CN118063752A - A method for preparing modified polybutylene succinate slices and a method for preparing low-elastic yarn - Google Patents
A method for preparing modified polybutylene succinate slices and a method for preparing low-elastic yarn Download PDFInfo
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- 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
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- C08G63/00—Macromolecular compounds obtained by reactions forming a carboxylic ester link in the main chain of the macromolecule
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- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/78—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from copolycondensation products
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Abstract
本发明公开了一种改性聚丁二酸丁二醇酯切片的制备方法及低弹丝的制备方法，属于可完全生物降解高分子材料领域。在连续聚合设备上，先将丁二酸、丁二醇、官能度≧3的单体及各类催化剂、稳定剂分别按设定的比例连续稳定计量，送入浆料调配槽进行配浆，然后经酯化、缩聚工序，制得改性聚丁二酸丁二醇酯(PBS)，最后经铸带、水下切粒，制得切片粒子。合成得到的改性PBS，经纺丝工艺技术路线制得PBS预取向丝(POY)；POY再经加弹工艺制得牵伸假捻丝(DTY)。本发明制备的改性PBS具有分子量高、熔体强度大、流动性好、结晶性能可控等特点，使纺丝、加弹过程操作性优良，产品质量稳定。终端产品可在使用废弃后，被自然界的微生物或酶分解为二氧化碳和水，是一种可完全生物降解高分子材料。
The invention discloses a method for preparing a modified polybutylene succinate slice and a method for preparing a low-elastic yarn, and belongs to the field of fully biodegradable polymer materials. On a continuous polymerization device, succinic acid, butanediol, monomers with a functionality of ≧3, and various catalysts and stabilizers are firstly measured continuously and stably according to a set ratio, and then sent to a slurry mixing tank for slurry mixing, and then esterification and polycondensation processes are performed to obtain modified polybutylene succinate (PBS), and finally, strip casting and underwater pelletization are performed to obtain slice particles. The synthesized modified PBS is used to obtain PBS pre-oriented yarn (POY) through a spinning process technology route; POY is then subjected to a texturizing process to obtain a drawn false twist yarn (DTY). The modified PBS prepared by the invention has the characteristics of high molecular weight, high melt strength, good fluidity, and controllable crystallization performance, so that the spinning and texturizing processes are excellent in operability and the product quality is stable. The terminal product can be decomposed into carbon dioxide and water by microorganisms or enzymes in nature after use and disposal, and is a fully biodegradable polymer material.
Description
Technical Field
The invention relates to the technical field of completely biodegradable high polymer materials, in particular to a preparation method of modified polybutylene succinate slices and a preparation method of low stretch yarns.
Background
With the increasing prominence of environmental problems, biodegradable materials are receiving more and more attention from all countries around the world. The main chain of the aliphatic polyester contains an ester bond which is easy to hydrolyze, is flexible and is easy to degrade under the action of microorganisms through the catalysis of enzymes, and the aliphatic polyester is used as an environment-friendly material and has become a hot point for research and development worldwide. Among them, polylactic acid (PLA), polycaprolactone (PCL) and aliphatic binary alkyd polyester, such as polybutylene succinate (PBS) are successfully industrialized as a typical biodegradable aliphatic polyester, which is favored by reasonable cost performance due to excellent comprehensive performance, and is a biodegradable material with the greatest research and development at home and abroad, relatively mature technology and maximum industrialization regulation, and is one of the earlier varieties entering the market, mainly used for producing packages, films, agriculture, forestry, aquatic products, civil engineering materials, and the like, and can realize complete biodegradation after being abandoned, thereby reducing environmental pollution.
