CN110358061A - For producing the polyester slice and preparation method thereof of low melting point core-sheath silk - Google Patents
For producing the polyester slice and preparation method thereof of low melting point core-sheath silk Download PDFInfo
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- CN110358061A CN110358061A CN201910778470.3A CN201910778470A CN110358061A CN 110358061 A CN110358061 A CN 110358061A CN 201910778470 A CN201910778470 A CN 201910778470A CN 110358061 A CN110358061 A CN 110358061A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/02—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds
- C08G63/12—Polyesters derived from hydroxycarboxylic acids or from polycarboxylic acids and polyhydroxy compounds derived from polycarboxylic acids and polyhydroxy compounds
- C08G63/16—Dicarboxylic acids and dihydroxy compounds
- C08G63/18—Dicarboxylic acids and dihydroxy compounds the acids or hydroxy compounds containing carbocyclic rings
- C08G63/181—Acids containing aromatic rings
- C08G63/183—Terephthalic acids
-
- 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
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
- C08G63/88—Post-polymerisation treatment
- C08G63/90—Purification; Drying
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/28—Formation of filaments, threads, or the like while mixing different spinning solutions or melts during the spinning operation; Spinnerette packs therefor
- D01D5/30—Conjugate filaments; Spinnerette packs therefor
- D01D5/34—Core-skin structure; Spinnerette packs therefor
-
- 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
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/14—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one polyester as constituent
Abstract
The invention discloses a kind of for producing the polyester slice and preparation method thereof of low melting point core-sheath silk, synthesis meets the polyester slice that technique requires first: utilizing semi-continuous polymerization reaction unit, the fusing point of product is reduced by introducing isomers in an esterification, it polymerize means again by the way that congruent melting and alcoholysis is blended in class reaction, realizes that target polyesters slice possesses excellent crystal property；Finally by catalyst compounded, control reaction temperature and vacuum degree, the target polyesters that final composite character viscosity is 0.750-0.770dl/g are sliced bottom material；By the product of synthesis by solid phase drum device boiling crystallization processes, the pre-crystallized of polyester slice is completed；By the processing technology of temperature control continuous negative pressure, the drying of polyester slice is completed, polyester slice water content is not higher than 0.05% after the completion of drying, and inherent viscosity is not less than 0.725dl/g.It can be prepared by meeting by three above step industrial for producing the polyester slice of low melting point core-sheath silk.
Description
Technical field
The present invention relates to polyester slices and preparation method thereof, are a kind of for producing low melting point core-sheath silk specifically
Polyester slice and preparation method thereof.
Background technique
Terylene core-skin low melting point composite filament is chiefly used in the production of no glue compound nonwoven cloth, since it does not use adhesive, symbol
Requirement of the market to low-carbon environment-friendly is closed, application range and usage amount expand year by year, also increasingly recognized by domestic market
It can.Although this kind of cloth rises in foreign countries for a long time, because the process is more complicated, production cost is higher for Material synthesis early period, in original
The material aspect country rarely has people to set foot in, and especially complicated modified low-melting fiber polyester slice, domestic there are few producers to give birth to
It produces, leads to the non-woven fabrics supply wretched insufficiency using the raw material, high-end cloth is still based on import.
Currently, domestic existing producer of the production without glue bicomponent filament yarn, the general fusing point of the raw material used concentrate on 200 DEG C
Under, but the problems such as composite filament bonding force is insufficient, and drying is difficult, and weatherability is poor is generally faced, particular problem is described as follows:
1, common low melting point Modified polyester chips, amorphous domain is wider, is unfavorable for subsequent drying crystalline processing；
2, general low melting point Modified polyester chips, strong degree is not high when progress binder-treatment after completion spinning, and finished product is durable
Property is poor；
3, general boiling crystallization, technology controlling and process is unstable, and crystallinity cannot ensure, and inherent viscosity fluctuation is larger, after
Continuous practicability is poor；
4, low melting point polyester chip is dry difficult, agglomeration easy to reunite, inherent viscosity susceptible, traditional low-temperature air-drying
Method, cannot sufficiently dry low melting point polyester chip, will cause extrusion pressure shakiness, the silk that floats, fracture of wire etc. during the spinning process in this way,
It is unfavorable for consecutive production.
