Extra-black far-infrared matte master batch for polyester fibers and preparation method of extra-black far-infrared matte master batch

Abstract

The invention discloses a preparation method of an extra-black far-infrared matte master batch for polyester fibers, which realizes the cooperation of a far-infrared function and a matte effect by optimizing a powder dispersion and composite extinction technology, and meets the dual requirements of high-end textiles on aesthetics and performance. The functional powder additive used in the invention has the characteristics of safety and high efficiency, and does not influence the spinning process of the color master batch and the subsequent application of the fiber. The prepared product has health protection and thermal comfort, is suitable for the fields of intelligent wearing, health protection and the like, and promotes the industry to be upgraded to a high value-added direction. The method is simple, the modification cost is low, expensive equipment is not needed, and large-scale application and popularization are facilitated.

Description

Technical Field

[0001] This invention belongs to the field of functional textile and chemical fiber technology, specifically relating to a special black far-infrared matte masterbatch for polyester fibers and its preparation method. Background Technology

[0002] With the continued growth in demand for functional textile materials, polyester fiber products are increasingly being used in fields such as smart wearables and health protection. Traditional polyester fiber materials often face problems such as excessive gloss and limited functionality, making it difficult to meet the market's demand for high-end products that combine aesthetics and performance. Far-infrared functionality, due to its properties such as promoting microcirculation and improving thermal comfort, has become an important development direction for health textiles; while the matte effect can give products a low-key and luxurious appearance while reducing light pollution.

[0003] However, achieving the synergistic effect of far-infrared functionality and matte finish in existing technologies remains challenging: inorganic matting agents can easily lead to a decline in the mechanical properties of materials, uneven dispersion of far-infrared powder affects functional stability, and multi-component compounding can easily cause phase separation problems. Therefore, it is necessary to propose a method that can effectively mix far-infrared matte functionality with the fiber matrix and achieve continuous and efficient production. Summary of the Invention

[0004] The purpose of this section is to outline some aspects of embodiments of the present invention and to briefly describe some preferred embodiments. Simplifications or omissions may be made in this section, as well as in the abstract and title of this application, to avoid obscuring the purpose of these documents; however, such simplifications or omissions should not be construed as limiting the scope of the invention.

[0005] In view of the problems existing in the above and / or prior art, the present invention is proposed.

[0006] Therefore, the purpose of this invention is to overcome the shortcomings of the prior art and provide a special black far-infrared matte masterbatch for polyester fibers.

[0007] To solve the above-mentioned technical problems, the present invention provides the following technical solution: a special black far-infrared matte masterbatch for polyester fibers, characterized in that, by mass parts, it comprises the following components: 45-75 parts of high molecular weight polymer resin; 15-30 parts carbon black; 10-25 parts of functional powder additives; 1-5 parts of dispersant; The functional powder additives include barium sulfate, nano-silica, and carbon nanomaterials.

[0008] As a preferred embodiment of the extra-black far-infrared matte masterbatch for polyester fibers described in this invention, the polymer resin includes one of polyethylene terephthalate (PET) and polybutylene terephthalate (PBT), wherein the intrinsic viscosity of the resin is 0.65 dL / g to 1.10 dL / g.

[0009] As a preferred embodiment of the extra-black far-infrared matte masterbatch for polyester fibers described in this invention, the carbon nanomaterial is selected from at least one of multi-walled carbon nanotubes, single-walled carbon nanotubes, and graphene powder.

[0010] As a preferred embodiment of the extra black far-infrared matte masterbatch for polyester fiber described in this invention, wherein, by mass parts, the functional powder additive comprises 50-70% barium sulfate, 10-20% nano-silica, and 20-30% carbon nanomaterials.

[0011] As a preferred embodiment of the extra-black far-infrared matte masterbatch for polyester fibers described in this invention, the dispersant includes one or more of stearamide, ethylene bis-stearamide, oxidized polyethylene homopolymer, montan wax, and polymeric dispersants.

[0012] As a preferred embodiment of the extra-black far-infrared matte masterbatch for polyester fiber described in this invention, the masterbatch has a haze value ≥85%, a far-infrared emissivity ≥0.86, and a breaking strength of the fiber obtained by spinning ≥3.5 cN / dtex.

