CN112708961A - POY pre-network filament and processing technology thereof - Google Patents
POY pre-network filament and processing technology thereof Download PDFInfo
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- 238000012545 processing Methods 0.000 title claims abstract description 16
- 238000005516 engineering process Methods 0.000 title abstract description 7
- 229920000728 polyester Polymers 0.000 claims abstract description 55
- 229920000168 Microcrystalline cellulose Polymers 0.000 claims abstract description 39
- 239000008108 microcrystalline cellulose Substances 0.000 claims abstract description 39
- 235000019813 microcrystalline cellulose Nutrition 0.000 claims abstract description 39
- 229940016286 microcrystalline cellulose Drugs 0.000 claims abstract description 39
- 238000001816 cooling Methods 0.000 claims abstract description 30
- 239000004200 microcrystalline wax Substances 0.000 claims abstract description 30
- 235000019808 microcrystalline wax Nutrition 0.000 claims abstract description 30
- 238000000034 method Methods 0.000 claims abstract description 28
- 230000006855 networking Effects 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 15
- 238000001125 extrusion Methods 0.000 claims abstract description 8
- 238000004804 winding Methods 0.000 claims abstract description 8
- 238000007493 shaping process Methods 0.000 claims abstract description 3
- 238000010438 heat treatment Methods 0.000 claims description 35
- DTQVDTLACAAQTR-UHFFFAOYSA-N Trifluoroacetic acid Chemical compound OC(=O)C(F)(F)F DTQVDTLACAAQTR-UHFFFAOYSA-N 0.000 claims description 30
- 238000002156 mixing Methods 0.000 claims description 27
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 26
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 26
- 239000004359 castor oil Substances 0.000 claims description 24
- 235000019438 castor oil Nutrition 0.000 claims description 24
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 24
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical group O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 24
- -1 polybutylene terephthalate Polymers 0.000 claims description 22
- 230000008569 process Effects 0.000 claims description 20
- 239000007789 gas Substances 0.000 claims description 18
- 238000003756 stirring Methods 0.000 claims description 18
- 239000002202 Polyethylene glycol Substances 0.000 claims description 17
- 229920001223 polyethylene glycol Polymers 0.000 claims description 17
- 239000004698 Polyethylene Substances 0.000 claims description 12
- 229920000573 polyethylene Polymers 0.000 claims description 12
- 229920001707 polybutylene terephthalate Polymers 0.000 claims description 10
- 238000009987 spinning Methods 0.000 claims description 9
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 208000012886 Vertigo Diseases 0.000 claims description 8
- 238000009423 ventilation Methods 0.000 claims description 8
- 239000011148 porous material Substances 0.000 claims description 5
- 238000009998 heat setting Methods 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 235000010675 chips/crisps Nutrition 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000002243 precursor Substances 0.000 claims description 2
- 238000004321 preservation Methods 0.000 claims description 2
- 230000000694 effects Effects 0.000 abstract description 15
- 238000004519 manufacturing process Methods 0.000 abstract description 13
- 239000000835 fiber Substances 0.000 abstract description 8
- 239000000126 substance Substances 0.000 abstract description 4
- 230000000052 comparative effect Effects 0.000 description 15
- 239000000203 mixture Substances 0.000 description 14
- 239000005020 polyethylene terephthalate Substances 0.000 description 13
- 229920004934 Dacron® Polymers 0.000 description 12
- 238000002474 experimental method Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 7
- 238000001035 drying Methods 0.000 description 6
- 238000002844 melting Methods 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 238000004132 cross linking Methods 0.000 description 4
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- 239000002131 composite material Substances 0.000 description 2
- 229910001873 dinitrogen Inorganic materials 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 238000010309 melting process Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 239000001993 wax Substances 0.000 description 2
- 239000008118 PEG 6000 Substances 0.000 description 1
- 229920002584 Polyethylene Glycol 6000 Polymers 0.000 description 1
- 229920004933 Terylene® Polymers 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 229940126678 chinese medicines Drugs 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000007334 copolymerization reaction Methods 0.000 description 1
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- 238000009826 distribution Methods 0.000 description 1
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- 230000017525 heat dissipation Effects 0.000 description 1
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- 238000005259 measurement Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
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Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/92—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of polyesters
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
Landscapes
- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Treatments For Attaching Organic Compounds To Fibrous Goods (AREA)
Abstract
The application relates to the field of chemical fiber industry, in particular to a POY pre-network filament and a processing technology thereof. The POY pre-network filament comprises the following raw materials: the POY pre-network filament is prepared from polyester chips, microcrystalline wax, a compatilizer and microcrystalline cellulose through the steps of preheating, melt extrusion, oiling, cooling, drafting, shaping, networking and winding. In addition, the production method of the POY pre-network filament is further provided, wherein the preheating temperature of the polyester chips is 150-215 ℃, and the preheating time is 145-210 min. The method and the device can reduce the preheating time required by the POY pre-network filament in the production process, and have the effects of saving energy and reducing the production cost of enterprises.
