CN114350141A - PHA master batch for polyamide-6 fiber and preparation method thereof - Google Patents
PHA master batch for polyamide-6 fiber and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of preparation and application of functional master batch materials, and particularly discloses PHA master batch for nylon-6 fiber, wherein the formula of the PHA master batch for the nylon-6 fiber is as follows in percentage by mass: 78-89% of spinning-grade chinlon 6 chips, 10-20% of PHA powder and 1-2% of a dispersing agent; the gloss of the spinning-grade nylon-6 slice is glossy or semi-dull; the relative viscosity of the spinning-grade nylon-6 chip is 2.47-2.50; the dispersing agent is an amide high-molecular polymer.
Description
Technical Field
The invention particularly relates to PHA master batch for nylon-6 fiber and a preparation method thereof, belonging to the technical field of functional master batch materials.
Background
The chinlon 6 civil filament fiber is one of main raw materials of textiles, the difference of the chinlon 6 civil fiber is the development trend with the highest added value in a textile industry chain, and according to statistics, the product difference rate is increased from 55% to 61% from 2012 to 2016, and the ratio of the functional chinlon 6 civil fiber is increased. With the great advance of the green development of the industry, the green and environment-friendly industry is actively developed, the development of the bio-based material is mainly based on the comprehensive utilization of biomass resources and the manufacture of high-performance bio-based chemicals, the key core technology attacks such as biotransformation, chemical transformation and composite forming in the manufacturing process of the bio-based chemicals are enhanced, the advanced green advanced manufacturing technology at the front edge of the bio-based material is deployed, the high-valued basic research of the bio-based material is stably supported, the multi-element synchronous development such as the innovation and development platform of the scientific and technological industry is constructed, and the method is an important attack and hardening direction for supporting and promoting the novel energy-saving and environment-friendly technology and the efficient and economical utilization of resources. Under the background, the research of the bio-based nylon 6 civil filament fiber is promoted, and becomes one of the key development directions of the current nylon 6 civil filament differentiated fiber industry.
In recent years, bio-based materials represented by polylactic acid (PLA) and Polyhydroxyalkanoate (PHA) are becoming hot spots in the fiber industry due to their characteristics of green, environment-friendly, resource-saving, and the like. The PLA/PHA fiber has similar performance to general fiber, but also has the advantages of biodegradation, bacteriostasis, better ultraviolet resistance, certain flame retardance, barrier property and the like, and the produced synthetic silk can replace natural silk, is positioned in green, functional and high-added-value products, and can be applied to the fields of high-end textiles, infant products, hygienic products, medical care consumables and the like. Chinese patent with application number CN202010431722.8 discloses a PLA/PHA fiber and a device and a method for preparing the PLA/PHA fiber on line, wherein a polylactic acid melt obtained by PLA through a polylactic acid polymerization device is specifically disclosed, and then the polylactic acid melt and PHA are mixed to obtain a PLA/PHA polymerization melt, and the PLA/PHA polymerization melt is spun in a spinning device; chinese patent CN201610326575.1, application No. CN201610326575.1, discloses the application of PHA as a novel natural antibacterial material in textile preparation, specifically that pure PHA or a mixture of PHA polymer and other polymers or copolymers is injected into an extrusion device with a heating device for melting, fibers are collected at 170-225 ℃ and 300-3000 m/min, and FDY long fibers are prepared according to a draft ratio of 2-4 or short fibers are prepared according to a conventional short fiber process; in the above patents, PHA is directly used for melt spinning, which results in poor spinnability, specifically in severe plate sticking phenomenon and severe filament breaking phenomenon, and finally results in low filament forming rate and poor product quality.
Disclosure of Invention
In order to solve the problems in the prior art, the invention provides the PHA master batch for the nylon-6 fiber and the preparation method thereof, the prepared PHA master batch can show excellent spinning condition performance, has good antibacterial performance, and provides a new material selection for the production of bio-based nylon-6 domestic filament fibers.
The technical scheme of the invention is as follows:
the PHA master batch for the nylon-6 fiber comprises the following components in percentage by mass: 78-89% of spinning-grade nylon-6 chips, 10-20% of PHA powder and 1-2% of dispersing agent.
Further, the luster of the spinning-grade nylon-6 chip is glossy or semi-dull; the relative viscosity of the spinning-grade nylon-6 chip is 2.47-2.50.
Further, the dispersing agent is an amide high-molecular polymer.
The invention also provides a preparation method of the PHA master batch for the nylon-6 fiber, which comprises the following steps: quantitative raw material feeding, melt plasticizing, screw shearing, water cooling and grain cutting, vibration screening and vacuum drying, and finally obtaining the PHA master batch with the water content of 300-500ppm, the melt index of 71.8-74.6g/10min and the relative viscosity of 2.13-2.35.