[0013] Another objective of this invention is to overcome the shortcomings of the prior art and provide a method for preparing extra-black far-infrared matte masterbatch for polyester fibers, characterized by comprising: Pretreatment: Dry the polymer resin; Pre-dispersion: Carbon black, functional powder additives and dispersant are mixed at high speed to obtain a premix; Melt extrusion: The dried resin and premix are added to a twin-screw extruder, melt-blended, extruded, cooled, and pelletized to obtain the masterbatch.

[0014] In a preferred embodiment of the preparation method described in this invention, the drying temperature is 120~140℃ and the drying time is 3~5 hours; the high-speed stirring speed is 800~1200 rpm and the time is 10~30 minutes.

[0015] In a preferred embodiment of the preparation method described in this invention, the temperature range of the twin-screw extruder from the feeding section to the die head is 240~280℃, and the screw speed is 200~400 rpm; the temperatures of each zone of the extruder include: zone 1 temperature 200~220℃, zone 2 temperature 250~265℃, zone 3 temperature 260~275℃, zone 4 temperature 260~280℃, zone 5 temperature 260~280℃, zone 6 temperature 220~230℃, zone 7 temperature 210~220℃, zone 8 temperature 190~210℃, zone 9 temperature 180~200℃, zone 10 temperature 220~240℃, zone 11 temperature 220~240℃, and the die head temperature 255~265℃.

[0016] Another objective of this invention is to overcome the shortcomings of the prior art and provide an application of a special black far-infrared matte masterbatch for polyester fibers in the preparation of polyester fibers, textiles, or smart wearable products with matte effect and far-infrared health care function.

[0017] Beneficial effects of this invention: (1) Good functional synergy: By precisely combining components such as carbon black, barium sulfate, carbon nanotubes / graphene, this invention achieves the synergy of three major functions: black coloring, matte finish, and far-infrared radiation, thus solving the problem of single function or poor synergy in the prior art. (2) Excellent dispersibility and compatibility: By selecting suitable dispersants and pre-dispersion processes, multi-component agglomeration and phase separation are avoided, ensuring the compatibility between the masterbatch and the polyester matrix and ensuring smooth subsequent spinning. (3) Stable mechanical properties: The type, particle size and proportion of functional powder are limited to avoid the fiber strength reduction caused by excessive inorganic powder. The fiber breaking strength is ≥3.6cN / dtex, which meets the requirements of textile application. (4) Simple and scalable process: The conventional high-speed mixing + twin-screw extrusion granulation process is adopted. The parameters are clear and no special equipment is required, which is convenient for the transformation of the existing production line and continuous production in the factory. (5) Wide range of applications: It is suitable for high-end polyester fiber products such as thermal underwear, waist and knee pads, and smart wearable fabrics, and has a broad market prospect. Detailed Implementation

[0018] To make the above-mentioned objects, features and advantages of the present invention more apparent and understandable, the specific embodiments of the present invention will be described in detail below with reference to the examples in the specification.

[0019] Many specific details are set forth in the following description in order to provide a full understanding of the invention. However, the invention may also be practiced in other ways different from those described herein, and those skilled in the art can make similar extensions without departing from the spirit of the invention. Therefore, the invention is not limited to the specific embodiments disclosed below.

[0020] Secondly, the term "one embodiment" or "embodiment" as used herein refers to a specific feature, structure, or characteristic that may be included in at least one implementation of the present invention. The phrase "in one embodiment" appearing in different places in this specification does not necessarily refer to the same embodiment, nor is it a single or selective embodiment that is mutually exclusive with other embodiments.

[0021] The matrix resins selected in this invention include polyethylene terephthalate (PET) and polybutylene terephthalate (PBT), specifically WB-8863 produced by SK Chemicals (Korea) and Celanex® 3300-2 produced by Celanex (Germany). The carbon nanomaterials encompass three categories: multi-walled carbon nanotubes, single-walled carbon nanotubes, and graphene powder, corresponding to multi-walled carbon nanotubes TNIM9 produced by Tiannai Technology (China), single-walled carbon nanotubes SG76 produced by Shenzhen Nanoport (China), and graphene powder GR-100 produced by Ningbo Moxi (China). The inorganic fillers used are barium sulfate BLD-BaSO4-01 manufactured by Suzhou Baolidi and nano-silica AEROSIL® R972 produced by Evonik. The processing and dispersing agents used are stearamide SA1801 produced by Kao Corporation (Japan), ethylene bis-stearamide EBS-200 produced by Clariant (USA), oxidized polyethylene homopolymer OPE-10 produced by Honeywell (USA), and montmorillonite® produced by Clariant (Germany). E. DISPERBYK-163, a polymeric dispersant produced by BYK Chemicals in Germany.