Summary of the invention
The technical problem to be solved by the invention is to provide a kind of for producing the polyester slice of low melting point core-sheath silk
And preparation method thereof, the core-sheath long filament produced and processed using polyester slice of the invention, bonding demand temperature is low, bonding jail
It is high by degree, it is not easy the tomography that comes unglued, durability is splendid.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is that: one kind is multiple for producing low melting point core-skin
The polyester slice preparation method of plying, comprising the following steps:
(1) synthesis of polyester slice bottom material
1. M-phthalic acid and terephthaldehyde's acid blend are put into ethylene glycol solution, wherein M-phthalic acid Zhan is total
Acid amount molar fraction is 13%-28%, and total ethylene glycol molal quantity and total acid molal quantity ratio are 1.15-1.35, by what is mixed
Slurry is uniformly pumped into a reaction kettle of the esterification, and the uniform slurries of BHET and its derivatives intermediates are made；
2. adding PBT and auxiliary material in class reaction kettle, PBT mass accounts for the 14%- for participating in reaction solid gross mass
29%, it feeds intake and finishes, ethylene glycol and 1,4-butanediol is added and carries out alcoholysis, the molal quantity ratio of ethylene glycol and butanediol is 1.1-
1.7, obtain uniform melting slurries；
3. the slurries for 1. obtaining step are pressed into class kettle when 2. middle slurry temperature is stabilized to 235-245 DEG C to step,
Wherein the mass fraction of the class total slurries of slurries Zhan is 14%-29%, and it is mixed to carry out 1.5-2.0h high-speed stirred under nitrogen atmosphere
It closes, after mixeding liquid temperature is risen to 245-255 DEG C, is pressed into batch condensation polymerization reactor through 15-25 μm of stainless steel filter by class kettle；
4. after mixed serum enters polycondensation vessel, controlling 230-280 DEG C of reaction temperature, negative pressure polymerization reaction is carried out, it is desirable that true
Reciprocal of duty cycle≤30Pa under 250-280 DEG C of final temperature, controls stirring polycondensation electric current and power by equipment, synthesizes inherent viscosity and exist
The high viscosity polyester of 0.750-0.770dl/g is sliced melt, then through end of extruded band, underwater pelletizer and drying machine, vibrating screen, finally
Obtain the polyester slice for producing low melting point core-sheath silk；
(2) for producing the pre-crystallized processing of polyester slice of low melting point core-sheath silk: step (1) is obtained for giving birth to
The polyester slice of low melting point core-sheath silk is produced, is put into solid phase rotary drum crystallization apparatus, is added water not have polyester slice, will consolidate later
The sealing of phase rotary drum crystallization apparatus, opening conduits drain starts rotary drum motor, and opens heating, by rotary drum temperature from 35-45 DEG C
It is ramped up 70-100 DEG C through 10-16h, starts constant temperature 3-5h later, until polyester slice is fully crystallized, is then discharged water simultaneously
Surface moisture is blown away through air-heater vibrating screen；
(3) it is dried for producing the polyester slice of low melting point core-sheath silk: the pre- knot that will be handled well in step (2)
In crystalline substance slice investment dryer drums, rotary drum is sealed, and close drain, connect multistage water ring pump vacuum pipe, start negative
It heats up under pressure condition, it is desirable that vacuum degree≤600Pa, temperature are ramped up 90-110 DEG C through 8-16h by 30-50 DEG C of room temperature, enter
Continue to keep negative pressure 4-6h, sampling and testing moisture content and inherent viscosity after constant temperature, reaches and start to drop to rotary drum after technique requires
Temperature simultaneously discharges, and completes the drying process for producing the polyester slice of low melting point core-sheath silk.
Auxiliary material added by class reaction kettle includes catalyst compounded, antioxidant and toner, and wherein catalyst is
Antimony system and titanium system compounding are aided with a small amount of germanium series catalysts, and antioxidant is antioxidant 1010, and toner is red blue dyestuff.
It is described it is catalyst compounded add four butyl ester of phthalandione for antimony oxide, wherein antimony oxide accounts for the 20%- of gross mass
50%, butyl titanate accounts for 50-80%, and germanium series catalysts account for 0.1%-5%.
