CN114350141B - PHA master batch for nylon 6 fiber and preparation method thereof - Google Patents
PHA master batch for nylon 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 masterbatch materials, and in particular discloses a PHA masterbatch for nylon 6 fibers, which comprises the following components in percentage by mass: 78% -89% of spinning-grade chinlon 6 slices, 10% -20% of PHA powder and 1% -2% of dispersing agent; the luster of the spinning-grade chinlon 6 slices is bright or semi-dull; the relative viscosity of the spinning-grade chinlon 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 (polyhydroxyalkanoate) master batch for nylon 6 fibers and a preparation method thereof, and belongs to the technical field of functional master batch materials.
Background
The nylon 6 civil filament fiber is one of the main raw materials of the textile, the nylon 6 civil fiber differentiation is the development trend of the highest added value in the textile industry chain, and according to statistics, the product differentiation rate from 2012 to 2016 is increased from 55% to 61%, and the duty ratio of the functional nylon 6 civil fiber is in an increasing trend. Along with the strong promotion of the green development of industry, the green environment-friendly industry is actively developed, the development of the bio-based material focuses on comprehensive utilization of biomass resources and production of high-performance bio-based chemicals, the key technical aspects of biotransformation, chemical transformation, composite molding and the like in the manufacturing process of the bio-based chemicals are enhanced, the advanced manufacturing technology of the bio-based material is advanced, the basic research of the high-valued bio-based material is stably supported, the multi-element synchronous development of a technological industry innovation development platform and the like is constructed, and the multi-element synchronous development of supporting and promoting novel energy-saving environment-friendly technology and efficient resource conservation and utilization is important. Under the background, the research of the biobased nylon 6 civil filament fiber is raised to become one of the key development directions of the current nylon 6 civil filament differential fiber industry.
In recent years, biobased materials represented by polylactic acid (PLA) and Polyhydroxyalkanoate (PHA) are becoming hot spots in the fiber industry due to their characteristics of green, environmental friendliness, resource saving, and the like. The PLA/PHA fiber has similar performance to the common fiber, but also has the advantages of biodegradation, bacteriostasis, good 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, baby products, sanitary products, medical care consumables and the like. The Chinese patent with the application number of CN202010431722.8 discloses a PLA/PHA fiber and a device and a method for preparing the PLA/PHA fiber on line, wherein the method specifically discloses a polylactic acid melt obtained by using PLA through a polylactic acid polymerization device, and then the polylactic acid melt is mixed with PHA to obtain a PLA/PHA polymerization melt, and the PLA/PHA polymerization melt is spun in a spinning device; the Chinese patent with application number of CN201610326575.1 discloses that pure PHA or the mixture of PHA polymer and other polymer or copolymer is injected into extrusion equipment with a heating device to be melted, and the fiber is collected at 170-225 ℃ and 300-3000 m/min, and made into FDY long fiber according to the draft ratio of 2-4 or made into short fiber according to the conventional short fiber process; in the above patent, PHA is directly used for melt spinning, which results in poor spinnability, serious plate sticking phenomenon, serious filament floating phenomenon, 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, and the prepared PHA master batch can show excellent spinning condition performance and has good antibacterial performance, thereby providing a new material selection for the production of the bio-based nylon 6 civil filament fiber.
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 chinlon 6 slices, 10-20% of PHA powder and 1-2% of dispersing agent.
Further, the luster of the spinning-grade chinlon 6 slices is bright or semi-dull; the relative viscosity of the spinning-grade chinlon 6 chip is 2.47-2.50.
Further, the dispersing agent is an amide polymer.
The invention also provides a preparation method of the PHA master batch for the nylon 6 fiber, which specifically comprises the following steps: the PHA master batch is finally prepared by the steps of quantitative feeding of raw materials, melt plasticization, screw shearing, water cooling granulation, vibration screening and vacuum drying, and has 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 by a mode of linkage feeding of a main feeding position and a side feeding position: the main feeding position is added with spinning-grade nylon 6 slices, and the side feeding position is added with dispersing agent; the feeding rotational speed of the main feeding level and the side feeding level is controlled to be 15-25Hz.