The synthetic technology route of PBS mainly comprises an esterification method, an ester exchange method, a chain extension method and the like, and research is mainly focused on research and development of a composite catalyst and how to improve the molecular weight so as to improve the melt strength, thereby improving the mechanical property, foamability and the like of the product. The patent of application number CN202011266057.8 discloses a preparation method of low-melting-point polybutylene succinate, which comprises the steps of adding succinic acid, butanediol and a composite catalyst into a reaction kettle in one step, and sequentially carrying out esterification reaction, pre-polycondensation reaction and final polycondensation reaction to obtain low-melting-point high-molecular-weight polybutylene succinate; patent application number CN201510503757.7 discloses a preparation method of poly (butylene succinate), which adopts titanium-phosphorus coordination catalyst to prepare poly (butylene succinate) with number average molecular weight more than 10 ten thousand by esterification technical route; the application number CN202210884516.1 discloses a preparation method of expandable poly (butylene succinate), wherein a polyfunctional compound is added to participate in polycondensation reaction in the PBS preparation process, so that the melt strength is improved, and silicon microspheres are added as nucleating agents to improve the hydrophobic property of PBS at the same time, so that the preparation of the expandable PBS is realized.
However, due to the aliphatic structure of PBS, the intermolecular force is small, the melt strength is low, and due to the regularity and flexibility of the PBS chain segments, the crystallinity is high, and preliminary exploratory tests show that the spinning post-processing performance of the conventional PBS is poor. Generally, the melt strength of the polymer can be improved by increasing the molecular weight, but the problems of higher melt viscosity, poor flow property and the like can occur when the molecular weight is improved, so that the spinning performance is greatly reduced; meanwhile, due to the high crystallization property of PBS, the crystallinity of the obtained nascent fiber (such as pre-oriented yarn POY) is high, the internal stress is too large to bear high-time stretching in the subsequent texturing processing process, the mechanical property of the fiber is poor, and the requirement of subsequent spinning processing cannot be met. Therefore, the application of the fiber is rarely reported in the fiber field at home and abroad in recent years. The patent application numbers CN201310146280.2 and CN201310146352.3 respectively disclose a fully biodegradable poly (butylene succinate) filament and a fully biodegradable poly (butylene succinate) filament preparation method, and the poly (butylene succinate) pre-poly (butylene succinate) filament, the fully oriented filament, the high oriented filament and the textured filament are prepared by adopting a technical route and technological parameters close to polyester fiber (terylene) by taking conventional PBS purchased in the market as a raw material, but no specific spinnability and quality index of the prepared fiber are specified.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of modified polybutylene succinate slices and a preparation method of low stretch yarns. After being used and abandoned, the end product can be decomposed into carbon dioxide and water by microorganisms or enzymes in the nature, and is a completely biodegradable high polymer material.
In order to achieve the above purpose, the present invention adopts the following technical scheme:
according to the preparation method of the modified poly (butylene succinate) slice, succinic acid, butanediol and polyol monomers are continuously and stably metered and added into a slurry kettle respectively according to the mole ratio of succinic acid to butanediol of 1:1.10-1:1.30 and the mole percentage of polyol monomers to succinic acid of 0.2-0.5%, and simultaneously titanium catalysts are added for pulping; continuously and stably conveying the obtained slurry to an esterification reaction kettle I and an esterification reaction kettle II for esterification reaction, continuously adding a stabilizer during the reaction in the esterification reaction kettle II, and controlling the esterification rate to be 97.5-99.0%; pumping the esterified substance to a polycondensation section, and controlling the temperature of the polycondensation process to be 225-240 ℃ and the vacuum degree to be 0.1-10 KPa for reaction to prepare a modified PBS melt with the number average molecular weight of 4.5-6.5 ten thousand; and granulating the melt under water by a casting belt to obtain the slice particles.
The titanium catalyst accounts for 0.45% of the mass of the succinic acid.
The titanium catalyst is at least one of tetrabutyl titanate and isopropyl titanate.
The added stabilizer accounts for 0.1 percent of the mass of the succinic acid.
The stabilizer is at least one of triphenyl phosphate, phosphorous acid and trimethyl phosphate.
The polyol monomer is glycerol or pentaerythritol.