Further, the quantitative raw material feeding is realized in a mode of linkage feeding through a main feeding position and a side feeding position: spinning grade nylon 6 chips are added at the main feeding position, and a dispersing agent is added at the side feeding position; controlling the feeding speed of the main feeding position and the side feeding position to be 15-25 Hz.
Further, the temperature of each temperature zone of the melting and plasticizing is controlled as follows: the temperature of the first temperature zone is 210 ℃; the temperature of the second temperature zone is 220 ℃; the temperature of the third temperature zone is 225 ℃; the temperature of the fourth-section temperature zone is 215-225 ℃; the temperature of the fifth-stage temperature zone is 205-215 ℃; the temperature of the sixth section temperature zone is 200-210 ℃; the temperature of the seventh section, the eighth section and the ninth section is 180-; the temperature of the temperature zone of the machine head is 230-240 ℃.
Further, the rotating speed of the host machine for shearing the screw rod is 500-550 r/min; the rotating speed of the main machine of the granulator for water-cooling granulation is 850-950 r/min.
Further, the diameter of the screen mesh of the vibration screening is 2-8 mm.
The invention also provides nylon-6 fiber which is prepared by melt spinning at least one master batch, wherein the at least one master batch comprises the PHA master batch for the nylon-6 fiber.
Compared with the prior art, the invention has the beneficial effects that:
1. the PHA master batch for the nylon-6 fiber provided by the invention shows excellent spinning condition performance, can provide a new material selection for the continuous production of bio-based nylon-6 domestic filament fibers, and the specific spinning condition performance is described in specific examples.
2. In the invention, PHA is used as a raw material to prepare functional master batches, and the master batches are applied to spinning, so that the spinnability of the master batches can be greatly improved, the problem of plate sticking is effectively solved, and the phenomenon of filament breaking in the spinning process is reduced; in the process of preparing master batches, PHA with low polymerization degree can be reduced through the shearing action of the twin screw, so that the excellent antibacterial performance is achieved, cell membranes of microorganisms can be damaged, acid-base balance can be changed after the PHA enters cells, metabolism is disturbed, and the PHA is killed.
Reference numerals
FIG. 1 is a pictorial view of a PHA masterbatch made in accordance with example 1;
FIG. 2 is a diagram of a bio-based nylon-6 staple fiber produced from PHA masterbatch prepared according to example 1;
FIG. 3 is a diagram of the bio-based nylon-6 civil filament fiber produced from the PHA masterbatch prepared in example 1 after being bulked.
Detailed Description
The invention is further described with reference to the drawings and the preferred embodiments, and the endpoints of the ranges and any values disclosed in the present invention are not limited to the precise range or value, and should be understood to encompass values close to these ranges or values; for ranges of values, between the endpoints of each of the ranges and the individual points, and between the individual points may be combined with each other to give one or more new ranges of values, and these ranges of values should be considered as specifically disclosed herein.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified;
the experimental procedures in the following examples are conventional unless otherwise specified.
The master batch hundred-grain weight analysis of the invention adopts an electronic balance of ME104E model purchased from Mettler-Torledo instruments (Shanghai) Co., Ltd to carry out the test;
the master batch water content analysis is carried out by adopting a model 860KF Thermoprep Karman sample heating processor purchased from Switzerland Wantong (Metrohm) China Limited company;
the melt index analysis of the master batches was carried out using a melt flow rate tester model ZRZ1452 from Meits Industrial systems (China) Ltd;
the master batch relative viscosity analysis is tested by adopting a viscometer of PV60AVS600 model purchased from Shanghai Lu & instruments Co., Ltd;
the fiber fineness was tested using a yarn length measuring machine available from the firm YG086 model of Fukushi textile Instrument, Inc., Changzhou;
the fiber breaking strength was tested using a fully automatic single yarn strength tester model YG023B available from Fungis textile instruments Inc., of Babearing, Changzhou;
the fiber elongation at break was tested using a fully automatic single yarn strength tester model YG023B available from eight-Fang Leishi textile instruments Inc., Changzhou;
the fiber evenness was tested using a evenness tester model CFE400C from Suzhou Changfeng instruments Inc.;
the oil content of the fibers was measured using an oil analyzer model MQC from shanghai unicon instruments ltd;
the boiling water shrinkage of the fibers was measured using a fully automatic crimper model YG368 available from Fuji textile instruments Inc., of Oershire, Changzhou;
the fiber network was tested using a standard light box plus water bath, model Cac-1200L (YG60), available from eight-direction Leisha textile instruments, Inc., of Changzhou;
the fiber cake hardness was measured using a hardness tester model HP-5 from SCHMIDT, Germany.