Further, the temperature of each section of temperature zone of the melting plasticization is controlled as follows: the temperature of the first-stage temperature zone is 210 ℃; the temperature of the second-stage temperature zone is 220 ℃; the temperature of the third-stage temperature zone is 225 ℃; the temperature of the fourth temperature zone is 215-225 ℃; the temperature of the fifth temperature zone is 205-215 ℃; the temperature of the sixth temperature zone is 200-210 ℃; the temperature of the seventh section, the eighth section and the ninth section is 180-200 ℃; the temperature of the temperature zone of the machine head is 230-240 ℃.
Further, the rotation speed of the main machine for shearing the screw is 500-550r/min; the main machine rotating speed of the water-cooling granulating machine is 850-950r/min.
Further, the diameter of the screen holes of the vibration screening is 2-8mm.
The invention also provides a nylon 6 fiber which is prepared from at least one master batch through melt spinning, 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 has excellent spinning condition performance, and can provide a new material selection for continuous production of the bio-based nylon 6 civil filament fiber, and the specific spinning condition performance is described in specific examples.
2. The PHA is used as a raw material to prepare the functional master batch, and the master batch is applied to spinning, so that the spinnability of the master batch can be greatly improved, the problem of sticking plates is effectively solved, and the phenomenon of yarn floating and breaking in the spinning process is reduced; in the process of preparing the master batch, through the shearing action of the double screws, the polymerization degree of PHA can be reduced, PHA with low polymerization degree has excellent antibacterial performance, can destroy cell membranes of microorganisms, can change acid-base balance in cells, disturb metabolism and kill the cells, and meanwhile, PHA is added into the master batch and is not easy to change color due to sweat stain in the use process like other inorganic antibacterial agents (such as silver, copper and zinc), so that the yarn is easy to have chromatic aberration in the subsequent processing.
Reference numerals
FIG. 1 is a pictorial view of PHA master batches prepared according to example 1;
FIG. 2 is a pictorial view of biobased nylon 6 household filament fiber produced from PHA concentrate produced in accordance with example 1;
FIG. 3 is a pictorial view of a biobased nylon 6 civil filament fiber produced from PHA concentrate produced in accordance with example 1 after texturing.
Detailed Description
The invention is further described below with reference to the drawings and the preferred embodiments, and the endpoints and any values of the ranges disclosed in the invention are not limited to the precise range or value, and the range or value should be understood to include the value near the range or value; for numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and are to be considered as specifically disclosed herein.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified;
the experimental methods in the following examples are conventional methods unless otherwise specified.
The master batch hundred-particle weight analysis in the invention adopts an electronic balance of ME104E model purchased from Metrele-Tolyduo instruments (Shanghai) limited to test;
the water content of the master batch is analyzed by adopting a Karsch sample heating processor of 860KF thermo prep model purchased from Metrohm China Co., ltd;
the melt index analysis of the master batch was performed using a melt flow rate tester model ZRZ1452 available from the Meter Industrial System (China) Co., ltd;
the relative viscosity of the master batch was measured using a viscometer model PV60AVS600 available from Shanghai Lu scientific instruments Co., ltd;
the fiber fineness was tested using a yarn length measuring machine of model YG086 available from Alcalizer textile instruments, inc. of Hexacum;
the fiber breaking strength was tested using a full automatic single yarn strength tester available from YG023B model of Alrange textile instruments, inc. of Heng;
the elongation at break of the fiber was tested using a fully automatic single yarn tester model YG023B from Alrange textile instruments, inc. of Heng;
the fiber stem unevenness was tested using a stem tester of CFE400C model purchased from sostate gale instruments limited;
the fiber oil content is tested by an oil content analyzer of MQC model purchased from Shanghai Linn instruments Co., ltd;
the shrinkage of the fiber was measured using a fully automatic crimp instrument model YG368 from Alcalizer textile instruments, inc. of Heng;
the fiber network was tested using a standard light source box plus water bath from Cac-1200L (YG 60) model of Alcalizer textile instruments, inc. of Heng;
the hardness of the fiber cake was measured using a hardness tester of model HP-5 available from the company SCHMIDT, germany.