The preparation method of the modified poly (butylene succinate) low-stretch yarn comprises the steps of taking slices prepared by the method as raw materials, drying the slices, carrying out melt transportation by a screw extruder, metering by a metering pump, extruding by a spinneret orifice, cooling by cross-blowing, oiling and winding to prepare POY; POY is then elasticized to produce DTY.
The spinning adopts 4-bit x 6-head spinning.
The POY process parameters are as follows: the slice drying temperature is 80-90 ℃ and the time is 18-24 hours, the temperature of each area of the screw extruder is 200-240 ℃, the temperature of the spinning box body is 220-240 ℃, the side blowing wind speed is 0.4-0.6 m/s, the winding speed is 2500-3000 m/min, and the oiling rate is controlled to be 1.0-1.5%.
The DTY process parameters are as follows: the first heat box temperature is 70-80 ℃, the second heat box temperature is 80-90 ℃, the draft multiple is 1.4-1.6 times, and the elasticizing speed is 400-600 m/min.
The beneficial effects of the invention are as follows:
1) By introducing the glycerol or pentaerythritol with multiple functionalities, the defect of overlong reaction time of synthesizing PBS by a common esterification polycondensation method is overcome, the polycondensation reaction time is shortened, the production efficiency is improved, and the melt degradation yellowing is avoided.
2) The method solves the contradiction of high molecular weight and poor fluidity of the conventional PBS, and can increase the melt strength and improve the melt fluidity while increasing the molecular weight, thereby improving the spinnability and the fiber mechanical property of spinning.
3) The introduction of the polyalcohol damages the regularity of macromolecular chains, so that the crystallization capability of the modified PBS is reduced, the grain size is reduced, and the drafting false twisting processing is facilitated.
4) A screw extruder is designed to be matched with a spinning process with 4 spinning positions, so that the residence time of a melt in a spinning pipeline is reduced as much as possible, and the viscosity drop in the melt conveying process is improved.
Drawings
FIG. 1 is a graph showing the crystal morphology test of the modified PBS slices prepared in examples 1-6 and comparative example 1 (corresponding to examples 1 and 1-3 in the order from left to right in FIG. 1 (a; corresponding to examples 1 and 4-6 in the order from left to right in FIG. 1 (b)).
Detailed Description
The invention is further described with reference to the drawings and detailed description which follow:
Molecular weight and distribution thereof: using a PL-GPC50 gel permeation chromatograph, 7.5 x 300mm column; a detector: a differential refractive detector; test temperature: 40 ℃; solvent flow rate: 1.0mL/min; solvent: hexafluoroisopropanol.
Intrinsic viscosity: according to GB/T14190-2008, phenol-tetrachloroethane is used as a solvent according to the mass ratio of 50:50, are tested.
B value: according to the specification of 5.5.2 in GB/T14190-2008.
Melting point and crystallinity: a DSC1 differential scanning calorimeter of Mettler-Toledo company of Switzerland is adopted, the heating and cooling speed is 10 ℃/min, the nitrogen flow rate is 50mL/min, and the temperature is kept constant at 150 ℃ for 3min to eliminate the heat history; crystallinity degree (Wherein DeltaH m is the melting heat absorption enthalpy of the modified PBS;)Melting enthalpy of adsorption at hundred crystals of pure PBS, 110J/g).
Melt index: from the determination of GBT 3682.1-2018 plastics thermoplastic melt Mass Flow Rate (MFR) and melt volume flow rate (MVR), the experimental conditions are temperature: 190 ℃, load: 2160g.
Crystallization morphology: THMS-600 hot stage polarization microscope from Linkam, england was used. The temperature was raised to 150℃at a heating rate of 100℃per minute, and the sample was kept at the temperature for 5 minutes to completely melt, followed by rapid cooling to the set temperature at a rate of 80℃per minute. Then photographing is carried out at 2min and 5min respectively, and crystal morphology and growth process in the isothermal crystallization process are observed.