It is in 235-275 DEG C by control polycondensation reaction temperature, in conjunction with stirring frequency conversion adjustment, realizes polycondensation reaction in 5-8h
Inside reach inherent viscosity 0.750dl/g or more, meets inherent viscosity requirement in crystallization treatment and drying process process.
Above-mentioned preparation method is obtained for producing the polyester slice of low melting point core-sheath silk.
The beneficial effects of the present invention are:
1, by introducing M-phthalic acid in a lactate synthesis, finished product may be implemented and be sliced stable low melting point section,
To lay a good foundation for the production of Low Temperature Thermal fuse；Meanwhile the modification carried out using the product, it is on bonding effect after spinning
3-5 times of conventional polyester slice, firmness is higher；
2, by introducing PBT polyester slice and auxiliary material in class reaction, it can be good at solution low-melting point polyester and cut
The persistent ailment of piece later crystallization difficulty has eradicated the not high problem of low melting point polyester chip crystallinity, experimental result, knot from structure
Brilliant degree is not less than 90%, creates highly beneficial condition for subsequent spinning drying；
3, by boiling crystallization processes, the high characteristic of water specific heat capacity is utilized, it can be ensured that the stabilization of temperature in crystallization process,
The phenomenon that inherent viscosity caused by reducing to the greatest extent because of crystallization reduces and agglomeration is reunited, passes through the control hand in scheme
Section, it can be ensured that crystallization process medium viscosity, which reduces, is not more than 0.020dl/g, and crystallization whole process is without caking phenomenon；
4, by simulation vacuum drying, slice water content can be controlled to greatest extent, while in the feelings for guaranteeing vacuum degree
Under condition, drying process medium viscosity hardly has significant change, and experimental data shows that viscosity reduction amplitude is no more than 0.003dl/g, together
When moisture content be generally not higher than 0.05%, fully meet the requirement of composite filament silk.
Specific embodiment
Invention is further described in detail With reference to embodiment:
The polyester slice preparation method for being used to produce low melting point core-sheath silk of the invention, comprising the following steps:
(1) synthesis of polyester slice bottom material
1. M-phthalic acid and terephthaldehyde's acid blend are put into ethylene glycol solution, wherein M-phthalic acid Zhan is total
Acid amount molar fraction is 13%-28%, and total ethylene glycol molal quantity and total acid molal quantity ratio are 1.15-1.35, by what is mixed
Slurry is uniformly pumped into a reaction kettle of the esterification, and the uniform slurries of BHET and its derivatives intermediates are made；
2. adding PBT and auxiliary material in class reaction kettle, PBT mass accounts for the 14%- for participating in reaction solid gross mass
29%, it feeds intake and finishes, ethylene glycol and 1,4-butanediol is added and carries out alcoholysis, the molal quantity ratio of ethylene glycol and butanediol is 1.1-
1.7, obtain uniform melting slurries；
3. the slurries for 1. obtaining step are pressed into class kettle when 2. middle slurry temperature is stabilized to 235-245 DEG C to step,
Wherein the mass fraction of the class total slurries of slurries Zhan is 14%-29%, and it is mixed to carry out 1.5-2.0h high-speed stirred under nitrogen atmosphere
It closes, after mixeding liquid temperature is risen to 245-255 DEG C, is pressed into batch condensation polymerization reactor through 15-25 μm of stainless steel filter by class kettle；
4. after mixed serum enters polycondensation vessel, controlling 230-280 DEG C of reaction temperature, negative pressure polymerization reaction is carried out, it is desirable that true
Reciprocal of duty cycle≤30Pa under 250-280 DEG C of final temperature, controls stirring polycondensation electric current and power by equipment, synthesizes inherent viscosity and exist
The high viscosity polyester of 0.750-0.770dl/g is sliced melt, then through end of extruded band, underwater pelletizer and drying machine, vibrating screen, finally
Obtain the polyester slice for producing low melting point core-sheath silk；
(2) for producing the pre-crystallized processing of polyester slice of low melting point core-sheath silk: step (1) is obtained for giving birth to
The polyester slice of low melting point core-sheath silk is produced, is put into solid phase rotary drum crystallization apparatus, is added water not have polyester slice, will consolidate later
The sealing of phase rotary drum crystallization apparatus, opening conduits drain starts rotary drum motor, and opens heating, by rotary drum temperature from 35-45 DEG C
It is ramped up 70-100 DEG C through 10-16h, starts constant temperature 3-5h later, until polyester slice is fully crystallized, is then discharged water simultaneously
Surface moisture is blown away through air-heater vibrating screen；
(3) it is dried for producing the polyester slice of low melting point core-sheath silk: the pre- knot that will be handled well in step (2)
In crystalline substance slice investment dryer drums, rotary drum is sealed, and close drain, connect multistage water ring pump vacuum pipe, start negative
It heats up under pressure condition, it is desirable that vacuum degree≤600Pa, temperature are ramped up 90-110 DEG C through 8-16h by 30-50 DEG C of room temperature, enter
Continue to keep negative pressure 4-6h, sampling and testing moisture content and inherent viscosity after constant temperature, reaches and start to drop to rotary drum after technique requires
Temperature simultaneously discharges, and completes the drying process for producing the polyester slice of low melting point core-sheath silk.
