and last group of setting roller are 300mm；
Spinning technology parameter is as follows:
It stretches, the technological parameter of thermal finalization are as follows:
The process flow of plying are as follows: creel → sensor → pressure tensioner → godet roller → guide rod or Network device → sensing
Device → linear speed inductor → pulley → traverse filar guide → winding paper tube, the technological parameter of plying are as follows: number of share of stock 16, speed 420m/
min。
The filament number of the final polyester industrial yarn obtained for heavy-duty hoisting band is 8.4dtex, and breaking strength is
8.6N, line density 4000dtex, line density deviation ratio be -2.0%, elongation at break 6.9%, 177 DEG C × 10min ×
Dry-hot shrinkage under the conditions of 0.05cN/dtex is 10.0%, and internet pricing is 8/m.
Claims (10)
1. the preparation method of the polyester industrial yarn for heavy-duty hoisting band, it is characterized in that: polyester fondant is carried out solid phase polycondensation increasing
It glues, melts, measure, squeeze out, cool down, oil, combining, stretching, twisting, thermal finalization, heat treatment without tension and winding are made for weight
The polyester industrial yarn of type hanging belt；
Polyester the preparation method comprises the following steps: by the Sb of terephthalic acid (TPA), ethylene glycol and doping vario-property before the solid phase polycondensation viscosifies2O3Powder
Body successively carries out esterification and polycondensation reaction after mixing；
Sb2O3The process of doping vario-property are as follows: first by metal ion Mx+Solution with contain Sb3+Solution be uniformly mixed, then
The pH value that precipitating reagent is added dropwise to mixed liquor is 9~10, finally calcines precipitated product and crushes；Metal ions Mx+For Mg2+、Ca2+、
Ba2+And Zn2+One or more of；
The heat treatment without tension refers to the space by polyester tow in relaxed state appropriate Jing Guo certain temperature；
The relaxed state appropriate refers to that the over feed rate(OFR) of winding is 3.0~5.0%；
The certain temperature refers to 200~240 DEG C.
2. the preparation method of the polyester industrial yarn according to claim 1 for heavy-duty hoisting band, which is characterized in that be used for
The filament number of the polyester industrial yarn of heavy-duty hoisting band be 8.0~9.0dtex, breaking strength >=8.2N, line density be 3300~
4400dtex, line density deviation ratio are ± 2.0%, and elongation at break is 6.5~9.5%, in 177 DEG C × 10min × 0.05cN/
Dry-hot shrinkage under the conditions of dtex is 7.0~10.0%, and internet pricing is 6~14/m.
3. the preparation method of the polyester industrial yarn according to claim 1 for heavy-duty hoisting band, which is characterized in that described
Metal ion Mx+Solution concentration be 0.5~1.0mol%, solvent is water, the anion in solution be NO3 -；It is described to contain
Sb3+Solution be 5~10mol% of concentration Sb2O3Solution, solvent is oxalic acid；The precipitating reagent is the ammonia of concentration 2mol/L
Water；When precipitating starts, metal ions M in mixed solutionx+With Sb3+Molar ratio be 1~3:100；
Precipitated product is washed and dried before the calcining, dry temperature is 105~110 DEG C, and the time is 2~3h；Institute
State the process of calcining are as follows: keep the temperature 2~3h after being warming up to 400 DEG C first, 1~2h is kept the temperature after then heating to 900 DEG C, finally in sky
It is cooling in gas；
Sb2O3It is crushed to obtain powder of the average grain diameter less than 0.5 micron after doping vario-property.
4. the preparation method of the polyester industrial yarn according to claim 3 for heavy-duty hoisting band, which is characterized in that described
The preparation step of polyester is as follows before solid phase polycondensation viscosifies:
(1) esterification；
Terephthalic acid (TPA) and ethylene glycol are made into slurry, the Sb of doping vario-property is added2O3Powder, delustering agent and stabilizer mixing are equal
After even, pressurization carries out esterification in nitrogen atmosphere, and 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 90% or more of theoretical value；
(2) polycondensation reaction；
After esterification, start the polycondensation reaction of 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 250~260 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, so that reaction pressure is further reduced to absolute pressure 100Pa hereinafter,
Reaction temperature is 270~282 DEG C, and the reaction time is 50~90min.