Description
Technical Field
The application relates to the field of chemical fiber industry, in particular to a POY pre-network filament and a processing technology thereof.
Background
POY, i.e. pre-oriented yarn, has at present had a sufficient market prospect and a more mature process. In the prior art, POY processing generally includes the steps of preheating, spinning, cooling, oiling, networking, winding and the like, wherein the preheating step mainly aims to improve the crystallinity of the polyester chips, reduce the softening temperature of the polyester chips, and dry the polyester chips.
Generally, the preheating process of the polyester chips needs to be carried out by heating for multiple times, each heating process needs several hours, and a large amount of cost is increased for enterprise production.
Disclosure of Invention
In order to reduce the preheating time of the POY silk thread and reduce the production cost of enterprises, the application provides the POY pre-network filament and the processing technology thereof.
In a first aspect, the present application provides a POY pre-networking filament, which adopts the following technical scheme:
the POY pre-network filament comprises the following raw materials in parts by mass:
polyester slicing: 130-160 parts;
microcrystalline wax: 25-40 parts;
a compatilizer: 10-20 parts;
microcrystalline cellulose: 2-7 parts;
the POY pre-network filament is obtained through the steps of preheating, melt extrusion, oiling, cooling, drafting, shaping, networking and winding.
In the technical scheme, the microcrystalline wax and the microcrystalline cellulose are added into the polyester chips and have combined action, so that the softening temperature of the polyester chips can be reduced, the crystallization of the polyester chips can be promoted, and the tackifying effect to a certain degree can be achieved. The addition of the compatilizer can keep the materials in a more uniform mixed state after melting. After the technical scheme is adopted, the preheating time of the polyester chips can be reduced to 150-200 min, and the properties of the POY pre-network filaments obtained by the production of the polyester chips are not obviously changed, so that the production cost of enterprises is remarkably reduced,
preferably, the compatilizer is maleic anhydride, polybutylene terephthalate and maleic anhydride graft modified polyethylene, wherein the mass ratio of the sum of the maleic anhydride and the polybutylene terephthalate to the maleic anhydride graft modified polyethylene is 1 (0.3-0.6) to 1.2-4.
In the technical scheme, the combination of maleic anhydride, polybutylene terephthalate and maleic anhydride graft modified polyethylene is selected, so that on one hand, the uniformity and compatibility of the whole system can be further improved, and meanwhile, the composite system is also beneficial to guiding polyester fibers in polyester chips to form a better cross-linking state in the melting process, so that the prepared POY filaments have better strength.
Preferably, the raw materials of the POY pre-network filament further comprise 1.5-2.4 parts by mass of polyethylene glycol and 0.8-1.3 parts by mass of trifluoroacetic acid.
The polyethylene glycol and the trifluoroacetic acid can reduce the generated pore structure on the silk thread in the melting process, improve the strength of the silk thread and reduce the probability of silk thread breakage.
Preferably, the raw material of the POY pre-network filament further comprises 7-15 parts by mass of castor oil.
Castor oil can play the effect of solvent on the one hand, in the heating process, can dissolve microcrystalline wax and microcrystalline cellulose on the one hand, makes microcrystalline wax and microcrystalline cellulose mix with the dacron section more fully, also can improve the sliced drying effect of dacron simultaneously, makes the dacron section can be dried more rapidly in short time.
Preferably, the raw material of the POY pre-network filament further comprises 6-12 parts by mass of acrylic acid.
Acrylic acid can take place the polymerization crosslinking effect of certain degree between the dacron section at the in-process that preheats, has the effect of tackifing on the one hand, makes the POY silk intensity that obtains in the follow-up course of working higher, and simultaneously, there is polar group on the terminal group of acrylic acid, consequently can improve the mixing degree of consistency between microcrystalline cellulose and the dacron section, and then improves the quality of silk thread.
In a second aspect, the present application provides a processing technology of a POY pre-network filament, which is used for producing the above POY pre-network filament, and adopts the following technical scheme:
the method comprises the following steps:
s1, preheating polyester chips, microcrystalline wax, microcrystalline cellulose, castor oil and acrylic acid to obtain a first mixed system, wherein the preheating temperature is 150-215 ℃, and the preheating time is 145-210 min;
s2, adding a compatilizer into the first blending system, heating to 144-150 ℃, and continuously and uniformly mixing to obtain a second blending system;
s3, heating the second blending system to be molten, adding a pore eliminating agent, continuously mixing for 5-10 min, and performing spinning treatment to obtain precursor;
and S4, cooling the protofilament obtained in the step S3, oiling, drafting and heat setting, pre-networking, winding and forming to obtain the POY pre-networking filament.