Auxiliary material added by class reaction kettle includes catalyst compounded, antioxidant and toner, and wherein catalyst is
Antimony system and titanium system compounding are aided with a small amount of germanium series catalysts, and antioxidant is antioxidant 1010, and toner is red blue dyestuff.
It is described it is catalyst compounded add four butyl ester of phthalandione for antimony oxide, wherein antimony oxide accounts for the 20%- of gross mass
50%, butyl titanate accounts for 50-80%, and germanium series catalysts account for 0.1%-5%.
It is in 235-275 DEG C by control polycondensation reaction temperature, in conjunction with stirring frequency conversion adjustment, realizes polycondensation reaction in 5-8h
Inside reach inherent viscosity 0.750dl/g or more, meets inherent viscosity requirement in crystallization treatment and drying process process.
Above-mentioned preparation method is obtained for producing the polyester slice of low melting point core-sheath silk.
Polyester slice prepared by the present invention solves the silk that floats, fracture of wire, bonding in general low melting point polyester chip spinning process
Bad problem, while improving the performance of product composite filament, it is ensured that the technical problems such as the good toughness of bicomponent filament yarn and weatherability,
The present invention synthesizes polyester slice, polyester slice is pre-crystallized and the dry substep of polyester slice carries out, synchronously control:
1, technical solution is realized in fusing point control:
In fusing point control, market has more mature technical solution at present, and difference is additive amount and addition type
It will be different, the present invention accounts for the isophthalic acid moiety substitution terephthalic acid (TPA) of total acid molal quantity 13%-28% by introducing,
Come realize 170-200 DEG C of polyester slice melting range control, meet the requirement of low melting point Modified polyester chips.One esterification reaction temperature
230-270 DEG C of control, reaction process normal pressure.
2, technical solution is realized in crystal property control:
After realizing that low melting point polyester chip is successive modified, there is excellent crystal property, the present invention passes through sufficiently benefit
With the advantage of semi-continuous polymerization technique, the PBT modified additive for accounting for polyester slice total amount 14%-29% is added in class reaction kettle
With a small amount of auxiliary material, quantitative ethylene glycol is added and carries out alcoholysis reaction processing, is configured to target modified solution, then with an esterification
The mixing that product carries out forms prepolymerization reaction slurries by 30-50 minutes high-speed stirreds；Class reaction temperature control
235-245 DEG C, reactiveness normal pressure.
3, inherent viscosity control technology scheme:
To ensure that products application behind downstream, has good caking property and weatherability, it is desirable that complete crystallizing and drying processing
The inherent viscosity of Modified polyester chips later is not less than 0.730dl/g, so the Modified polyester chips before crystallization treatment are necessary
(inherent viscosity when general low melting point polyester chip polymerize is not higher than 0.680dl/g, at crystallization for inherent viscosity with higher
After reason generally above or below 0.660dl/g), to meet this requirement, must just adjust the technology controlling and process of polymerization, it is otherwise, special
Property viscosity will be unable to by polymerization realize.Target product of the present invention, it is desirable that polymerization temperature is at 230-280 DEG C, vacuum degree≤30Pa,
Done using antimony system, titanium system etc. catalyst compounded, while temperature-rise period will continue and steady, be not allow for rising and fall sharply and quickly, fluctuate width
Spend it is larger, will directly affect reaction be it is positive carry out or it is reverse carry out, moreover, low temperature and overtemperature are unfavorable for the present invention
Product characteristic viscosity build.