5. the preparation method of the polyester industrial yarn according to claim 4 for heavy-duty hoisting band, which is characterized in that described
The molar ratio of terephthalic acid (TPA) and ethylene glycol is 1:1.2~2.0, the Sb of the doping vario-property2O3Powder, delustering agent and stabilizer
Additional amount be respectively terephthalic acid (TPA) additional amount 0.012~0.015wt%, 0.20~0.25wt% and 0.01~
0.05wt%.
6. the preparation method of the polyester industrial yarn according to claim 5 for heavy-duty hoisting band, which is characterized in that described
Delustering agent is titanium dioxide, and the stabilizer is triphenyl phosphate, trimethyl phosphate or Trimethyl phosphite.
7. the preparation method of the polyester industrial yarn according to claim 6 for heavy-duty hoisting band, which is characterized in that described
The inherent viscosity of polyester is 1.0~1.2dL/g after solid phase polycondensation thickening.
8. the preparation method of the polyester industrial yarn according to claim 1 for heavy-duty hoisting band, which is characterized in that described
The space of certain temperature refers to the space between a pair of arranged in parallel and non-coplanar hot plate, and hot plate is located in FDY equipment finally
One group between setting roller and take-up roll；Along the traffic direction of polyester tow, the length of two hot plates is 3.0~4.0m, two hot plates
Both ends flush；When polyester tow passes through among two hot plates, the distance between two hot plates are 5~10mm.
9. the preparation method of the polyester industrial yarn according to claim 8 for heavy-duty hoisting band, which is characterized in that last
One group of spacing between setting roller and take-up roll is 300~400mm；Spacing between two hot plates and last group of setting roller
For 200~300mm.
10. the preparation method of the polyester industrial yarn according to claim 1 for heavy-duty hoisting band, which is characterized in that institute
It states as follows for the spinning technology parameter of the polyester industrial yarn of heavy-duty hoisting band:
It stretches, the technological parameter of thermal finalization are as follows:
The process flow of the plying are as follows: creel → sensor → pressure tensioner → godet roller → guide rod or Network device → sensing
Device → linear speed inductor → pulley → traverse filar guide → winding paper tube；
The technological parameter of the plying are as follows: number of share of stock 10~20,400~500m/min of speed.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811614105.0A CN109735936B (en) | 2018-12-27 | 2018-12-27 | Preparation method of polyester industrial yarn for heavy-duty hoisting belt |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811614105.0A CN109735936B (en) | 2018-12-27 | 2018-12-27 | Preparation method of polyester industrial yarn for heavy-duty hoisting belt |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109735936A true CN109735936A (en) | 2019-05-10 |
| CN109735936B CN109735936B (en) | 2020-07-07 |
Family
ID=66360245
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811614105.0A Active CN109735936B (en) | 2018-12-27 | 2018-12-27 | Preparation method of polyester industrial yarn for heavy-duty hoisting belt |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109735936B (en) |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1119836A (en) * | 1993-12-22 | 1996-04-03 | 花王株式会社 | Alkoxylation catalyst, process for the preparation of the catalyst and process for preparing alkoxylate with the use of the catalyst |
| CN105504244A (en) * | 2015-12-29 | 2016-04-20 | 江苏恒力化纤股份有限公司 | Ultrahigh-strength polyester industrial yarn and preparation method thereof |
| CN108035156A (en) * | 2017-12-14 | 2018-05-15 | 江苏恒力化纤股份有限公司 | Terylene heavy caliber conveyer belt and preparation method thereof |
| CN108071009A (en) * | 2017-12-14 | 2018-05-25 | 江苏恒力化纤股份有限公司 | A kind of method for reducing spun polyester thread filoplume |