Through adopting above-mentioned technical scheme, carry out preheating treatment to micrite wax, microcrystalline cellulose, castor oil, dacron section and acrylic acid earlier, under the solubilization of castor oil, soften the dacron section through micrite wax and microcrystalline cellulose, the compatilizer is added after preheating and accomplishing again, has reduced the compatilizer and has taken place excessive coupling with the dacron section at preheating the in-process, and then leads to the phenomenon of dacron section caking to take place. The hole eliminating agent is added after the system is melted, and the POY filament with uniform and stable integral structure, less cracks and high strength can be obtained by immediately carrying out spinning treatment after the hole elimination.
Preferably, in step S1, the preheating process is performed by the following steps:
s1-1, mixing the polyester chips, the microcrystalline wax and the castor oil, heating to 153-158 ℃, stirring, and keeping for 40-50 min;
s1-2, after the step S1-1 is finished, introducing dry gas with the temperature of-20-0 ℃ into the system, wherein the introduction speed of the gas corresponding to each kilogram of polyester chips is 0.1-0.4 m3/S, and the introduction time is 15-25 min;
s1-3, after the step S1-2 is finished, adding microcrystalline cellulose into the system, heating the system to 162-166 ℃ again, and continuing to keep the temperature and mix for 60-80 min;
s1-4, after the step S1-3 is finished, introducing dry gas with the temperature of-20-0 ℃ into the system, wherein the introduction speed of the gas corresponding to each kilogram of polyester chips is 0.1-0.4 m3/S, and the introduction time is 10-15 min;
s1-5, after the step S1-4 is finished, putting acrylic acid into the system, heating the system to 206-215 ℃ again, and continuing to mix for 30-40 min in a heat preservation mode;
s1-6, cooling the system to 20-30 ℃ under the condition of keeping dry.
In the technical scheme, the mode of heating many times is adopted for preheating treatment, the polyester slices are mixed with the microcrystalline wax, so that the microcrystalline wax is adsorbed on the surface of the polyester slices firstly, then the microcrystalline cellulose is added, and in the process, the moisture in the polyester slices is primarily dried and is not easily adsorbed by the microcrystalline cellulose, so that the drying effect in the preheating process is improved.
In addition, in the process, the steps of heating-cooling-heating are adopted, and dry low-temperature gas is introduced into the system during cooling, so that on one hand, the gas flow can quickly take away the moisture in the system, the drying effect is improved, and meanwhile, the process of introducing cold air is also beneficial to reducing the melting or agglomeration of the polyester chips due to overheating.
In addition, in the system, acrylic acid is added in the step S1-5, and when the step S1-5 is carried out, the polyester chips are basically crystallized and dried, and at the moment, the acrylic acid is added to form a crosslinking system, so that the drying and crystallization effects of the polyester cannot be influenced.
Preferably, in the step S1-2 and the step S1-4, the introduced dry gas is nitrogen.
In the scheme, the nitrogen is selected to reduce the oxidation of materials (such as microcrystalline cellulose and castor oil) in the system at high temperature, so that the strength of the obtained silk thread is improved, and the silk thread has better quality.
Preferably, in step S3, the spinning process is performed using a twin-screw extruder, and the temperature of the extrusion head is 318 to 324 ℃.
In the technical scheme, the spinning temperature is specifically set, and due to the existence of the microcrystalline wax and the microcrystalline cellulose, the spinning temperature is slightly lower than that in a normal condition, so that the yarn strength is better.
In summary, the present application has the following beneficial effects:
1. in this application, through microcrystalline wax and microcrystalline cellulose's combined action, help drying and the crystallization process of accelerating the dacron section, reduce the time that the process of preheating needs to reduce the manufacturing cost of enterprise.
2. Castor oil is added in the further setting of this application, helps improving microcrystalline wax and microcrystalline cellulose and dacron sliced mixed effect to improve dacron sliced drying effect, thereby obtain the higher POY filament yarn of intensity.
3. The application provides a processing technology of a POY pre-network filament, the preheating time is short in the processing process, and the energy consumption and the production cost of enterprises are reduced.
Detailed Description
The present application will be described in further detail with reference to examples and comparative examples.