[0022] Test items and standards in this embodiment of the invention: (1) Matte effect: The haze value of the masterbatch pressed sample was tested by a haze meter (haze ≥85% is excellent, 70~85% is good, <70% is unqualified); (2) Far-infrared emissivity: The emissivity in the 2~18μm band was tested using a far-infrared spectrometer (≥0.90 is excellent, 0.85~0.90 is good, <0.85 is unqualified). (3) Dispersibility: The powder agglomeration of the masterbatch slices was observed by polarizing microscope (no obvious agglomeration is excellent, a small amount of agglomeration is good, and a large amount of agglomeration is unqualified). (4) Mechanical properties: Add the masterbatch to the polyester chips at a ratio of 10% and spin them. Test the fiber breaking strength (≥3.5cN / dtex is acceptable). (5) Coloring effect: The L value of the fiber is tested by a colorimeter (L≤15 is extra black, 15~20 is dark black, >20 is unqualified).

[0023] Example 1 This embodiment provides a method for preparing extra-black far-infrared matte masterbatch for polyester fibers, including the following steps: (1) Preparation of raw materials: by mass, 60 parts of PET resin (intrinsic viscosity 0.95dL / g), 20 parts of carbon black (Cabot N330), 18 parts of functional powder additives (including 10 parts of 5μm barium sulfate, 2 parts of nano silica, 4 parts of multi-walled carbon nanotubes, and 2 parts of graphene powder), and 2 parts of dispersant (EBS and montan wax mixed in a 1:1 ratio).

[0024] (2) Pretreatment: Place the PET resin in a 130℃ oven and dry for 5 hours to ensure that the moisture content is ≤0.05%; (3) Pre-dispersion: The dried PET resin, carbon black, functional powder additives and dispersant are put into a high-speed mixer and stirred at 1000 r / min for 20 min to complete the pre-dispersion. (4) Melt extrusion: The pre-dispersed mixture is added to a twin-screw extruder, and the temperatures of each zone of the extruder are set as follows: Zone 1 210℃, Zone 2 260℃, Zone 3 270℃, Zone 4 275℃, Zone 5 275℃, Zone 6 225℃, Zone 7 215℃, Zone 8 200℃, Zone 9 190℃, Zone 10 230℃, Zone 11 230℃, the die temperature is 260℃, and the screw speed is 400r / min. The blending melt extrusion is carried out. (5) Cooling and pelletizing: The extruded melt is cooled with 25°C cooling water, air-dried, and then pelletized by a pelletizer to obtain extra black far-infrared matte masterbatch.

[0025] Example 2 This embodiment provides a method for preparing extra-black far-infrared matte masterbatch for polyester fibers, including the following steps: (1) Preparation of raw materials: by mass, 55 parts of PET resin (intrinsic viscosity 0.95dL / g), 25 parts of carbon black (Cabot N330), 17 parts of functional powder additives (including 12 parts of 5μm barium sulfate, 1 part of nano silica, 3 parts of multi-walled carbon nanotubes, and 1 part of graphene powder), and 3 parts of dispersant (EBS and montan wax mixed in a 1:1 ratio).

[0026] (2) Pretreatment: The PET resin was dried in an oven at 125℃ for 5.5 hours, and the moisture content was ≤0.05%; (3) Pre-dispersion: High-speed mixer speed 900 r / min, mixing time 25 min; (4) Melt extrusion: The extruder die temperature was 258°C, the screw speed was 350 r / min, and the temperatures of the other zones were the same as in Example 1; (5) Cooling and pelletizing: The extruded melt is cooled by 22°C cooling water, air-dried, and then pelletized by a pelletizer to obtain extra black far-infrared matte masterbatch.

[0027] Example 3 This embodiment provides a method for preparing extra-black far-infrared matte masterbatch for polyester fibers, including the following steps: (1) Preparation of raw materials: by mass, 70 parts of PET resin (intrinsic viscosity 0.95dL / g), 18 parts of carbon black (Cabot N330), 10 parts of functional powder additives (including 8 parts of 5μm barium sulfate, 2 parts of nano silica, and no multi-walled carbon nanotubes and graphene powder), and 2 parts of dispersant (EBS and montan wax mixed in a 1:1 ratio).

