LU501702B1 - Carbon Black Masterbatch for Nylon 6 Civil Filament Fiber, Preparation and Application Thereof - Google Patents

Carbon Black Masterbatch for Nylon 6 Civil Filament Fiber, Preparation and Application Thereof Download PDF

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LU501702B1
LU501702B1 LU501702A LU501702A LU501702B1 LU 501702 B1 LU501702 B1 LU 501702B1 LU 501702 A LU501702 A LU 501702A LU 501702 A LU501702 A LU 501702A LU 501702 B1 LU501702 B1 LU 501702B1
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carbon black
nylon
masterbatch
civil
die
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LU501702A
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English (en)
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Ziming Zhang
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Fujian Eversun Jinjiang Co Ltd
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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
    • 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
    • D01F1/04—Pigments
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K3/00—Use of inorganic substances as compounding ingredients
    • C08K3/02—Elements
    • C08K3/04—Carbon
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L77/00—Compositions of polyamides obtained by reactions forming a carboxylic amide link in the main chain; Compositions of derivatives of such polymers
    • C08L77/02—Polyamides derived from omega-amino carboxylic acids or from lactams thereof
    • 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
    • D01F6/58—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products
    • D01F6/60—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from homopolycondensation products from polyamides
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/011—Nanostructured additives
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00—Specific properties of additives
    • C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K

Abstract

The carbon black masterbatch for nylon 6 civil filament fiber includes 57.79 wt percent polyamide 6 chips, 20.40 wt percent nano-grade carbon black powder and 1.3 wt percent single carbon black super dispersant powder. According to the preparation method, the raw materials are sequentially subjected to constant feeding, melting plasticization, screw transmission and shearing, water cooling granulation, vibration screening and blast drying to prepare the carbon black masterbatch for nylon 6 civil filament fiber. The carbon black masterbatch for nylon 6 civil filament fiber provided by the invention can be directly applied to the production of black nylon 6 civil filament fiber with excellent dyeing effect and continuous production. The production cycle of spinning components in the spinning process can reach 21-24 days, and it can effectively solve the problems of uneven evenness and sharp increase of wool fibers.