The POY pre-network filament is a chemical fiber raw material widely applied to the field of textile, and is obtained by processing polyester chips through a series of treatment processes after hot melting and extrusion. Generally, the polyester chips are subjected to a long-time preheating treatment before processing, so that the moisture in the polyester chips is removed, the crystallinity of the polyester chips is improved, and the softening point of the polyester chips is reduced. The above process generally requires tens of hours or even tens of hours, and for enterprises, the large time cost and energy consumption will undoubtedly bring a heavy burden to the enterprises.
For a long time, the applicant has conducted a great deal of research aiming at the above problems, and finally found that the time required for preheating can be reduced by adding the composite system of microcrystalline wax and microcrystalline cellulose into the preheating process of polyester chips, and the strength of the obtained POY pre-network filaments is not obviously reduced. The present application has been made based on the above findings.
Some of the raw material purchase sources used in this application are shown in table 1.
TABLE 1 partial raw materials Source Table
| Raw materials | Manufacturer or model |
| Polyester chip | Dupont L2268 |
| Microcrystalline wax | SINOPEC NANYANG ENERGY CHEMICAL Co.,Ltd. |
| Microcrystalline cellulose | Shanghai Jizhi Biochemical Technology Co.,Ltd. |
| Maleic anhydride graft modified polyethylene | SHANGHAI MACKLIN BIOCHEMICAL Co.,Ltd. |
| Polyethylene glycol | PEG-6000 as group of Chinese medicines |
| Castor oil | Zhengzhou Mofu chemical products Co., Ltd |
Examples 1 to 16
The POY pre-network filament comprises the raw materials in percentage by mass as shown in Table 2.
TABLE 2 ingredient tables for materials of examples 1 to 16 and comparative examples 1 to 3
| Composition (I) | Polyester chip | Microcrystalline wax | Microcrystalline cellulose | Compatilizer | Polyethylene glycol | Trifluoroacetic acid | Castor oil | Acrylic acid |
| Example 1 | 140 | 30 | 6 | 16 | 0 | 0 | 0 | 0 |
| Example 2 | 150 | 35 | 4 | 13 | 0 | 0 | 0 | 0 |
| Example 3 | 160 | 25 | 2 | 10 | 0 | 0 | 0 | 0 |
| Example 4 | 130 | 40 | 7 | 20 | 0 | 0 | 0 | 0 |
| Example 5 | 150 | 35 | 4 | 13 | 1.8 | 1.0 | 0 | 0 |
| Example 6 | 150 | 35 | 4 | 13 | 1.5 | 1.3 | 0 | 0 |
| Example 7 | 150 | 35 | 4 | 13 | 2.4 | 0.8 | 0 | 0 |
| Example 8 | 150 | 35 | 4 | 13 | 1.8 | 0 | 0 | 0 |
| Example 9 | 150 | 35 | 4 | 13 | 0 | 1.0 | 0 | 0 |
| Example 10 | 150 | 35 | 4 | 13 | 0 | 0 | 10 | 0 |
| Example 11 | 150 | 35 | 4 | 13 | 0 | 0 | 7 | 0 |
| Example 12 | 150 | 35 | 4 | 13 | 0 | 0 | 15 | 0 |
| Example 13 | 150 | 35 | 4 | 13 | 0 | 0 | 0 | 6 |
| Example 14 | 150 | 35 | 4 | 13 | 0 | 0 | 0 | 12 |
| Example 15 | 150 | 35 | 4 | 13 | 0 | 0 | 10 | 12 |
| Practice ofExample 16 | 150 | 35 | 4 | 13 | 1.8 | 1.0 | 10 | 12 |
| Comparative example 1 | 185 | 0 | 4 | 13 | 0 | 0 | 0 | 0 |
| Comparative example 2 | 154 | 35 | 0 | 13 | 0 | 0 | 0 | 0 |
| Comparative example 3 | 150 | 35 | 4 | 0 | 0 | 0 | 0 | 0 |
Wherein the compatilizer is maleic anhydride, polybutylene terephthalate and maleic anhydride graft modified polyethylene with the mass ratio of 1:0.5: 2.
Each portion of material in Table 2 refers to 50g of the material.
The POY pre-network filament is produced by the following steps:
s1, carrying out preheating treatment on the polyester chips, the microcrystalline wax, the microcrystalline cellulose, the castor oil (if the mass part is 0, the microcrystalline cellulose is not added) and the acrylic acid (if the mass part is 0, the acrylic acid is not added) to obtain a first blending system;
s2, adding a compatilizer into the first blending system, heating to 144 ℃, and continuously and uniformly mixing to obtain a second blending system;
s3, heating the second blending system to be molten, adding polyethylene glycol and trifluoroacetic acid (if the mass part is 0, the polyethylene glycol and the trifluoroacetic acid are not added), continuously mixing for 5min, and carrying out spinning through a double-screw extruder to obtain protofilaments, wherein the temperature of each section of the double-screw extruder from a feeding port is 315 ℃, 330 ℃ and 336 ℃, the length ratio of the three sections is 2:3:2, and the temperature of an extrusion head is 318 ℃.