[0028] (2) Pretreatment: The PET resin was dried in an oven at 135℃ for 4.5h, and the moisture content was ≤0.05%; (3) Pre-dispersion: High-speed mixer speed 1100 r / min, mixing time 18 min; (4) Melt extrusion: The extruder die temperature was 262℃, the screw speed was 450r / min, and the temperatures of the other zones were the same as in Example 1; (5) Cooling and pelletizing: Cooling water temperature 28℃.

[0029] Example 4 This embodiment provides a method for preparing extra-black far-infrared matte masterbatch for polyester fibers, including the following steps: (1) Preparation of raw materials: by mass, 48 ​​parts of PET resin (intrinsic viscosity 0.95dL / g), 28 parts of carbon black (Cabot N330), 23 parts of functional powder additives (including 15 parts of 5μm barium sulfate, 3 parts of nano silica, 3 parts of multi-walled carbon nanotubes, and 2 parts of graphene powder), and 1 part of dispersant (EBS and montan wax mixed in a 1:1 ratio).

[0030] (2) Pretreatment: The PET resin was dried in an oven at 120℃ for 6 hours, and the moisture content was ≤0.05%; (3) Pre-dispersion: High-speed mixer speed 850 r / min, mixing time 30 min; (4) Melt extrusion: The extruder die temperature is 255℃, the screw speed is 380r / min, and the temperatures of the other zones are the same as in Example 1; (5) Cooling and pelletizing: Cooling water temperature 20℃, pellet size after pelletizing is 2.5mm.

[0031] Example 5 This embodiment provides a method for preparing extra-black far-infrared matte masterbatch for polyester fibers, including the following steps: (1) Preparation of raw materials: by mass, 65 parts of PET resin (intrinsic viscosity 0.95dL / g), 22 parts of carbon black (Cabot N330), 12 parts of functional powder additives (including 7 parts of 5μm barium sulfate, 3 parts of multi-walled carbon nanotubes, 2 parts of graphene powder, and no nano silica), and 1 part of dispersant (EBS and montan wax mixed in a 1:1 ratio).

[0032] (2) Pretreatment: The PET resin was dried in an oven at 140℃ for 4 hours, and the moisture content was ≤0.05%; (3) Pre-dispersion: High-speed mixer speed 1200 r / min, mixing time 15 min; (4) Melt extrusion: The extruder die temperature was 265℃, the screw speed was 420r / min, and the temperatures of the other zones were the same as in Example 1; (5) Cooling and pelletizing: Cooling water temperature 30℃.

[0033] The core differences between Examples 1 to 5 are shown in Table 1.

[0034] Table 1

[0035] The differences between Comparative Examples 1-5 and Example 1 are shown in Table 2. All other steps are the same as in Example 1.

[0036] Table 2

[0037] Performance tests were conducted on Examples 1-5 and Comparative Examples 1-5, and the test results are shown in Table 3.

[0038] Table 3

[0039] As shown in Table 3, the test results of Examples 1 to 5 all meet the requirements of "extra black (L*≤15), high haze (≥88%), high far-infrared emissivity (≥0.88), good / excellent dispersibility, and fiber breaking strength ≥3.6cN / dtex", indicating that the formulation and process design of the present invention are reasonable and can achieve synergy of the three major functions and good processing performance.

[0040] Comparative Example 1 showed severe agglomeration of functional powders due to the lack of dispersant, resulting in a decrease in fiber breaking strength (3.2 cN / dtex) and a slight decrease in far-infrared emissivity, demonstrating the key role of dispersant in multi-component compatibility. Comparative Example 2 had a haze of only 68% (unacceptable), and the excessive amount of nano-silica led to a decrease in fiber strength, indicating that barium sulfate is the core matting component and its proportion needs to be controlled. Comparative Example 3 showed a far-infrared emissivity of only 0.82 (unacceptable), proving that carbon nanotube / graphene powder is the core source of far-infrared function; Comparative Example 4 showed severe carbon nanotube agglomeration and decreased fiber strength, indicating that functional powders need to be formulated according to the proportions specified in this invention to avoid excessive amounts of any single component. Comparative Example 5 had a fiber L* value of 22 (unqualified), which could not achieve a special black effect, proving that the amount of carbon black used should be in the range of 15 to 30 parts.