4, crystallization treatment technical solution:
For PET polyester slice, the PET polyester slice of normal melting point can realize crystallization treatment with fluidized bed or drier,
But it for low melting point Modified polyester chips and is not suitable for.Most of low melting point product is existed with amorphous state, general fusing point
Lower, crystallization difficulty is bigger, heated easily to stick together and agglomerate.The crystallization treatment for realizing product of the present invention needs to change
Previous crystallization treatment thinking.This product crystallization treatment adds the scheme of boiling using drum device, and the benefit of this programme is crystallization
It is not easy adhesion agglomeration, drawback is that the technology controlling and process of crystallization process will affect the inherent viscosity of Modified polyester chips, such as technology controlling and process
Improper, inherent viscosity decline is serious, it is desirable that heating process must be strictly controlled, it is ensured that viscosity reduction influences within controlled range.This
Invention temperature control is the core of crystallization, it is desirable that in room temperature to 100 DEG C of linear increases, crystallization time is strict controlled in for 24 hours crystallization temperature
Within.
The crystallization treatment stage will control the steady rising of heating, control heating-up time 10-16h, constant temperature time 3-5h is avoided
Heating big rise and big fall, cause crystallization to be not thorough or balling.
5, Drying Treatment Technology scheme:
Traditional low-temperature air-drying method can only take away the portion of water of slice surface, and it is multiple to be unable to satisfy low melting point core-skin
The aqueous requirement of plying special polyester chip spinning 0.05%, for this requirement, the present invention adds the technique control of heating using vacuum
System is to realize.The Modified polyester chips crystallized are squeezed into vacuum desiccator, are persistently vacuumized by vacuum pump, vacuum degree≤
600Pa and the control of 70-100 DEG C of temperature, it can be ensured that product moisture content is not higher than 0.05%, and inherent viscosity is almost without drop
It is low.
Embodiment 1
1. an esterification stage: adding 13% M-phthalic acid and 87% terephthalic acid (TPA) into slurry mixing kettle
(percentage is molar fraction, similarly hereinafter) amounts to 2 tons, then adds ethylene glycol according to acid alcohol molar ratio 1:1.20, be uniformly mixed
Afterwards, it is at the uniform velocity pumped into a reaction kettle of the esterification by pipeline pump, in 255 DEG C of progress esterifications, obtains the equal of BHET and its derivative
With mixed serum.
2. putting into the metatitanic acid fourth of the PBT polyester slice and 490g antimony oxide, 500g of 400Kg in class reaction kettle
The germanium oxide of ester, 1g, 800g antioxidant, 2.4g dyestuff, the 1,4-butanediol that 120Kg ethylene glycol and 100Kg is added carry out alcoholysis
Reaction, diester alcoholysis finish, and are mixed with an esterification slurries, form uniform mixed serum, diester reaction by high-speed stirred
Temperature controls 245 DEG C.
3. 2. mixed serum that step is obtained using nitrogen by 25 μm of stainless steel filters be pressed into batch condensation polymerization reactors into
Row polymerization reaction controls interior 260 DEG C warm, vacuum degree≤30pa, discharges after reaching inherent viscosity after reaction 6.0h.
4. 3. step to be obtained to polyester slice be added in solid phase rotary drum, and water is added not have slice, from 25 DEG C of room temperature, with every
The speed of 5 DEG C of hour is ramped up 95 DEG C, later constant temperature 8h, and until slice is fully crystallized, then discharge water discharging, passes through wind
Machine blows clean slice surface moisture.
5. 4. polyester slice that step is obtained is put into vacuum solid phase rotary drum, vacuum evacuation device is opened in sealing, will be warm
Degree is slowly increased to 100 DEG C by room temperature, controls heating-up time 12h, reaches and continues dry 6h after set temperature, sampling and testing moisture,
Meet cooling discharge after moisture requirement, whole process requires vacuum degree not less than 600pa.