And S4, cooling and oiling the raw filaments, drafting, performing heat setting in an oven, performing pre-networking treatment by using a pre-networking machine after the heat setting is finished, and then winding and forming to obtain the POY pre-networking filaments.
In step S1, the method specifically includes the following steps:
s1-1, mixing the polyester chips, the microcrystalline wax and the castor oil, heating to 153 ℃, and stirring at the speed of 120r/min for 40 min;
s1-2, after the step S1-1 is finished, naturally cooling the system to be lower than 30 ℃, and continuously keeping for 25min after cooling;
s1-3, after the step S1-2 is finished, adding microcrystalline cellulose into the system, heating the system again to 162 ℃, and stirring the mixture for 60min at the speed of 120 r/min;
s1-4, after the step S1-3 is finished, naturally cooling the system to be lower than 30 ℃, and continuously keeping for 15min after cooling;
s1-5, after the step S1-4 is finished, adding acrylic acid into the system, heating to 206 ℃, and continuing stirring for 30min at the speed of 80 r/min;
s1-6, cooling the system to 30 ℃ by water cooling.
Meanwhile, for examples 1 to 16, comparative examples were set as follows.
Comparative examples 1 to 3
A POY pre-network filament, which differs from example 1 in that its raw material composition is shown in table 1.
Example 17
A POY pre-network filament differs from example 16 in that the compatibilizer is a mixture of maleic anhydride, polybutylene terephthalate, and maleic anhydride graft-modified polyethylene in a mass ratio of 1:0.3: 1.2.
Example 18
A POY pre-network filament differs from example 16 in that the compatibilizer is a mixture of maleic anhydride, polybutylene terephthalate, and maleic anhydride graft-modified polyethylene in a mass ratio of 1:0.6: 4.
Example 19
A POY pre-network filament differs from example 16 in that the compatibilizer is a mixture of maleic anhydride and polybutylene terephthalate in a mass ratio of 1: 0.5.
Example 20
A POY pre-network filament differs from example 16 in that the compatibilizer is a mixture of maleic anhydride, maleic anhydride graft-modified polyethylene in a mass ratio of 1: 2.
Example 21
A POY pre-network filament differs from example 16 in that the compatibilizer is a mixture of maleic anhydride, maleic anhydride graft-modified polyethylene in a mass ratio of 1: 4.
Example 22
A POY pre-web filament differs from example 16 in that in step S1, the following processing is specifically performed:
s1-1, mixing the polyester chips, the microcrystalline wax and the castor oil, heating to 153 ℃, and stirring at the speed of 120r/min for 40 min;
s1-2, after the step S1-1 is finished, dry air with the temperature of minus 20 ℃ is introduced into the system, and the introduction speed of the gas corresponding to each kilogram of polyester chips is 0.1m3The ventilation time is 25 min;
s1-3, after the step S1-2 is finished, adding microcrystalline cellulose into the system, heating the system again to 162 ℃, and stirring the mixture for 60min at the speed of 120 r/min;
s1-4, after the step S1-3 is finished, dry air with the temperature of-20 ℃ is introduced into the system, and the introduction speed of the gas corresponding to each kilogram of polyester chips is 0.3m3The ventilation time is 10 min;
s1-5, after the step S1-4 is finished, adding acrylic acid into the system, heating to 206 ℃, and continuing stirring for 30min at the speed of 80 r/min;
s1-6, cooling the system to 30 ℃ by water cooling.
Example 23
A POY pre-network filament, which is different from embodiment 22 in that step S1 is specifically processed as follows:
s1-1, mixing the polyester chips, the microcrystalline wax and the castor oil, heating to 155 ℃, and stirring at the speed of 120r/min for 45 min;
s1-2, after the step S1-1 is finished, dry air with the temperature of minus 10 ℃ is introduced into the system, and the introduction speed of the gas corresponding to each kilogram of polyester chips is 0.3m3The ventilation time is 20 min;
s1-3, after the step S1-2 is finished, adding microcrystalline cellulose into the system, heating the system again to 164 ℃, and stirring the mixture for 70min at the speed of 120 r/min;
s1-4, after the step S1-3 is finished, dry air with the temperature of-10 ℃ is introduced into the system, and the introduction speed of the gas corresponding to each kilogram of polyester chips is 0.3m3The ventilation time is 12 min;
s1-5, after the step S1-4 is finished, adding acrylic acid into the system, heating to 210 ℃, and continuing stirring for 35min at the speed of 80 r/min;
s1-6, cooling the system to 25 ℃ by water cooling.