Melt strength: the prepared samples were tested for melt strength using a Haul-off (melt strength) module of a capillary rheometer (Rosand RH7 CAPILLARY RHEOMETER, NETZSCH, germany). Setting the temperature of a melt cavity to 190 ℃, setting the diameter of a capillary hole special for Haul-off to be 2mm, setting the drawing distance to be 500mm, setting the piston speed to be 5mm/min in the test process, setting the drawing speed to be 10-300m/min, and setting the scanning time to be 5min.
Example 1:
Preparation of modified PBS slice: on continuous polyester equipment, continuously and stably metering succinic acid, butanediol and glycerol respectively and adding the succinic acid, the butanediol and the glycerol into a slurry kettle according to the mole ratio of the succinic acid to the butanediol of 1:1.30 and the mole percentage of the glycerol of 0.3%, and simultaneously adding a catalyst tetrabutyl titanate (accounting for 0.45% of the mass percentage of the succinic acid) into the slurry kettle for pulping; continuously and stably conveying the obtained slurry into an esterification reaction kettle I, controlling the pressure of the esterification reaction kettle I to be 0.12MPa, controlling the temperature to be 210.0 ℃ and the residence time to be 2.5 hours, conveying the material of the esterification reaction kettle I into an esterification reaction kettle II, simultaneously continuously adding a stabilizer triphenyl phosphate accounting for 0.1 percent of succinic acid in percentage by mass, controlling the temperature of the esterification reaction kettle II to be 220 ℃ and the residence time to be 0.5 hour, measuring the esterification rate to be 98.9 percent, then pumping the obtained product into a polycondensation working section, controlling the temperature of each polycondensation reaction kettle to be 235-240 ℃, automatically adjusting the vacuum degree and the polycondensation time to be 174 minutes, and extruding, casting a belt, granulating, drying and packaging by a melt pump after the melt viscosity reaches a set value (the relevant test results of slicing are shown in table 1 and figure 1).
The amounts of pentaerythritol added in examples 2-6 below are all mole percent based on succinic acid; the content of the catalyst and the stabilizer is the mass percentage of the succinic acid.
Example 2:
Sections were prepared as described in example 1, except that: the molar ratio of succinic acid to butanediol is 1:1.20, the mol percentage of glycerol to succinic acid is 0.4%, and the esterification rate is 98.2%. Controlling the temperature of each reaction kettle in polycondensation at 235-240 ℃, automatically adjusting the vacuum degree, carrying out polycondensation for 156min, extruding by a melt pump after the melt viscosity is set value, casting a belt, granulating, drying and packaging (relevant test results of slicing are shown in table 1 and figure 1).
Example 3:
sections were prepared as described in example 1, except that: the molar ratio of succinic acid to butanediol is 1:1.10, the mol percentage of glycerol to succinic acid is 0.5%, and the esterification rate is 97.6%. Controlling the temperature of each reaction kettle in polycondensation to be 235-240 ℃, automatically adjusting the vacuum degree, carrying out polycondensation for 142min, extruding by a melt pump after the melt viscosity is set value, casting a belt, granulating, drying and packaging (relevant test results of slicing are shown in table 1 and figure 1).
Example 4:
Sections were prepared as described in example 1, except that: the esterification rate was measured to be 98.8% with a succinic acid to butanediol mole ratio of 1:1.30 and pentaerythritol at a succinic acid mole percent of 0.2%. Controlling the temperature of each reaction kettle in polycondensation at 235-240 ℃, automatically adjusting the vacuum degree, carrying out polycondensation for 185min, extruding by a melt pump after the melt viscosity is set value, casting a belt, granulating, drying and packaging (relevant test results of slicing are shown in table 1 and figure 1).
Example 5:
sections were prepared as described in example 1, except that: the esterification rate was measured to be 98.1% with a succinic acid to butanediol mole ratio of 1:1.20 and pentaerythritol at a succinic acid mole percent of 0.3%. Controlling the temperature of each reaction kettle in polycondensation to be 235-240 ℃, automatically adjusting the vacuum degree, carrying out polycondensation for 160min, extruding by a melt pump after the melt viscosity is set value, granulating, and packaging (the relevant test results of the slicing are shown in table 1 and figure 1).