[0041] In summary, this invention achieves a synergistic effect of three major functions—extra black coloring, matte finish, and far-infrared radiation—through the precise combination of components such as carbon black, barium sulfate, and carbon nanotubes / graphene. This solves the problem of single function or poor synergy in existing technologies. By selecting suitable dispersants and pre-dispersion processes, it avoids multi-component agglomeration and phase separation, ensuring the compatibility of the masterbatch and the polyester matrix, and ensuring smooth subsequent spinning. By limiting the type, particle size, and proportion of functional powders, it avoids the decrease in fiber strength caused by excessive inorganic powders. The resulting fiber has a breaking strength ≥3.6 cN / dtex, meeting the requirements of textile applications.

[0042] It should be noted that the above embodiments are only used to illustrate the technical solutions of the present invention and are not intended to limit it. Although the present invention has been described in detail with reference to preferred embodiments, those skilled in the art should understand that modifications or equivalent substitutions can be made to the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, and all such modifications or substitutions should be covered within the scope of the present invention.

Claims

1. A special black far-infrared matte masterbatch for polyester fibers, characterized in that, Based on the mass fractions of the raw materials, it includes the following components: 45-75 parts of high molecular weight polymer resin; 15-30 parts carbon black; 10-25 parts of functional powder additives; 1-5 parts of dispersant; The functional powder additive is composed of barium sulfate, nano-silica, and carbon nanomaterials.

2. The extra-black far-infrared matte masterbatch for polyester fibers as described in claim 1, characterized in that: The polymeric resin includes one of polyethylene terephthalate (PET) and polybutylene terephthalate (PBT), wherein the intrinsic viscosity of the resin is 0.65 dL / g to 1.10 dL / g.

3. The extra-black far-infrared matte masterbatch for polyester fibers as described in claim 1, characterized in that: The carbon nanomaterial is selected from at least one of multi-walled carbon nanotubes, single-walled carbon nanotubes, and graphene powder.

4. The extra-black far-infrared matte masterbatch for polyester fibers as described in claim 1, characterized in that: By mass percentage, the functional powder additive contains 50-70% barium sulfate, 10-20% nano-silica, and 20-30% carbon nanomaterials.

5. The extra-black far-infrared matte masterbatch for polyester fibers as described in claim 1, characterized in that: The dispersant includes one or more of stearamide, ethylene bis-stearamide, oxidized polyethylene homopolymer, montan wax, and polymeric dispersants.

6. The extra-black far-infrared matte masterbatch for polyester fibers as described in claim 1, characterized in that: The masterbatch has a haze value of ≥85%, a far-infrared emissivity of ≥0.86, and a breaking strength of ≥3.5 cN / dtex for the fibers obtained by spinning.

7. The method for preparing extra-black far-infrared matte masterbatch for polyester fibers as described in any one of claims 1 to 6, characterized in that: include, Pretreatment: Dry the polymer resin; Pre-dispersion: Carbon black, functional powder additives and dispersant are mixed at high speed to obtain a premix; Melt extrusion: The dried resin and premix are added to a twin-screw extruder, melt-blended, extruded, cooled, and pelletized to obtain the masterbatch.

8. The preparation method according to claim 7, characterized in that, The drying temperature is 120~140℃, and the drying time is 3~5 hours; the high-speed stirring speed is 800~1200 rpm, and the time is 10~30 minutes.

9. The preparation method according to claim 7, characterized in that, The twin-screw extruder has a temperature range of 240~280℃ from the feeding section to the die, and a screw speed of 200~400 rpm. The temperatures of each zone of the extruder are as follows: Zone 1: 200~220℃; Zone 2: 250~265℃; Zone 3: 260~275℃; Zone 4: 260~280℃; Zone 5: 260~280℃; Zone 6: 220~230℃; Zone 7: 210~220℃; Zone 8: 190~210℃; Zone 9: 180~200℃; Zone 10: 220~240℃; Zone 11: 220~240℃; and the die temperature is 255~265℃.

10. The use of the extra-black far-infrared matte masterbatch for polyester fibers as described in any one of claims 1 to 6 in the preparation of polyester fibers, textiles or smart wearable products with matte effect and far-infrared health care function.

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