Example 24
A POY pre-network filament, which is different from embodiment 22 in that step S1 is specifically processed as follows:
s1-1, mixing the polyester chips, the microcrystalline wax and the castor oil, heating to 158 ℃, and stirring at the speed of 120r/min for 50 min;
s1-2, after the step S1-1 is finished, dry air with the temperature of 0 ℃ is introduced into the system, and the introduction speed of the gas corresponding to each kilogram of polyester chips is 0.4m3The ventilation time is 25 min;
s1-3, after the step S1-2 is finished, adding microcrystalline cellulose into the system, heating the system to 166 ℃ again, and stirring the mixture for 80min at the speed of 120 r/min;
s1-4, after the step S1-3 is finished, dry air with the temperature of 0 ℃ is introduced into the system, and the introduction speed of the gas corresponding to each kilogram of polyester chips is 0.4m3The ventilation time is 15 min;
s1-5, after the step S1-4 is finished, adding acrylic acid into the system, heating to 215 ℃, and continuing stirring for 40min at the speed of 80 r/min;
s1-6, cooling the system to 20 ℃ by water cooling.
Example 25
A POY pre-network filament, different from example 23, was blown with dry nitrogen gas instead of dry air in step S1-2 and step S1-4.
Example 26
A POY pre-network filament, which is different from example 23 in that acrylic acid was added to the system in step S1-1.
Example 27
A POY pre-network filament, which is different from example 23 in that microcrystalline cellulose was added to the system in step S1-1.
Example 28
A POY pre-network filament, different from example 23 in that polyethylene glycol and trifluoroacetic acid were added to the system in S1-1.
Example 29
A POY pre-network filament, different from example 23 in that polyethylene glycol and trifluoroacetic acid were added to the system in S1-1.
Example 30
A POY pre-network filament, which is different from embodiment 23 in that the step S1 specifically includes the following steps:
mixing the polyester chips, microcrystalline wax, castor oil, microcrystalline cellulose and acrylic acid, heating to 210 ℃, keeping the temperature for 120min, and then cooling the system to 20 ℃ by water cooling.
Example 31
A POY pre-network filament, which is different from embodiment 23 in that the step S1 specifically includes the following steps:
s1-1, mixing the polyester chips, the microcrystalline wax and the castor oil, heating to 155 ℃, and stirring at the speed of 120r/min for 45 min;
s1-2, adding microcrystalline cellulose into the system, continuously heating to 164 ℃, and stirring at the speed of 120r/min for 70 min;
s1-3, adding acrylic acid into the system, continuously heating to 210 ℃, and continuously stirring for 35min at the speed of 80 r/min;
s1-4, cooling the system to 25 ℃ by water cooling.
The following experiments were set up for the above examples and comparative examples to determine the properties of the POY pre-network filaments produced therefrom.
Experiment 1, fiber strength experiment: the filaments were tested for strength according to the method of GB/T19975-2005 high tenacity filament tensile test method.
Experiment 2, production experiment: for the above examples and comparative examples, production was carried out for 24 hours, and the number of times of occurrence of yarn breakage was observed.
First, experiments 1 and 2 were performed on examples 1 to 4 and comparative examples 1 to 3, and the measurement results are shown in table 3.
Table 3, examples 1 to 4 and comparative examples 1 to 3
| Examples | Breaking strength (cN/dtex) | Number of filament breakage |
| Example 1 | 2.04 | 3 |
| Example 2 | 2.05 | 3 |
| Example 3 | 2.05 | 2 |
| Example 4 | 2.02 | 4 |
| Comparative example 1 | 1.23 | 19 |
| Comparative example 2 | 1.14 | 10 |
| Comparative example 3 | 1.29 | 12 |
As can be seen from the above examples and comparative examples, in the present application, the addition of microcrystalline cellulose and microcrystalline wax, and the adjustment of the compatibility between the components by the compatibilizer, contribute to the reduction of the preheating time required for the reaction. Obviously, the lack of microcrystalline cellulose or the lack of microcrystalline wax causes the POY pre-network filaments to require a long preheating time, and therefore, when the processing method in the application is adopted for processing, the strength of the produced POY pre-network filaments is low, and the filament breakage phenomenon is easy to occur, which are caused by the insufficient preheating treatment time.
In the present application, by adding microcrystalline wax and microcrystalline cellulose. The microcrystalline cellulose has more polar groups on the surface, can form a relatively orderly arrangement structure in a system, and simultaneously the polar groups on the surface can generate a certain dipole adsorption effect with polyester molecules, so that the crystallization process of the polyester molecules is promoted. The microcrystalline wax has a lower melting point and a stronger molecular chain flexibility, so that the microcrystalline wax can form a winding structure with microcrystalline cellulose and terylene molecules, the strength of the prepared POY pre-network filament is improved, and the materials have better flexibility in the reaction process. The compatibilizer in the above system allows the components to be more uniformly mixed together after melting.