Example 1
The PHA master batch for the nylon-6 fiber comprises the following components in percentage by mass: 89% of spinning grade bright chinlon 6 slices (in a granular shape, the grain diameter is 2-3mm, and the grain diameter is purchased from Fujian Yongrong Jinjiang, the same below), 10% of PHA powder (purchased from Nanjing Heyu chemical Co., Ltd, the same below), and 1% of dispersing agent powder are amide high-molecular polymers (the optimized chemical JHX-200 is purchased from the optimized chemical Co., Ltd, the same below).
The preparation method of the PHA master batch comprises the following steps:
(1) adding spinning-grade bright chinlon 6 slices into a main feeding position of a parallel co-rotating twin-screw extrusion granulator through a weightlessness scale, and controlling the feeding rotating speed of the main feeding position to be 25 Hz;
(2) adding PHA powder into a side feeding position of a parallel co-rotating twin-screw extrusion granulator through a weightlessness scale, and controlling the feeding rotating speed of the side feeding position to be 25 Hz;
(3) melting and plasticizing, and controlling the temperature of each temperature zone as follows: the temperature of the first temperature zone is 210 ℃; the temperature of the second temperature zone is 220 ℃; the temperature of the third temperature zone is 225 ℃; the temperature of the fourth temperature zone is 215 ℃; the temperature of the fifth temperature zone is 205 ℃; the temperature of the sixth temperature zone is 200 ℃; the temperature of the seventh, eighth and ninth temperature zones is 180 ℃; the temperature of a machine head temperature area is 230 ℃;
(4) sequentially carrying out screw shearing, water-cooling granulation, vibrating screen and vacuum drying after melting and plasticizing, and further preparing PHA master batch (the details are shown in figure 1, and physical property parameters are shown in attached table 1); wherein the rotating speed of a main machine for screw shearing is 550r/min, the rotating speed of a main machine for a granulator is 890r/min, and the diameter of a screen mesh is 2-6 mm.
Example 2
The PHA master batch for the nylon-6 fiber comprises the following components in percentage by mass: the spinning grade bright chinlon 6 slice is 86.25 percent, the PHA powder is 12.5 percent, and the dispersant powder is 1.25 percent, which is optimized chemical JHX-200 powder.
The preparation method of the PHA master batch comprises the following steps:
(1) adding spinning-grade bright chinlon 6 slices into a main feeding position of a parallel co-rotating twin-screw extrusion granulator through a weightlessness scale, and controlling the feeding rotating speed of the main feeding position to be 20 Hz;
(2) adding PHA powder into a side feeding position of a parallel co-rotating twin-screw extrusion granulator through a weightlessness scale, and controlling the feeding rotating speed of the side feeding position to be 20 Hz;
(3) melting and plasticizing, and controlling the temperature of each temperature zone as follows: the temperature of the first temperature zone is 210 ℃; the temperature of the second temperature zone is 220 ℃; the temperature of the third temperature zone is 225 ℃; the temperature of the fourth temperature zone is 220 ℃; the temperature of the fifth temperature zone is 215 ℃; the temperature of the sixth temperature zone is 210 ℃; the temperature of the seventh, eighth and ninth temperature zones is 200 ℃; the temperature of a nose temperature zone is 240 ℃;
(4) sequentially carrying out the processes of screw shearing, water-cooling granulation, vibrating screen and vacuum drying after melting and plasticizing, and further preparing PHA master batches (physical property parameters are shown in the attached table 1); wherein the rotating speed of a main machine for screw shearing is 500r/min, the rotating speed of a main machine for a granulator is 950r/min, and the diameter of a screen mesh is 6-8 mm.
Example 3
The PHA master batch for the nylon-6 fiber comprises the following components in percentage by mass: the spinning grade bright chinlon 6 slice is 83.5 percent, the PHA powder is 15 percent, and the dispersant powder is 1.5 percent, which is optimized chemical JHX-200 powder.