Example 6:
Sections were prepared as described in example 1, except that: the esterification rate was measured to be 97.7% based on a succinic acid to butanediol mole ratio of 1:1.10, pentaerythritol at a succinic acid mole percentage of 0.4%. Controlling the temperature of each reaction kettle in polycondensation at 235-240 ℃, automatically adjusting the vacuum degree, carrying out polycondensation for 130min, extruding by a melt pump after the melt viscosity is set value, casting a belt, granulating, drying, and packaging (relevant test results of slicing are shown in table 1 and figure 1).
Comparative example 1:
Sections were prepared as described in example 1, except that: according to the mol ratio of succinic acid to butanediol of 1:1.20, no glycerol is added, and the esterification rate is measured to be 98.0 percent. Controlling the temperature of each reaction kettle in polycondensation to be 235-240 ℃, automatically adjusting the vacuum degree, carrying out polycondensation for 220min, extruding by a melt pump after the melt viscosity is set value, casting a belt, granulating, drying and packaging (relevant test results of slicing are shown in table 1 and figure 1).
TABLE 1 Synthesis process of modified PBS and product test results
As can be seen from Table 1, the modified PBS obtained in examples 1 to 6 after adding glycerol or pentaerythritol has b values smaller than 10.0 and melting points slightly different from those of the PBS obtained in comparative example 1 without adding glycerol or pentaerythritol, but the modified PBS has lower intrinsic viscosity and higher number average and weight average molecular weight and lower molecular weight dispersion coefficient under the same final polycondensation discharge power; the modified PBS's of examples 1-6, which had melt indices higher than those of the PBS's of comparative example 1, showed good melt flowability without deterioration due to an increase in molecular weight; the modified PBS's of examples 1-6 all had higher melt strength than the PBS's of comparative example 1, demonstrating better ability of the melt trickle to withstand spinning stress during spinning; the crystallinity of the modified PBS of examples 1-6 was lower than that of the PBS of comparative example 1, indicating that the addition of the modified monomer destroyed the regularity of the molecular chain, and the crystallinity of the modified PBS was lower than that of PBS, which was advantageous for the subsequent processing of drawing false twist. As can be seen from fig. 1, the modified PBS added with different GL and PER contents has smaller grain size compared with pure PBS, and is also beneficial to the processing of the subsequent drawing false twist.
Example 7:
Taking the modified PBS prepared in the example 2 as a raw material, and preparing the POY with the specification of 105dtex/24f on corresponding filament production equipment through slicing and drying, melting and conveying by a screw extruder, metering by a metering pump, extruding by a spinneret orifice, cooling by a lateral blowing, oiling and winding; the POY is then elasticized to produce DTY with the specification of 65dtex/24 f.
Slicing and drying at 80-90 ℃ for 18 hours; the temperature of each area of the screw extruder is 200-240 ℃; spinning box: 4-position x 6-head spinning (namely, a screw extruder is adopted to be matched with 4 spinning positions), and the temperature of a spinning box body is 220 ℃; the air speed of the lateral blowing air is 0.4m/s; the winding speed is 2500m/min; the oil application rate is controlled to be 1.0%. The first hot box temperature is 70 ℃, the second hot box temperature is 80 ℃, the draft multiple is 1.6 times, and the processing speed is 400m/min. The filament performance test results are shown in table 2.
Example 8:
Taking the modified PBS prepared in the example 2 as a raw material, and preparing the POY with the specification of 165dtex/36f on corresponding filament production equipment through slicing and drying, melting and conveying by a screw extruder, metering by a metering pump, extruding by a spinneret orifice, cooling by a lateral blowing, oiling and winding; the POY is then elasticized to produce DTY with 110dtex/36f specification.