According to step 1.~method 5., implement other 2-4 examples, specific data are shown in Table 1:
Table 1:
| Parameter item | Example 1 | Example 2 | Example 3 | Example 4 |
| M-phthalic acid accounts for total acid content/% | 13 | 15 | 28 | 20 |
| PBT accounts for total yield output/% | 17 | 20 | 29 | 20 |
| Polycondensation reaction temperature/DEG C | 260 | 270 | 240 | 255 |
| Polycondensation reaction time/h | 6.0 | 6.5 | 8.0 | 6.2 |
| Pre-crystallization temperature/DEG C | 95 | 90 | 80 | 100 |
| Drying temperature/DEG C | 100 | 105 | 90 | 110 |
Low melting point core-sheath silk special polyester chip of the invention, the core-skin spun compared to common low melting point polyester chip
Bicomponent filament yarn can reduce the silk that floats in spinning process to greatest extent, fracture of wire, bond bad problem, while it is multiple to improve product
The performance of plying, it is ensured that the good toughness of bicomponent filament yarn and weatherability.
It is illustrated combined with specific embodiments below:
Low melting point core-sheath silk special polyester chip produced in above example 1-4, is tested through multinomial physical and chemical indexes, will
Test result is summarized as follows listed by table 2:
Table 2:
| Project | Compare application example 1 | Compare application example 2 | Compare application example 3 | Compare application example 4 |
| Melting range/DEG C | 192-200 | 187-198 | 170-180 | 180-190 |
| Moisture content/% | 0.03 | 0.02 | 0.04 | 0.01 |
| Polymerization property viscosity (dl/g) | 0.755 | 0.758 | 0.750 | 0.760 |
| Inherent viscosity (dl/g) after drying | 0.737 | 0.740 | 0.732 | 0.741 |
| Crystallinity/% | 98.3 | 97.9 | 99.0 | 98.6 |
Embodiment described above is merely to illustrate technical idea and feature of the invention, in the art its object is to make
Technical staff it will be appreciated that the contents of the present invention and implement accordingly, patent model of the invention only cannot be limited with the present embodiment
It encloses, i.e., same changes or modifications made by all disclosed spirit are still fallen in the scope of the patents of the invention.
Claims (5)
1. a kind of for producing the polyester slice preparation method of low melting point core-sheath silk, which comprises the following steps:
(1) synthesis of polyester slice bottom material
1. M-phthalic acid and terephthaldehyde's acid blend are put into ethylene glycol solution, wherein M-phthalic acid accounts for total acid content
Molar fraction is 13%-28%, and total ethylene glycol molal quantity and total acid molal quantity ratio are 1.15-1.35, the slurry that will be mixed
It uniformly is pumped into a reaction kettle of the esterification, the uniform slurries of BHET and its derivatives intermediates are made；
2. adding PBT and auxiliary material in class reaction kettle, PBT mass accounts for the 14%-29% for participating in reaction solid gross mass,
It feeding intake and finishes, ethylene glycol and 1,4-butanediol is added and carries out alcoholysis, the molal quantity ratio of ethylene glycol and butanediol is 1.1-1.7,
Obtain uniform melting slurries；
3. the slurries for 1. obtaining step are pressed into class kettle when 2. middle slurry temperature is stabilized to 235-245 DEG C to step, wherein
The mass fraction of the class total slurries of slurries Zhan is 14%-29%, carries out the mixing of 1.5-2.0h high-speed stirred under nitrogen atmosphere, will
After mixeding liquid temperature rises to 245-255 DEG C, batch condensation polymerization reactor is pressed into through 15-25 μm of stainless steel filter by class kettle；
4. after mixed serum enters polycondensation vessel, controlling 230-280 DEG C of reaction temperature, negative pressure polymerization reaction is carried out, it is desirable that vacuum degree
≤ 30Pa under 250-280 DEG C of final temperature, controls stirring polycondensation electric current and power by equipment, synthesizes inherent viscosity in 0.750-
The high viscosity polyester of 0.770dl/g is sliced melt, then through end of extruded band, underwater pelletizer and drying machine, vibrating screen, finally obtains use
In the polyester slice of production low melting point core-sheath silk；
(2) for producing the pre-crystallized processing of polyester slice of low melting point core-sheath silk: step (1) is obtained low for producing
The polyester slice of fusing point core-sheath silk puts into solid phase rotary drum crystallization apparatus, water is added not have polyester slice, later turns solid phase
Drum crystallization apparatus sealing, opening conduits drain start rotary drum motor, and open heating, and rotary drum temperature is passed through from 35-45 DEG C
10-16h is ramped up 70-100 DEG C, starts constant temperature 3-5h later, until polyester slice is fully crystallized, then discharges water and passes through
Air-heater vibrating screen blows away surface moisture；
(3) it is dried for producing the polyester slice of low melting point core-sheath silk: pre-crystallized being cut what is handled well in step (2)
Piece is put into dryer drums, rotary drum is sealed, and close drain, is connected multistage water ring pump vacuum pipe, is started in negative pressure shape
It heats up under state, it is desirable that vacuum degree≤600Pa, temperature are ramped up 90-110 DEG C through 8-16h by 30-50 DEG C of room temperature, into constant temperature
After continue to keep negative pressure 4-6h, sampling and testing moisture content and inherent viscosity reach and start to cool down simultaneously to rotary drum after technique requires
Discharging, completes the drying process for producing the polyester slice of low melting point core-sheath silk.