The preparation method of the PHA master batch comprises the following steps:
(1) adding spinning-grade bright chinlon 6 slices into a main feeding position of a parallel co-rotating twin-screw extrusion granulator through a weightlessness scale, and controlling the feeding rotating speed of the main feeding position to be 22 Hz;
(2) adding PHA powder into a side feeding position of a parallel co-rotating twin-screw extrusion granulator through a weightlessness scale, and controlling the feeding rotating speed of the side feeding position to be 22 Hz;
(3) melting and plasticizing, and controlling the temperature of each temperature zone as follows: the temperature of the first temperature zone is 210 ℃; the temperature of the second temperature zone is 220 ℃; the temperature of the third temperature zone is 225 ℃; the temperature of the fourth temperature zone is 225 ℃; the temperature of the fifth temperature zone is 210 ℃; the temperature of the sixth temperature zone is 205 ℃; the temperature of the seventh, eighth and ninth temperature zones is 195 ℃; the temperature of a machine head temperature area is 235 ℃;
(4) sequentially carrying out the processes of screw shearing, water-cooling granulation, vibrating screen and vacuum drying after melting and plasticizing, and further preparing PHA master batches (physical property parameters are shown in the attached table 1); wherein the rotating speed of a main machine for screw shearing is 530r/min, the rotating speed of a main machine for a granulator is 850r/min, and the diameter of a screen mesh is 4-6 mm.
Example 4
The PHA master batch for the nylon-6 fiber comprises the following components in percentage by mass: 80.75% of spinning-grade semi-dull chinlon 6 chips, 17.5% of PHA powder and 1.75% of dispersing agent powder are optimized chemical JHX-200 powder.
The preparation method of the PHA master batch comprises the following steps:
(1) adding spinning-grade semi-dull nylon 6 slices into a main feeding position of a parallel co-rotating twin-screw extrusion granulator through a weightlessness scale, and controlling the feeding rotating speed of the main feeding position to be 25 Hz;
(2) adding PHA powder into a side feeding position of a parallel co-rotating twin-screw extrusion granulator through a weightlessness scale, and controlling the feeding rotating speed of the side feeding position to be 25 Hz;
(3) melting and plasticizing, and controlling the temperature of each temperature zone as follows: the temperature of the first temperature zone is 210 ℃; the temperature of the second temperature zone is 220 ℃; the temperature of the third temperature zone is 225 ℃; the temperature of the fourth temperature zone is 225 ℃; the temperature of the fifth temperature zone is 205 ℃; the temperature of the sixth temperature zone is 200 ℃; the temperature of the seventh, eighth and ninth temperature zones is 190 ℃; the temperature of a machine head temperature area is 235 ℃;
(4) sequentially carrying out the processes of screw shearing, water-cooling granulation, vibrating screen and vacuum drying after melting and plasticizing, and further preparing PHA master batches (physical property parameters are shown in the attached table 1); wherein the rotating speed of the main machine for screw shearing is 520r/min, the rotating speed of the main machine for the granulator is 900r/min, and the diameter of the screen mesh is 6-8 mm.
Example 5
The PHA master batch for the nylon-6 fiber comprises the following components in percentage by mass: 78% of spinning-grade semi-dull chinlon 6 chips, 20% of PHA powder and 2% of dispersing agent powder are optimized chemical JHX-200 powder.
The preparation method of the PHA master batch comprises the following steps:
(1) adding spinning-grade semi-dull nylon 6 slices into a main feeding position of a parallel co-rotating twin-screw extrusion granulator through a weightlessness scale, and controlling the feeding rotating speed of the main feeding position to be 23 Hz;
(2) adding PHA powder into a side feeding position of a parallel co-rotating twin-screw extrusion granulator through a weightlessness scale, and controlling the feeding rotating speed of the side feeding position to be 23 Hz;
(3) melting and plasticizing, and controlling the temperature of each temperature zone as follows: the temperature of the first temperature zone is 210 ℃; the temperature of the second temperature zone is 220 ℃; the temperature of the third temperature zone is 225 ℃; the temperature of the fourth temperature zone is 220 ℃; the temperature of the fifth temperature zone is 210 ℃; the temperature of the sixth temperature zone is 205 ℃; the temperature of the seventh, eighth and ninth temperature zones is 200 ℃; the temperature of a nose temperature zone is 240 ℃;
(4) sequentially carrying out the processes of screw shearing, water-cooling granulation, vibrating screen and vacuum drying after melting and plasticizing, and further preparing PHA master batches (physical property parameters are shown in the attached table 1); wherein the rotating speed of a main machine for screw shearing is 550r/min, the rotating speed of a main machine for a granulator is 920r/min, and the diameter of a screen mesh is 2-4 mm.