Further, example 1 and examples 5 to 16 were compared and test 1 and test 2 were performed, and the specific test results are shown in table 4.
Table 4, example 1 and examples 5 to 16 of the experimental results
| Examples | Breaking strength (cN/dtex) | Number of filament breakage |
| Example 1 | 2.05 | 3 |
| Example 5 | 2.16 | 0 |
| Example 6 | 2.18 | 0 |
| Example 7 | 2.18 | 0 |
| Example 8 | 2.04 | 4 |
| Example 9 | 2.02 | 4 |
| Example 10 | 2.23 | 3 |
| Example 11 | 2.22 | 2 |
| Example 12 | 2.20 | 3 |
| Example 13 | 2.17 | 2 |
| Example 14 | 2.16 | 1 |
| Example 15 | 2.28 | 1 |
| Example 16 | 2.36 | 0 |
In the above examples, different effects are achieved by adding different components additionally to the system. In examples 5-7, trifluoroacetic acid and polyethylene glycol are added, and the combination of the trifluoroacetic acid and the polyethylene glycol can reduce the pores generated in the extrusion process of the second blending system, so that the strength of the protofilament and the POY pre-network filament is enhanced, and the occurrence of filament breakage is reduced. The principle of the method may be that, on one hand, polyethylene glycol and trifluoroacetic acid can form a cross-linked structure, in the process of temperature change, a pore structure generated due to temperature change in a filling system is enabled, meanwhile, trifluoroacetic acid has certain reactivity and can react with microcrystalline cellulose and terminal groups of polyethylene glycol, and a larger steric hindrance group can be generated in the reaction process, so that air is limited from entering. The overall result is a further increase in the strength of the processed fiber. Examples 8 and 9 demonstrate that both polyethylene glycol and trifluoroacetic acid are indispensable.
Castor oil is added in the embodiment 10-12, the castor oil has better lubricating effect and softening effect on the one hand, and further promotes better mixing among all components, and on the other hand, the castor oil can enhance cohesive force and further improve the strength of the POY pre-network filaments. In examples 13 to 15, acrylic acid was added so that acrylic acid could undergo a copolymerization reaction at a high temperature to some extent, and the branched chain thereof contained a large amount of carboxyl groups, which contributed to the formation of a more stable crosslinked structure in the second mixed system, and had the effect of improving the strength of the pre-network POY filaments. In example 16, polyethylene glycol, trifluoroacetic acid, castor oil and acrylic acid were added together, and the overall strength was the strongest.
Further, experiments 1 and 2 were performed on examples 17 to 31, and compared with example 16, and specific results are shown in table 5.
Table 5 and Experimental results of examples 16 to 31
| Examples | Breaking strength (cN/dtex) | Number of filament breakage | Examples | Breaking strength (cN/dtex) | Number of filament breakage |
| Example 16 | 2.36 | 0 | Example 24 | 2.67 | 0 |
| Example 17 | 2.35 | 0 | Example 25 | 2.72 | 0 |
| Example 18 | 2.38 | 0 | Example 26 | 2.59 | 0 |
| Example 19 | 2.25 | 2 | Example 27 | 2.48 | 0 |
| Example 20 | 2.17 | 1 | Example 28 | 2.34 | 3 |
| Example 21 | 2.22 | 2 | Example 29 | 2.20 | 2 |
| Example 22 | 2.67 | 0 | Example 30 | 2.42 | 3 |
| Example 23 | 2.65 | 0 | Example 31 | 2.39 | 1 |
In examples 17 to 21, the components of the compatibilizer were adjusted, and it can be seen from the above data that the compound system of maleic anhydride, polybutylene terephthalate, and maleic anhydride graft-modified polyethylene has better compatibility, and thus contributes to higher overall uniformity of the second blend system.
In examples 22 to 24, the cooling was performed by dry air in steps S1-2 and S1-4, which can improve the heat dissipation efficiency and rapidly complete the cooling of the system, so that the system can maintain the cross-linked structure in a hot state, and the final processed limit strength is higher. In addition, in example 25, dry nitrogen gas was further used instead of dry air, reducing the possibility of oxidation of the system, thereby further improving the strength and weather resistance of the fiber.