2. according to claim 1 for producing the polyester slice preparation method of low melting point core-sheath silk, which is characterized in that
Auxiliary material added by class reaction kettle includes catalyst compounded, antioxidant and toner, and wherein catalyst is antimony system and titanium
System's compounding is aided with a small amount of germanium series catalysts, and antioxidant is antioxidant 1010, and toner is red blue dyestuff.
3. according to claim 2 for producing the polyester slice preparation method of low melting point core-sheath silk, which is characterized in that
It is described it is catalyst compounded add four butyl ester of phthalandione for antimony oxide, wherein antimony oxide accounts for the 20%-50% of gross mass, metatitanic acid
Four butyl esters account for 50-80%, and germanium series catalysts account for 0.1%-5%.
4. according to claim 1 for producing the polyester slice preparation method of low melting point core-sheath silk, which is characterized in that
It is in 235-275 DEG C by control polycondensation reaction temperature, in conjunction with stirring frequency conversion adjustment, realizes that polycondensation reaction reaches special in 5-8h
Property viscosity 0.750dl/g or more, meet in crystallization treatment and drying process process inherent viscosity requirement.
5. the preparation method according to any one of claims 1-4 polyester obtained for producing low melting point core-sheath silk is cut
Piece.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910778470.3A CN110358061B (en) | 2019-08-22 | 2019-08-22 | Polyester chip for producing low-melting-point sheath-core composite filament and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910778470.3A CN110358061B (en) | 2019-08-22 | 2019-08-22 | Polyester chip for producing low-melting-point sheath-core composite filament and preparation method thereof |
Publications (2)
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Cited By (4)
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| CN113005563A (en) * | 2021-02-26 | 2021-06-22 | 浙江理工大学 | Preparation method of low-melting-point PTT sheath-core composite copolyester fiber |
| CN113583228A (en) * | 2021-08-05 | 2021-11-02 | 常州浩阳新材料科技有限公司 | Synthesis method of polyester chip for high-temperature-resistant film |
| CN113736070A (en) * | 2021-09-15 | 2021-12-03 | 天津华新盈聚酯材料科技有限公司 | Polyester chip for producing vehicle-mounted perfume stick and fiber pen point and preparation method thereof |
| CN117567733A (en) * | 2024-01-16 | 2024-02-20 | 山东瑞丰高分子材料股份有限公司 | PETG copolyester and synthetic method for improving transparency of PETG copolyester |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113005563A (en) * | 2021-02-26 | 2021-06-22 | 浙江理工大学 | Preparation method of low-melting-point PTT sheath-core composite copolyester fiber |
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| CN113736070A (en) * | 2021-09-15 | 2021-12-03 | 天津华新盈聚酯材料科技有限公司 | Polyester chip for producing vehicle-mounted perfume stick and fiber pen point and preparation method thereof |
| CN117567733A (en) * | 2024-01-16 | 2024-02-20 | 山东瑞丰高分子材料股份有限公司 | PETG copolyester and synthetic method for improving transparency of PETG copolyester |
| CN117567733B (en) * | 2024-01-16 | 2024-04-02 | 山东瑞丰高分子材料股份有限公司 | PETG copolyester and synthetic method for improving transparency of PETG copolyester |
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