The slice drying temperature is 80-90 ℃ and the time is 21 hours, the temperature of each area of the screw extruder is 200-240 ℃, and the spinning box body is: 4-position X6-head spinning (namely, a screw extruder is adopted to be matched with 4 spinning positions), the temperature of a spinning box body is 230 ℃, the wind speed of side blowing is 0.5m/s, the winding speed is 2750m/min, and the oiling rate is controlled to be 1.25%; the temperature of the first hot box is 75 ℃, the temperature of the second hot box is 85 ℃, the drafting multiple is 1.5 times, and the processing speed is 500m/min. The filament performance test results are shown in table 2.
Example 9:
Taking the modified PBS prepared in the example 2 as a raw material, and preparing the POY with the specification of 231dtex/48f on corresponding filament production equipment through slicing and drying, melting and conveying by a screw extruder, metering by a metering pump, extruding by a spinneret orifice, cooling by a lateral blowing, oiling and winding; the POY is then elasticized to produce DTY with 165dtex/48f specification.
The slice drying temperature is 80-90 ℃ and the time is 24 hours, the temperature of each area of the screw extruder is 200-240 ℃, and the spinning box body is: 4-position X6-head spinning (namely, a screw extruder is adopted to be matched with 4 spinning positions), the temperature of a spinning box body is 240 ℃, the wind speed of side blowing is 0.6m/s, the winding speed is 3000m/min, and the oiling rate is controlled to be 1.50%. The temperature of the first hot box is 80 ℃, the temperature of the second hot box is 90 ℃, the drafting multiple is 1.4 times, and the processing speed is 600m/min. The filament performance test results are shown in table 2.
Example 10:
Taking the modified PBS prepared in the example 5 as a raw material, and preparing the POY with the specification of 105dtex/24f on corresponding filament production equipment through slicing and drying, melting and conveying by a screw extruder, metering by a metering pump, extruding by a spinneret orifice, cooling by a lateral blowing, oiling and winding; the POY is then elasticized to produce DTY with the specification of 65dtex/24 f.
The slice drying temperature is 80-90 ℃ and the time is 18 hours, the temperature of each area of the screw extruder is 200-240 ℃, and the spinning box body is: 4-position X6-head spinning (namely, a screw extruder is adopted to be matched with 4 spinning positions), the temperature of a spinning box body is 220 ℃, the wind speed of side blowing is 0.4m/s, the winding speed is 2500m/min, and the oiling rate is controlled to be 1.0%. The first hot box temperature is 70 ℃, the second hot box temperature is 80 ℃, the draft multiple is 1.6 times, and the processing speed is 400m/min. The filament performance test results are shown in table 2.
Example 11:
Taking the modified PBS prepared in the example 5 as a raw material, and preparing the POY with the specification of 165dtex/36f on corresponding filament production equipment through slicing and drying, melting and conveying by a screw extruder, metering by a metering pump, extruding by a spinneret orifice, cooling by a lateral blowing, oiling and winding; the POY is then elasticized to produce DTY with 110dtex/36f specification.
The slice drying temperature is 80-90 ℃ and the time is 21 hours, the temperature of each area of the screw extruder is 200-240 ℃, and the spinning box body is: 4-position X6-head spinning (namely, a screw extruder is adopted to be matched with 4 spinning positions), the temperature of a spinning box body is 230 ℃, the wind speed of side blowing is 0.5m/s, the winding speed is 2750m/min, and the oiling rate is controlled to be 1.25%. The temperature of the first hot box is 75 ℃, the temperature of the second hot box is 85 ℃, the drafting multiple is 1.5 times, and the processing speed is 500m/min. The filament performance test results are shown in table 2.
Example 12:
Taking the modified PBS prepared in the example 5 as a raw material, and preparing the POY with the specification of 231dtex/48f on corresponding filament production equipment through slicing and drying, melting and conveying by a screw extruder, metering by a metering pump, extruding by a spinneret orifice, cooling by a lateral blowing, oiling and winding; the POY is then elasticized to produce DTY with 165dtex/48f specification.