In example 26, acrylic acid was added in step S1-1, and the acrylic acid was previously polymerized, so that the stirring was not uniform enough in step S1, and the dispersibility between different materials was poor, thereby decreasing the strength of the processed POY pre-network filaments. In example 27, microcrystalline cellulose was added in step S1-1, and the microcrystalline cellulose was liable to absorb water and agglomerate, so that the moisture in the polyester chips could not be sufficiently absorbed, and the overall distribution was not uniform. In example 28, the addition of polyethylene glycol and trifluoroacetic acid in step S1-1 results in the crosslinking between the surface of the polyester fiber and polyethylene glycol, which in turn results in the formation of a network-like crosslinked structure in the chain structure of the polyester polymer, which reduces the fluidity and compatibility of the system, thereby affecting the properties of the subsequent processing. In example 30, the strength of the obtained POY pre-network filaments was reduced by heating once without cooling, and in example 31, the strength was reduced by gradually increasing the temperature without cooling.
In summary, the present application provides a POY pre-network filament, which requires a short preheating time in the production process, and is helpful to greatly reduce the production cost of enterprises and save energy.
The present embodiment is only for explaining the present application, and it is not limited to the present application, and those skilled in the art can make modifications of the present embodiment without inventive contribution as needed after reading the present specification, but all of them are protected by patent law within the scope of the claims of the present application.
Claims (9)
1. The POY pre-network filament is characterized by comprising the following raw materials in parts by mass:
polyester slicing: 130-160 parts;
microcrystalline wax: 25-40 parts;
a compatilizer: 10-20 parts;
microcrystalline cellulose: 2-7 parts;
the POY pre-network filament is obtained through the steps of preheating, melt extrusion, oiling, cooling, drafting, shaping, networking and winding.
2. A POY pre-network filament according to claim 1, wherein: the compatilizer is maleic anhydride, polybutylene terephthalate and maleic anhydride grafted modified polyethylene, wherein the mass ratio of the maleic anhydride to the polybutylene terephthalate to the maleic anhydride grafted modified polyethylene is 1 (0.3-0.6) to 1.2-4.
3. A POY pre-network filament according to claim 1, wherein: the raw materials of the POY pre-network filament further comprise 1.5-2.4 parts by mass of polyethylene glycol and 0.8-1.3 parts by mass of trifluoroacetic acid.
4. A POY pre-network filament according to claim 1, wherein: the raw material of the POY pre-networking filament also comprises 7-15 parts by mass of castor oil.
5. A POY pre-network filament according to claim 1, wherein: the raw material of the POY pre-network filament further comprises 6-12 parts by mass of acrylic acid.
6. A process for producing a POY pre-networked filament according to any of claims 1 to 5, comprising the steps of:
s1, preheating polyester chips, microcrystalline wax, microcrystalline cellulose, castor oil and acrylic acid to obtain a first mixed system, wherein the preheating temperature is 150-215 ℃, and the preheating time is 145-210 min;
s2, adding a compatilizer into the first blending system, heating to 144-150 ℃, and continuously and uniformly mixing to obtain a second blending system;
s3, heating the second blending system to be molten, adding a pore eliminating agent, continuously mixing for 5-10 min, and performing spinning treatment to obtain precursor;
and S4, cooling the protofilament obtained in the step S3, oiling, drafting and heat setting, pre-networking, winding and forming to obtain the POY pre-networking filament.
7. The process of claim 6, wherein in step S1, the pre-heating treatment is performed by the following steps:
s1-1, mixing the polyester chips, the microcrystalline wax and the castor oil, heating to 153-158 ℃, stirring, and keeping for 40-50 min;
s1-2, after the step S1-1 is finished, introducing dry gas with the temperature of-20 to 0 ℃ into the system, wherein the introduction speed of the gas corresponding to each kilogram of polyester chips is 0.1 to 0.4m3The ventilation time is 15-25 min;
s1-3, after the step S1-2 is finished, adding microcrystalline cellulose into the system, heating the system to 162-166 ℃ again, and continuing to keep the temperature and mix for 60-80 min;
s1-4, after the step S1-3 is finished, introducing dry gas with the temperature of-20 to 0 ℃ into the system, wherein the introduction speed of the gas corresponding to each kilogram of polyester chips is 0.1 to 0.4m3The ventilation time is 10-15 min;
s1-5, after the step S1-4 is finished, putting acrylic acid into the system, heating the system to 206-215 ℃ again, and continuing to mix for 30-40 min in a heat preservation mode;
s1-6, cooling the system to 20-30 ℃ under the condition of keeping dry.
8. The POY pre-networking filament processing process of claim 7, wherein the introduced dry gas is nitrogen in steps S1-2 and S1-4.
9. A POY pre-networking filament processing process according to claim 6, wherein: in step S3, a double-screw extruder is used for spinning, and the temperature of an extrusion head is 318-324 ℃.
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