Example 1
The PHA master batch for the nylon 6 fiber comprises the following components in percentage by mass: spinning grade glossy nylon 6 chip 89% (granular, particle size 2-3mm, purchased from Fujian Yongrong Jinjiang Co., ltd., hereinafter the same), PHA powder 10% (purchased from Nanjing He chemical Co., ltd., hereinafter the same), dispersant powder 1% is amide polymer (optimization chemistry JHX-200 purchased from optimization chemistry Co., ltd., hereinafter the same).
The preparation method of the PHA master batch comprises the following steps:
(1) Adding the spinning-grade bright nylon 6 slices into a main feeding position of a parallel co-rotating double-screw extrusion granulator through weightlessness, and controlling the feeding rotating speed of the main feeding position to be 25Hz;
(2) Adding PHA powder into a side feeding position of a parallel co-rotating double-screw extrusion granulator through weightlessness, and controlling the feeding rotating speed of the side feeding position to be 25Hz;
(3) Melting and plasticizing, wherein the temperature of each section of temperature zone is controlled as follows: the temperature of the first-stage temperature zone is 210 ℃; the temperature of the second-stage temperature zone is 220 ℃; the temperature of the third-stage 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 temperatures of the seventh, eighth and ninth temperature zones are 180 ℃; the temperature of the machine head temperature zone is 230 ℃;
(4) Sequentially performing the procedures of screw shearing, water-cooling granulating, vibrating screen and vacuum drying after melting and plasticizing to obtain PHA master batches (see figure 1 for details and physical parameters in figure 1); wherein, the main machine rotating speed of the screw shearing is 550r/min, the main machine rotating speed of the granulator is 890r/min, and the diameter of the screen holes is 2-6mm.
Example 2
The PHA master batch for the nylon 6 fiber comprises the following components in percentage by mass: 86.25% of spinning-grade glossy nylon 6 slice, 12.5% of PHA powder and 1.25% of dispersing agent powder are optimization chemical JHX-200 powder.
The preparation method of the PHA master batch comprises the following steps:
(1) Adding the spinning-grade bright nylon 6 slices into a main feeding position of a parallel co-rotating double-screw extrusion granulator through weightlessness, and controlling the feeding rotating speed of the main feeding position to be 20Hz;
(2) Adding PHA powder into a side feeding position of a parallel co-rotating double-screw extrusion granulator through weightlessness, and controlling the feeding rotating speed of the side feeding position to be 20Hz;
(3) Melting and plasticizing, wherein the temperature of each section of temperature zone is controlled as follows: the temperature of the first-stage temperature zone is 210 ℃; the temperature of the second-stage temperature zone is 220 ℃; the temperature of the third-stage 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 temperatures of the seventh, eighth and ninth temperature zones are 200 ℃; the temperature of the machine head temperature zone is 240 ℃;
(4) Sequentially performing the procedures of screw shearing, water-cooling granulating, vibrating screen and vacuum drying after melting and plasticizing to further prepare PHA master batches (physical parameters are shown in the attached table 1); wherein, the main machine rotating speed of the screw shearing is 500r/min, the main machine rotating speed of the granulator is 950r/min, and the diameter of the screen holes is 6-8mm.
Example 3
The PHA master batch for the nylon 6 fiber comprises the following components in percentage by mass: 83.5% of spinning-grade lustrous nylon 6 chips, 15% of PHA powder and 1.5% of dispersing agent powder are optimization chemical JHX-200 powder.
The preparation method of the PHA master batch comprises the following steps:
(1) Adding the spinning-grade bright nylon 6 slices into a main feeding position of a parallel co-directional double-screw extrusion granulator through weightlessness, and controlling the feeding rotating speed of the main feeding position to be 22Hz;
(2) Adding PHA powder into a side feeding position of a parallel co-rotating double-screw extrusion granulator through weightlessness, and controlling the feeding rotating speed of the side feeding position to be 22Hz;
(3) Melting and plasticizing, wherein the temperature of each section of temperature zone is controlled as follows: the temperature of the first-stage temperature zone is 210 ℃; the temperature of the second-stage temperature zone is 220 ℃; the temperature of the third-stage 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 temperatures of the seventh, eighth and ninth temperature zones are 195 ℃; the temperature of the machine head temperature zone is 235 ℃;
(4) Sequentially performing the procedures of screw shearing, water-cooling granulating, vibrating screen and vacuum drying after melting and plasticizing to further prepare PHA master batches (physical parameters are shown in the attached table 1); wherein, the main machine rotating speed of the screw shearing is 530r/min, the main machine rotating speed of the granulator is 850r/min, and the diameter of the screen holes is 4-6mm.
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 nylon 6 slice, 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 the spinning-grade semi-dull nylon 6 slices into a main feeding position of a parallel co-rotating double-screw extrusion granulator through weightlessness, and controlling the feeding rotating speed of the main feeding position to be 25Hz;
(2) Adding PHA powder into a side feeding position of a parallel co-rotating double-screw extrusion granulator through weightlessness, and controlling the feeding rotating speed of the side feeding position to be 25Hz;
(3) Melting and plasticizing, wherein the temperature of each section of temperature zone is controlled as follows: the temperature of the first-stage temperature zone is 210 ℃; the temperature of the second-stage temperature zone is 220 ℃; the temperature of the third-stage 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 temperatures of the seventh, eighth and ninth temperature zones are 190 ℃; the temperature of the machine head temperature zone is 235 ℃;
(4) Sequentially performing the procedures of screw shearing, water-cooling granulating, vibrating screen and vacuum drying after melting and plasticizing to further prepare PHA master batches (physical parameters are shown in the attached table 1); wherein, the main machine rotating speed of the screw shearing is 520r/min, the main machine rotating speed of the granulator is 900r/min, and the diameter of the screen holes is 6-8mm.
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 nylon 6 slice, 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 the spinning-grade semi-dull nylon 6 slices into a main feeding position of a parallel co-rotating double-screw extrusion granulator through weightlessness, and controlling the feeding rotating speed of the main feeding position to be 23Hz;
(2) Adding PHA powder into a side feeding position of a parallel co-rotating double-screw extrusion granulator through weightlessness, and controlling the feeding rotation speed of the side feeding position to be 23Hz;
(3) Melting and plasticizing, wherein the temperature of each section of temperature zone is controlled as follows: the temperature of the first-stage temperature zone is 210 ℃; the temperature of the second-stage temperature zone is 220 ℃; the temperature of the third-stage 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 temperatures of the seventh, eighth and ninth temperature zones are 200 ℃; the temperature of the machine head temperature zone is 240 ℃;
(4) Sequentially performing the procedures of screw shearing, water-cooling granulating, vibrating screen and vacuum drying after melting and plasticizing to further prepare PHA master batches (physical parameters are shown in the attached table 1); wherein, the main machine rotating speed of the screw shearing is 550r/min, the main machine rotating speed of the granulator is 920r/min, and the diameter of the screen holes is 2-4mm.
Physical properties of PHA master batches for nylon 6 fibers according to examples 1 to 5 are shown in Table 1, PHA master batches for nylon 6 fibers prepared in examples 1 to 5 are used for directly spinning nylon 6 civil filament fibers (specification: POY FD 25D/24F), and the master batch addition ratio of each example is shown in Table 2; FIG. 2 is a physical image of biobased nylon 6 domestic filament fiber produced from PHA masterbatch produced according to example 1, and Table 3 shows physical indexes of biobased nylon 6 domestic filament fiber produced from PHA masterbatch produced according to examples 1 to 5 of the present invention; FIG. 3 is a fiber object diagram (specification: DTY FD 20D/24F) of a biobased nylon 6 civil filament fiber obtained by PHA masterbatch production according to example 1, and tables 4 and 5 are fiber physical properties indexes of the biobased nylon 6 civil filament fiber obtained by PHA masterbatch production according to examples 1 to 5 of the present invention; antibacterial data for the production of civil filament fibers from PHA masterbatch prepared in example 1 are shown in table 6; as can be seen from the drawings and the attached tables, the PHA master batch for the nylon 6 fiber prepared by the invention has excellent performance in the nylon 6 civil filament fiber, and can provide a new material selection for the continuous production of the bio-based nylon 6 civil filament fiber.
TABLE 1 PHA masterbatch physical parameters for chinlon 6 fibers
TABLE 2 masterbatch addition ratio in chinlon 6 household filament fiber
| Sequence number | Masterbatch addition ratio (%) |
| Example 1 | 10.0 |
| Example 2 | 8.0 |
| Example 3 | 6.7 |
| Example 4 | 5.7 |
| Example 5 | 5.0 |
TABLE 3 physical Properties index of biobased chinlon 6 household filament
TABLE 4 limiting physical Properties index after the ballistic application of biobased chinlon 6 civil filament fiber
TABLE 5 limiting physical Properties index after the ballistic loading of biobased chinlon 6 civil filament fiber
TABLE 6 antibacterial Property index of PHA masterbatch from example 1 to civil filament fiber
The foregoing description is only illustrative of the present invention and is not intended to limit the scope of the invention, and all equivalent structures or equivalent processes or direct or indirect application in other related arts 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 chinlon 6 slices, 10-20% of PHA powder and 1-2% of dispersing agent.
2. A PHA masterbatch for nylon 6 fiber as defined in claim 1, wherein: the luster of the spinning-grade chinlon 6 slices is bright or semi-dull; the relative viscosity of the spinning-grade chinlon 6 chip is 2.47-2.50.
3. A PHA masterbatch for nylon 6 fiber as defined in claim 1, wherein: the dispersing agent is an amide high molecular polymer.
4. A method for preparing PHA masterbatch for nylon 6 fiber as defined in claim 1, which comprises the following steps: quantitative feeding of raw materials, melt plasticizing, screw shearing, water-cooling granulating, vibration screening and vacuum drying, and finally preparing PHA master batch, wherein the water content is 300-500ppm, the melt index is 71.8-74.6g/10min, and the relative viscosity is 2.13-2.35; the formula of the PHA master batch for the nylon 6 fiber comprises the following components in percentage by mass: 78-89% of spinning-grade chinlon 6 slices, 10-20% of PHA powder and 1-2% of dispersing agent.
5. The method for preparing PHA master batch for nylon 6 fiber according to claim 4, wherein the method comprises the following steps: the quantitative raw material feeding is realized by a mode of linkage feeding of a main feeding position and a side feeding position: the main feeding position is added with spinning-grade nylon 6 slices, and the side feeding position is added with PHA powder; the feeding rotational speed of the main feeding level and the side feeding level is controlled to be 15-25Hz.
6. The method for preparing PHA master batch for nylon 6 fiber according to claim 4, wherein the method comprises the following steps: the temperature of each section of temperature zone of the melting plasticization is controlled as follows: the temperature of the first-stage temperature zone is 210 ℃; the temperature of the second-stage temperature zone is 220 ℃; the temperature of the third-stage temperature zone is 225 ℃; the temperature of the fourth temperature zone is 215-225 ℃; the temperature of the fifth temperature zone is 205-215 ℃; the temperature of the sixth temperature zone is 200-210 ℃; the temperature of the seventh section, the eighth section and the ninth section is 180-200 ℃; 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 method comprises the following steps: the rotation speed of the main machine for shearing the screw is 500-550r/min; the main machine rotating speed of the water-cooling granulating machine is 850-950r/min.
8. The method for preparing PHA master batch for nylon 6 fiber according to claim 4, wherein the method comprises the following steps: the diameter of the screen mesh hole of the vibration screening is 2-8mm.
9. A nylon 6 fiber made from at least one masterbatch by melt spinning, wherein the at least one masterbatch comprises the PHA masterbatch for nylon 6 fiber as defined in any one of claims 1 to 3.
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