The slice drying temperature is 80-90 ℃ and the time is 24 hours, the temperature of each area of the screw extruder is 200-240 ℃, and the spinning box body is: 4-position X6-head spinning (namely, a screw extruder is adopted to be matched with 4 spinning positions), the temperature of a spinning box body is 240 ℃, the wind speed of side blowing is 0.6m/s, the winding speed is 3000m/min, and the oiling rate is controlled to be 1.50%; the temperature of the first hot box is 80 ℃, the temperature of the second hot box is 90 ℃, the drafting multiple is 1.4 times, and the processing speed is 600m/min. The filament performance test results are shown in table 2.
Comparative example 2
The modified PBS prepared in comparative example 1 is used as a raw material, and POY with the specification of 165dtex/36f is prepared on corresponding filament production equipment through slicing and drying, melt conveying by a screw extruder, metering by a metering pump, extrusion by a spinneret orifice, cross-air cooling, oiling and winding; the POY is then elasticized to produce DTY with 110dtex/36f specification.
The slice drying temperature is 80-90 ℃ and the time is 21 hours, the temperature of each area of the screw extruder is 200-240 ℃, and the spinning box body is: 4-position X6-head spinning (namely, a screw extruder is adopted to be matched with 4 spinning positions), the temperature of a spinning box body is 230 ℃, the wind speed of side blowing is 0.5m/s, the winding speed is 2750m/min, and the oiling rate is controlled to be 1.25%. The temperature of the first hot box is 75 ℃, the temperature of the second hot box is 85 ℃, the drafting multiple is 1.5 times, and the processing speed is 500m/min. The filament performance test results are shown in table 2.
TABLE 2 fiber processing conditions and product test results
As can be seen from Table 2, the modified PBS obtained in examples 7 to 12 by adding glycerol or pentaerythritol has good spinning spinnability, and the obtained POY has higher breaking strength and lower elongation at break, can well meet the processing of DTY, and has higher breaking strength and excellent processability. In comparative example 2, pure PBS obtained without glycerol or pentaerythritol had a remarkable phenomenon of yarn floating during spinning, and poor spinnability, and the obtained POY had a low breaking strength and a large elongation at break, but the DTY obtained after drawing false twisting had a lower breaking strength than POY, and was easily broken and had poor processability.
In the invention, when the modified PBS slice is prepared, tetrabutyl titanate can be replaced by isopropyl titanate, triphenyl phosphate can be replaced by one of phosphorous acid and trimethyl phosphate, and the modified PBS slice and the modified polybutylene succinate low-elastic yarn with the same performance are also prepared.
The foregoing description of the preferred embodiments of the invention is not intended to limit the invention to the precise form disclosed, and any such modifications, equivalents, and alternatives falling within the spirit and scope of the invention are intended to be included within the scope of the invention.
Claims (10)
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| CN202410234252.4A CN118063752A (en) | 2024-03-01 | 2024-03-01 | A method for preparing modified polybutylene succinate slices and a method for preparing low-elastic yarn |
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| CN202410234252.4A CN118063752A (en) | 2024-03-01 | 2024-03-01 | A method for preparing modified polybutylene succinate slices and a method for preparing low-elastic yarn |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118773918A (en) * | 2024-09-09 | 2024-10-15 | 山东道恩高分子材料股份有限公司 | A softener for ultra-soft and degradable spunbond nonwoven fabrics and its preparation method and application |
| TWI892855B (en) * | 2024-10-04 | 2025-08-01 | 福盈生物材料股份有限公司 | Method for preparation of polybutylene succinate or its copolyester |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118773918A (en) * | 2024-09-09 | 2024-10-15 | 山东道恩高分子材料股份有限公司 | A softener for ultra-soft and degradable spunbond nonwoven fabrics and its preparation method and application |
| TWI892855B (en) * | 2024-10-04 | 2025-08-01 | 福盈生物材料股份有限公司 | Method for preparation of polybutylene succinate or its copolyester |
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