The physical parameters of the PHA master batch for the nylon 6 fiber prepared in the above examples 1-5 are shown in Table 1, the PHA master batch for the nylon 6 fiber prepared in the above examples 1-5 is used for direct spinning nylon 6 civil filament fiber (specification: POY FD 25D/24F), and the addition ratio of the master batch in each example is shown in Table 2; FIG. 2 is a drawing of a physical property of the bio-based nylon-6 staple fiber produced from the PHA masterbatch obtained in example 1, and Table 3 shows the physical property indexes of the bio-based nylon-6 staple fiber produced from the PHA masterbatch obtained in examples 1 to 5 of the present invention; FIG. 3 is a drawing of the physical fiber after the texturing of the bio-based nylon-6 civil filament fiber produced from the PHA masterbatch obtained in example 1 (DTY FD 20D/24F), and tables 4 and 5 are the physical index of the fiber after the texturing of the bio-based nylon-6 civil filament fiber produced from the PHA masterbatch obtained in examples 1 to 5 of the present invention; the antimicrobial data for producing civilian filament fibers from the PHA masterbatch made in example 1 are shown in table 6; as can be seen from the attached drawings and tables, the PHA master batch for the nylon 6 fiber prepared by the invention has excellent performance in the nylon 6 domestic filament fiber, and can provide a new material selection for the continuous production of the bio-based nylon 6 domestic filament fiber.
TABLE 1 PHA master batch physical property parameters for nylon-6 fiber
TABLE 2 addition ratio of master batch in nylon-6 civil filament fiber
| Serial number | Addition ratio of mother particle (%) |
| Example 1 | 10.0 |
| Example 2 | 8.0 |
| Example 3 | 6.7 |
| Example 4 | 5.7 |
| Example 5 | 5.0 |
TABLE 3 physical Properties of the bio-based Chinlon 6 civil filament fiber
TABLE 4 Limit physical index of bio-based chinlon 6 civil filament fiber after texturing
TABLE 5 Limit physical index of bio-based chinlon 6 civil filament fiber after texturing
TABLE 6 antibacterial index of civil filament prepared from PHA master batch in example 1
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (9)
1. The PHA master batch for the nylon-6 fiber comprises the following components in percentage by mass: 78-89% of spinning-grade nylon-6 chips, 10-20% of PHA powder and 1-2% of dispersing agent.
2. The PHA master batch for nylon 6 fiber as claimed in claim 1, wherein: the gloss of the spinning-grade nylon-6 slice is glossy or semi-dull; the relative viscosity of the spinning-grade nylon-6 chip is 2.47-2.50.
3. The PHA master batch for nylon 6 fiber as claimed in claim 1, wherein: the dispersing agent is an amide high-molecular polymer.
4. The preparation method of the PHA master batch for the polyamide-6 fiber is characterized by comprising the following steps: quantitative raw material feeding, melt plasticizing, screw shearing, water cooling and grain cutting, vibration screening and vacuum drying, and finally obtaining the PHA master batch with the water content of 300-500ppm, the melt index of 71.8-74.6g/10min and the relative viscosity of 2.13-2.35.
5. The method for preparing PHA master batch for nylon-6 fiber according to claim 4, wherein the PHA master batch comprises the following steps: the quantitative raw material feeding is realized in a mode of linkage feeding through a main feeding position and a side feeding position: spinning grade nylon 6 chips are added at the main feeding position, and a dispersing agent is added at the side feeding position; controlling the feeding speed of the main feeding position and the side feeding position to be 15-25 Hz.
6. The method for preparing PHA master batch for nylon-6 fiber according to claim 4, wherein the PHA master batch comprises the following steps: the temperature of each temperature zone of the melting plasticization is controlled as follows: the temperature of the first temperature zone is 210 ℃; the temperature of the second temperature zone is 220 ℃; the temperature of the third temperature zone is 225 ℃; the temperature of the fourth-section temperature zone is 215-225 ℃; the temperature of the fifth-stage temperature zone is 205-215 ℃; the temperature of the sixth section temperature zone is 200-210 ℃; the temperature of the seventh section, the eighth section and the ninth section is 180-; the temperature of the temperature zone of the machine head is 230-240 ℃.
7. The method for preparing PHA master batch for nylon-6 fiber according to claim 4, wherein the PHA master batch comprises the following steps: the rotating speed of a host machine for shearing the screw rod is 500-550 r/min; the rotating speed of the main machine of the granulator for water-cooling granulation is 850-950 r/min.
8. The method for preparing PHA master batch for nylon-6 fiber according to claim 4, wherein the PHA master batch comprises the following steps: the diameter of the screen mesh of the vibration screening is 2-8 mm.
9. A nylon-6 fiber prepared by melt spinning at least one masterbatch, wherein the at least one masterbatch comprises the PHA masterbatch for nylon-6 fiber of any one of claims 1 to 3.
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| CN116024697A (en) * | 2023-01-16 | 2023-04-28 | 广东新会美达锦纶股份有限公司 | Degradable fiber and preparation method and application thereof |
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