| CN108130624A (en) * | 2017-12-14 | 2018-06-08 | 江苏恒力化纤股份有限公司 | A kind of polyester imitates linen look abnormal contraction composite filament and preparation method thereof |
| CN108385186A (en) * | 2017-12-14 | 2018-08-10 | 江苏恒力化纤股份有限公司 | A kind of polyester POY fibers and preparation method thereof |
-
2018
- 2018-12-27 CN CN201811614105.0A patent/CN109735936B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1119836A (en) * | 1993-12-22 | 1996-04-03 | 花王株式会社 | Alkoxylation catalyst, process for the preparation of the catalyst and process for preparing alkoxylate with the use of the catalyst |
| CN105504244A (en) * | 2015-12-29 | 2016-04-20 | 江苏恒力化纤股份有限公司 | Ultrahigh-strength polyester industrial yarn and preparation method thereof |
| CN108035156A (en) * | 2017-12-14 | 2018-05-15 | 江苏恒力化纤股份有限公司 | Terylene heavy caliber conveyer belt and preparation method thereof |
| CN108071009A (en) * | 2017-12-14 | 2018-05-25 | 江苏恒力化纤股份有限公司 | A kind of method for reducing spun polyester thread filoplume |
| CN108130624A (en) * | 2017-12-14 | 2018-06-08 | 江苏恒力化纤股份有限公司 | A kind of polyester imitates linen look abnormal contraction composite filament and preparation method thereof |
| CN108385186A (en) * | 2017-12-14 | 2018-08-10 | 江苏恒力化纤股份有限公司 | A kind of polyester POY fibers and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109735936B (en) | 2020-07-07 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105908282B (en) | A kind of preparation method of the Manufacturing Pet Fine Filaments of 33dtex/144f | |
| KR101537131B1 (en) | Polyethylene naphthalate fiber and process for producing the polyethylene naphthalate fiber | |
| CN105862152A (en) | Production method for high-speed spinning low-stretching high-modulus low-shrinkage polyester industrial filaments | |
| TWI453311B (en) | Polyethylene naphthalate fiber and its manufacturing method | |
| CN102560717A (en) | High-strength low-contract polyphenylene sulfide filament and preparation method thereof | |
| CN109735926B (en) | Easily-dyed porous modified polyester fiber and preparation method thereof | |
| CN109706542B (en) | Flame-retardant polyester fiber and preparation method thereof | |
| KR20230104667A (en) | High-strength low-elongation polyester fiber industrial yarn and manufacturing method thereof | |
| KR100499220B1 (en) | High tenacity polyethylene-2,6-naphthalate fibers having excellent processability, and process for preparing the same | |
| CN108193303B (en) | Hydrophilic polyester fiber and preparation method thereof | |
| CN109735936A (en) | The preparation method of polyester industrial yarn for heavy-duty hoisting band | |
| CN109735928A (en) | Textilene cloth and preparation method thereof | |
| CN109763194A (en) | The preparation method of polyester industrial yarn for tire cord | |
| CN109722729B (en) | Hexanediol modified polyester fiber with tert-butyl side group and preparation method thereof | |
| CN109735919B (en) | Heptanediol modified polyester fiber with tertiary butyl side group and preparation method thereof | |
| CN109735947B (en) | Water-repellent canvas and preparation method thereof | |
| JP5431843B2 (en) | Belt-reinforcing fiber material and belt using the same | |
| CN112921439A (en) | Melt spinning method of low-melting-point polyester FDY filament | |
| KR20170091968A (en) | Manufacturing method of polyethylene terephthalate cord having excellent fatigue resistance | |
| JPH0450407B2 (en) | ||
| KR101746029B1 (en) | Process for preparing polyethylene terephthalate filament having excellent high strength and dimensional stability | |
| KR100630264B1 (en) | Hybrid dip cord | |
| CN109930231B (en) | Preparation method of polyester sun-shading cloth | |
| JPH0144810B2 (en) | ||
| CN109750363A (en) | The preparation method of ultralow shrinkage type polyester industrial fiber |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |