CN118835340A - Preparation method of inorganic powder modified polylactic acid fiber - Google Patents
Preparation method of inorganic powder modified polylactic acid fiber Download PDFInfo
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- CN118835340A CN118835340A CN202411032074.3A CN202411032074A CN118835340A CN 118835340 A CN118835340 A CN 118835340A CN 202411032074 A CN202411032074 A CN 202411032074A CN 118835340 A CN118835340 A CN 118835340A
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- polylactic acid
- inorganic powder
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- modified polylactic
- acid fiber
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- 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
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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Textile Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Artificial Filaments (AREA)
Abstract
The invention provides a preparation method of inorganic powder modified polylactic acid fibers, which comprises the following steps: (1) Mixing 30-50 parts of inorganic powder, 0-5 parts of lubricant and 45-70 parts of polylactic acid slices, and injecting into a double-screw extruder for extrusion granulation to obtain master batch; the inorganic powder is subjected to surface treatment in advance by using a surface treating agent containing lipophilic and hydrophilic groups; (2) Blending 0.5-3 parts of master batch and 97-99.5 parts of polylactic acid slices, drying, injecting into a screw feed port for melt spinning, and cooling and forming to obtain an inorganic powder modified polylactic acid precursor; drawing the obtained precursor by a drawing machine; (4) Carrying out tension heat setting treatment on the drawn tows; (5) After curling, loosening, drying, cutting off and packing, the inorganic powder modified polylactic acid fiber is obtained. According to the invention, the polylactic acid is modified by using the inorganic powder as the crystallization nucleating agent, the strength of the modified finished fiber is improved, and the stability is obviously improved.
Description
Technical Field
The invention relates to the field of polylactic acid fiber manufacturing, in particular to a preparation method of inorganic powder modified polylactic acid fiber.
Background
Polylactic acid is a novel biodegradable polymer material, can be biodegraded under natural conditions, is finally changed into carbon dioxide and water, does not leave any pollutant, and is a famous and real environment-friendly and environment-friendly material. Meanwhile, the polylactic acid is a polymer material which is produced by taking crops such as corn, sugarcane, potato, sweet potato, straw and the like as raw materials and then carrying out a special reaction process, and the raw materials are renewable plant resources, so that the source is sufficient and the cost is low. Polylactic acid is also a linear aliphatic polyester, and has good biocompatibility and outstanding melt processability. Accordingly, the polylactic acid can be widely applied to the fields of textile, plastics, packaging and the like.
However, when applied to the textile field, polylactic acid materials have some defects such as slow crystallization speed, easy occurrence of bad crystal forms and the like, which seriously affect the physical and mechanical properties thereof. Therefore, compared with the traditional polyester fiber, the polylactic acid fiber has the common problems of low strength and poor stability, and the problem is also a bottleneck for expanding the application of the polylactic acid fiber.
Crystallization behavior is generally related to various aspects such as form selection, crystallization conditions, and crystallization nucleating agents. Wherein, the crystallization nucleating agent can promote the crystallization process of polylactic acid and improve the crystallization performance and mechanical property of the fiber. Therefore, in order to improve the application performance of the polylactic acid fiber, a proper crystallization nucleating agent can be selected for modifying the polylactic acid.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of inorganic powder modified polylactic acid fibers, which utilizes inorganic powder as a crystallization nucleating agent to modify polylactic acid, and can obviously improve the strength and stability of finished fibers.
The invention adopts the following technical scheme to solve the technical problems:
the preparation method of the inorganic powder modified polylactic acid fiber comprises the following steps:
(1) Mixing 30-50 parts of inorganic powder, 0-5 parts of lubricant and 45-70 parts of polylactic acid slices, and injecting into a double screw extruder for extrusion granulation to obtain master batch; wherein, the inorganic powder is subjected to surface treatment in advance by using a surface treating agent containing lipophilic and hydrophilic groups;
(2) Blending 0.5-3 parts of master batch and 97-99.5 parts of polylactic acid slices by weight, drying, injecting into a screw feed port for melt spinning, and cooling and forming by using circular blowing or side blowing to obtain an inorganic powder modified polylactic acid precursor;
(3) Drawing the obtained precursor to a target fineness by using a drawing machine;
(4) Carrying out tension heat setting treatment on the drawn tows;
(5) And then curling, loosening, drying, cutting off and packaging to obtain the inorganic powder modified polylactic acid fiber.
In the step (1), one or more of the TiO 2、SiO2、BaSO4、CaCO3 is selected as the inorganic powder, and the average particle diameter is 0.05 to 1.0 μm.
As one of the preferred modes of the present invention, in the step (1), the surface treatment agent containing lipophilic and hydrophilic groups is one or more selected from titanate coupling agents, aluminate coupling agents, stearic acid coupling agents, and silane coupling agents.
In the step (1), the lubricant is one or more selected from polyoxyethylene wax, fatty alcohol polyoxyethylene ether and ethylene bis-stearamide.
In the step (1), the inorganic powder, the lubricant and the polylactic acid chips are mixed and then fed into a twin-screw extruder to be extruded and pelletized at 180 to 260 ℃.
In the step (2), the blend is injected from a screw feed port, melt-spun at 180 to 260℃and cooled and molded by a loop blow or a side blow at 15 to 30 ℃.
In the step (3), the obtained yarn is drawn to a target fineness at 60 to 100 ℃ by a drawing machine.
In the step (4), the drawn yarn is subjected to tension heat setting at 90 to 150 ℃.
Compared with the prior art, the invention has the advantages that:
(1) According to the invention, inorganic powder is used as a crystallization nucleating agent to modify polylactic acid, so that the strength of the modified finished fiber is improved, and the stability is obviously improved;
(2) In the preparation of the polylactic acid fiber, the invention avoids the conventional treatment thought that inorganic powder is not adopted to directly mix the polylactic acid slices (the polylactic acid slices have high viscosity and are easy to cause uneven mixing, so that the powder has poor compatibility with a resin matrix, more coagulated particles are produced, the problems of broken filaments, low fiber strength and the like are easily produced in the spinning process), and the invention selects to use a surface treatment agent containing lipophilic and hydrophilic groups in advance to carry out surface treatment on the polylactic acid fibers and then mix the surface treatment agent with the polylactic acid slices, so that the mode can improve the subsequent processing performance and the fiber quality.
Drawings
FIG. 1 is a flow chart showing the steps of the method for producing the inorganic powder modified polylactic acid fiber in examples 1 to 4.
Detailed Description
The following describes in detail the examples of the present invention, which are implemented on the premise of the technical solution of the present invention, and detailed embodiments and specific operation procedures are given, but the scope of protection of the present invention is not limited to the following examples. Meanwhile, the reagent products and experimental methods used in the following examples are not specifically described, and are conventional reagents or methods in the art, and will not be described in detail.
Example 1
The preparation method of the inorganic powder modified polylactic acid fiber in the embodiment, as shown in fig. 1, comprises the following steps:
(1) Preparation of master batch
30 Parts of inorganic powder TiO 2 (with the particle size of 0.05-1.0 micron) and 45 parts of polylactic acid slices are mixed in parts by weight, injected into a double-screw extruder, extruded and granulated at the temperature of 180 ℃ to obtain master batch. Wherein, the inorganic powder is subjected to surface treatment by using a titanate coupling agent in advance.
(2) Drying
0.5 Part of master batch and 97 parts of polylactic acid slices are blended and added into a vacuum drum dryer, the temperature is raised to 95 ℃ for vacuum drying for 10 hours, and then the mixture is cooled to 80 ℃ for vacuum drying for 2 hours. The water content of the slices was 35ppm.
(3) Spinning process
Injecting the dried mixture from a screw feed port for melt spinning, wherein the diameter of a spinning screw is 40mm, and the length-diameter ratio is 1:30, spinning at 180 ℃ and winding speed of 1020m/min, and cooling and molding by using 15 ℃ circular air blowing to obtain the inorganic powder modified polylactic acid precursor.
(3) Drafting
The obtained filaments were drawn by a drawing machine. Wherein, one section of stretching is carried out in a water bath in a drafting bath at 60 ℃; the second stretching is carried out in a steam heating box, the temperature is 80 ℃, the speed is 120m/min, and the stretching multiplying power is 3.62.
(4) Tension heat setting
The drawn yarn is subjected to tension heat setting treatment at 90 ℃, a crimping (steam) preheating box at 80 ℃, a crimping wheel main pressure of 0.35MPa, and a relaxation heat setting temperature of 65 ℃.
(5) Post-treatment
And then curling, loosening, drying, cutting off and packaging to obtain the inorganic powder modified polylactic acid fiber.
Example 2
The preparation method of the inorganic powder modified polylactic acid fiber in the embodiment, as shown in fig. 1, comprises the following steps:
(1) Preparation of master batch
According to parts by weight, 40 parts of inorganic powder SiO 2 (with the particle size of 0.05-1.0 micron), 2 parts of polyoxyethylene wax and 50 parts of polylactic acid slices are mixed, injected into a double-screw extruder, extruded and granulated at the temperature of 200 ℃ to obtain master batch. Wherein, the inorganic powder is subjected to surface treatment by using an aluminate coupling agent in advance.
(2) Drying
2 Parts of master batch and 98 parts of polylactic acid slices are blended and added into a vacuum drum dryer, the temperature is raised to 95 ℃ for vacuum drying for 10 hours, and then the mixture is cooled to 80 ℃ for vacuum drying for 2 hours. The water content of the slices was 35ppm.
(3) Spinning process
Injecting the dried mixture from a screw feed port for melt spinning, wherein the diameter of a spinning screw is 40mm, and the length-diameter ratio is 1:30, spinning holes with the number of 300, the spinning temperature of 240 ℃, the winding speed of 1020m/min, and cooling and molding by using side blowing air with the temperature of 24 ℃ to prepare the inorganic powder modified polylactic acid precursor.
(3) Drafting
The obtained filaments were drawn by a drawing machine. Wherein, one section of stretching is carried out in a water bath in a drafting bath at the temperature of 62 ℃; the second stretching is carried out in a steam heating box, the temperature is 80 ℃, the speed is 120m/min, and the stretching multiplying power is 3.62.
(4) Tension heat setting
The drawn yarn is subjected to tension heat setting treatment at 130 ℃, a crimping (steam) preheating box at 80 ℃, a crimping wheel main pressure of 0.35MPa, and a relaxation heat setting temperature of 65 ℃.
(5) Post-treatment
And then curling, loosening, drying, cutting off and packaging to obtain the inorganic powder modified polylactic acid fiber.
Example 3
The preparation method of the inorganic powder modified polylactic acid fiber in the embodiment, as shown in fig. 1, comprises the following steps:
(1) Preparation of master batch
According to parts by weight, 40 parts of inorganic powder BaSO 4 (with the particle size of 0.05-1.0 microns), 4 parts of fatty alcohol-polyoxyethylene ether and 60 parts of polylactic acid slices are mixed, injected into a double-screw extruder, extruded and granulated at the temperature of 250 ℃ to obtain master batch, wherein the inorganic powder is subjected to surface treatment by using a stearic acid coupling agent in advance.
(2) Drying
2.5 Parts of master batch and 99 parts of polylactic acid slices are blended and added into a vacuum drum dryer, the temperature is raised to 95 ℃ for vacuum drying for 10 hours, and then the mixture is cooled to 80 ℃ for vacuum drying for 2 hours. The water content of the slices was 35ppm.
(3) Spinning process
Injecting the dried mixture from a screw feed port for melt spinning, wherein the diameter of a spinning screw is 40mm, and the length-diameter ratio is 1:30, spinning at 250 ℃ and winding speed of 1020m/min with 300 holes of spinning hole number, and cooling and molding by using a ring air blow at 28 ℃ to obtain the inorganic powder modified polylactic acid precursor.
(3) Drafting
The obtained filaments were drawn by a drawing machine. Wherein, one section of stretching is carried out in a water bath in a stretching bath at 65 ℃; the second stretching is carried out in a steam heating box, the temperature is 80 ℃, the speed is 120m/min, and the stretching multiplying power is 3.62.
(4) Tension heat setting
The drawn yarn is subjected to tension heat setting treatment at 140 ℃, a crimping (steam) preheating box at 80 ℃, a crimping wheel main pressure of 0.35MPa, and a relaxation heat setting temperature of 65 ℃.
(5) Post-treatment
And then curling, loosening, drying, cutting off and packaging to obtain the inorganic powder modified polylactic acid fiber.
Example 4
The preparation method of the inorganic powder modified polylactic acid fiber in the embodiment, as shown in fig. 1, comprises the following steps:
(1) Preparation of master batch
50 Parts of inorganic powder CaCO 3 (with the particle size of 0.05-1.0 micron), 5 parts of ethylene bis-stearamide and 70 parts of polylactic acid slices are mixed by weight, and the mixture is injected into a double-screw extruder to be extruded and granulated at the temperature of 260 ℃ to obtain master batch. Wherein, the inorganic powder is subjected to surface treatment in advance by using a silane coupling agent.
(2) Drying
3 Parts of master batch and 99.5 parts of polylactic acid slices are blended and added into a vacuum drum dryer, the temperature is raised to 95 ℃ for vacuum drying for 10 hours, and then the mixture is cooled to 80 ℃ for vacuum drying for 2 hours. The water content of the slices was 35ppm.
(3) Spinning process
Injecting the dried mixture from a screw feed port for melt spinning, wherein the diameter of a spinning screw is 40mm, and the length-diameter ratio is 1:30, the number of spinning holes is 300, the spinning temperature is 260 ℃, the winding speed is 1020m/min, and cooling molding is carried out by side blowing at the temperature of 30 ℃ to prepare the inorganic powder modified polylactic acid precursor.
(3) Drafting
The obtained filaments are drawn by a drawing machine (60-100 ℃). Wherein, one section of stretching is carried out in a water bath in a drafting bath at the temperature of 62 ℃; the second-stage stretching is carried out in a steam heating box, the temperature is 100 ℃, the speed is 120m/min, and the stretching multiplying power is 3.62.
(4) Tension heat setting
The drawn yarn is subjected to tension heat setting treatment at 150 ℃, a crimping (steam) preheating box at 80 ℃, a crimping wheel main pressure of 0.35MPa, and a relaxation heat setting temperature of 65 ℃.
(5) Post-treatment
And then curling, loosening, drying, cutting off and packaging to obtain the inorganic powder modified polylactic acid fiber.
The inorganic powder modified polylactic acid fiber (example 2) obtained by the present invention was subjected to performance test, and the results are shown in table 1.
TABLE 1 detection results of the properties of the inorganic powder modified polylactic acid fiber of the present invention
| Item/unit | Standard of | Actual measurement values of the invention |
| Linear density (dtex) | 1.33 | 1.32 |
| Breaking strength (cn/dtex) | ≥3.60 | 4.15 |
| Breaking strength CV value (%) | ≤12.0 | 5.0 |
| Elongation at break (%) | 30.0±6.0 | 31.2 |
| Elongation at break CV value | / | 18.7 |
| 130 ℃ Dry heat shrinkage yield (%) | 5.0±2.0 | 4.6 |
| Number of curls (number/25 mm) | 12±2.5 | 12.2 |
| Curvature (%) | 12±2.5 | 12.8 |
| Oil content (%) | / | 0.16 |
| Specific resistance (omega cm) | ≤1*108 | 6.7*106 |
| Moisture regain (%) | / | 0.48 |
In conclusion, the invention adopts inorganic powder as crystallization nucleating agent to modify polylactic acid, and the modified finished fiber has high strength and good stability.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (8)
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| CN202411032074.3A CN118835340A (en) | 2024-07-30 | 2024-07-30 | Preparation method of inorganic powder modified polylactic acid fiber |
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| CN202411032074.3A CN118835340A (en) | 2024-07-30 | 2024-07-30 | Preparation method of inorganic powder modified polylactic acid fiber |
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Application publication date: 20241025 |
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