Description

DESCRIPTION LU501702 Carbon Black Masterbatch for Nylon 6 Civil Filament Fiber, Preparation and Application Thereof
TECHNICAL FIELD The invention belongs to the technical field of new chemical fiber materials, and particularly relates to a carbon black masterbatch for nylon 6 civil filament fiber, a preparation method and application thereof.
BACKGROUND Nylon 6 fiber is widely used in many fields because of its excellent physical properties, such as high strength, good hygroscopicity and bright dyeing. In recent years, the research of nylon 6 fiber, especially for nylon 6 fiber with various differences, has developed rapidly.
Nylon 6 civil filament fiber 1s one of the main raw materials for clothing textiles. According to statistics, in 2020, the apparent consumption of nylon 6 civil filament fiber in China has reached 1.859 million tons. Among them, the apparent consumption of black nylon 6 civil filament fiber has reached about 35,000 tons; the black nylon 6 civil filament fiber produced by adding black masterbatch occupies the core position in the product structure. The main carbon black masterbatch used in the domestic market mainly comes from imported products, which generally has the problems of high price and short spinning component cycle, which is not conducive to continuous production of spinning mills and affects production efficiency and economic benefits. At present, few mast batch manufacturers in China can provide high-quality carbon black mast batch products, and one of that difficulties in its preparation lies in that on the premise of high blackness and carbon content of mast batch, carbon black needs to maintain excellent dispersibility in carrier polyamide 6 resin. However, the conventional methods and additives used in the prior art can't achieve the dispersibility required by the preparation of carbon black masterbatch; another difficulty lies in the fact that carbon black masterbatch is easy to appear in the later stage of long-period spinning production, which leads to spinning jitter and uneven evenness of nylon 6 fiber and sharp increase of hair.
SUMMARY In order to solve the problems existing in the prior art, the invention provides a carbon black masterbatch and a preparation method thereof, and applies the carbon black masterbatch to nylon 6 civil filament fiber, so that the nylon 6 civil filament fiber has excellent spinnability, few broken ends and floating times, long service life of spinning components and can effectively 501702 solve the phenomena of uneven evenness and sharp increase of wool fibers.
The technical scheme of the invention is as follows: The invention discloses a carbon black masterbatch for nylon 6 civil filament fiber, which comprises the following components in percentage by weight: 57-79% of polyamide 6 chips, 20-40% of nano-grade carbon black powder and 1-3% of single carbon black hyperdispersant powder.
Further, the polyamide 6 chips are fiber-grade bright polyamide 6 chips or semi-dull polyamide 6 chips, and are granular.
Further, the particle size of thenano-grade carbon black powder is 25-30 nm.
Further, the single type carbon black hyperdispersant powder is CLIQ SPERSE” 330.
The invention discloses a preparation method of carbon black masterbatch for nylon 6 civil filament fiber, which specifically comprises the following steps: Polyamide 6 chips, nano-grade carbon black powder and single carbon black super dispersant powder were sequentially subjected to quantitative feeding, melting plasticization, screw transmission and shearing, water-cooling granulation, vibration screening and air drying to prepare carbon black master particles for nylon 6 civil filament fibers.
Further, the quantitative feeding 1s carried out through the linkage feeding mode of the main feeding position and the side feeding position; Adding polyamide 6 chips through the main feeding position, adding nano-grade carbon black powder and single carbon black hyperdispersant powder through the side feeding position; The feeding speed of the main feeding position and the side feeding position is 20-30 Hz.
Further, the melting and plasticizing process is divided into eleven temperature zones and a machine head temperature zone; The temperature control of each temperature zone is as follows: the first temperature zone is 200-215°C, the second temperature zone is 205-220°C, the third temperature zone is 210-225°C, the fourth, fifth and sixth temperature zones are 220-240°C, the seventh temperature zone is 200-215°C, the eighth temperature zone is 200-215°C, and the ninth temperature zone is 195-205°C.
Further, the rotating speed of the main machine for screw transmission and shearing is 600-825 r/min; The main engine speed of the water-cooled granulator is 670-730 r/min.
Furthermore, the moisture content of carbon black masterbatch for nylon 6 civil filament fiber after air-blast drying is 400-450 ppm, the melt index is 4.5-12.9 g/10 min, and the relatiye 501702 viscosity is 1.49-2.19.
The invention also discloses an application of the carbon black masterbatch prepared according to the preparation method of the carbon black masterbatch for nylon 6 civil filament fiber in nylon 6 civil filament fiber.
Compared with the prior art, the invention has the beneficial effects that: (1) The carbon black masterbatch for nylon 6 civil filament fiber provided by the invention only adds a single type of carbon black super dispersant powder in the components, and simultaneously controls the comparative example among polyamide 6 chips, nano-grade carbon black powder and single type carbon black super dispersant powder, so that nano-grade carbon black powder can have high dispersibility in carrier polyamide 6 chips, and further obtains excellent spinnability; The addition of single carbon black super dispersant powder can ensure that there will be no intermittent strip breakage in the extrusion drawing process of the extrusion granulator, which can effectively improve the glossiness of the obtained masterbatch and make it have a bright black feeling with smooth surface.
(2) The carbon black masterbatch for nylon 6 civil filament fiber provided by the invention is preferably nano-grade carbon black powder of 25-30 nm. First of all, the particle size of carbon black largely determines the dispersibility of carbon black. The finer the carbon black particles, the higher the inherent specific surface area, and the higher the required "wetting" energy. Therefore, the finer the particles, the more difficult it is to disperse the carbon black than the coarse ionic carbon black. Secondly, when the particles are finer, the more the number of carbon black aggregates in a certain volume of carrier medium, the smaller the distance between aggregates, thus generating greater attraction between aggregates and inducing the agglomeration of carbon black. However, if the particle size is too large, it will seriously affect the blackness, resulting in the product can’t be used by spinning mills and downstream customers. 25-30 nm carbon black is preferred, which not only ensures the excellent dispersibility of carbon black in carrier resin, but also has excellent blackness value, and is widely accepted by spinning factories and downstream customers. Moreover, 25-30 nm nano-gradecarbon black is beneficial to solve the problems of uneven evenness and sharp increase of hairiness caused by spinning jitter caused by spinneret wear of masterbatch in the later stage of long-period spinning production.
(3) The carbon black masterbatch prepared by the method provided by the invention can be 50 1702 directly applied to the production of black nylon 6 civil filament fiber with good dyeing effect and continuous spinning production. The carbon black masterbatch prepared by the invention does not have large-scale agglomeration and enrichment on the filter screen of the spinning assembly, so the production cycle of the spinning assembly in the spinning process can be as high as 21-24 days, which 1s higher than the mainstream carbon black masterbatch currently on the market; Furthermore, it can effectively solve the problems of uneven evenness and sharp increase of wool fibers caused by spinning jitter caused by spinneret wear in the later stage of long-period spinning production of masterbatch, and provide a new material choice for continuous production of black nylon 6 civil filament fiber.
(4) In the preparation process of carbon black masterbatch, the melting and plasticizing process 1s divided into eleven temperature zones and a machine head temperature zone; The side feed of the equipment is set between the fifth and sixth temperature zones. Because the powder feed in the side feed is "cold material", it is necessary to heat the powder at multi-stage temperature to achieve better blending effect with polyamide 6 chips, increase the wettability of carbon black in polyamide 6 chips and improve the dispersion effect of carbon black.
BRIEF DESCRIPTION OF THE FIGURES Fig. 1 is a carbon black masterbatch prepared according to Example 1 of the present invention; Fig. 2 is a black nylon 6 civil filament fiber produced by carbon black masterbatch prepared according to Example 1 of the present invention; Fig. 3 1s a trend diagram of the pressure after the pump of the spinning assembly when the carbon black masterbatch prepared according to Example 1 of the present invention 1s used to produce black nylon 6 civil filament fiber.
DESCRIPTION OF THE INVENTION In order to make the content of the present invention easier to understand, the technical scheme of the present invention will be further explained below with reference to the specific embodiments and drawings, but the present invention 1s not limited to this.
The fiber-grade glossy polyamide 6 chips or semi-dull polyamide 6 chips in this invention are in granular form, all of which are purchased from Fujian Eversun Jinjiang Co., Ltd; Nano-grade carbon black powder is in powder form, purchased from Shanghai Cosme New
Materials Co., Ltd; CLIOSPERSES 330 single carbon black hyperdispersant is in powdetJ501702 form and purchased from Shanghai Heshuo International Trade Co., Ltd.
The invention relates to a carbon black masterbatch for nylon 6 civil filament fiber, which comprises the following components in percentage by weight: 57-79% of polyamide 6 chips, 20-40% of nano-grade carbon black powder and 1-3% of single carbon black super dispersant powder; The polyamide 6 chips are fiber-grade bright polyamide 6 chips or semi-dull polyamide 6 chips, and are granular; The particle size of the nano-grade carbon black powder is 25-30 nm; The single type carbon black hyperdispersant powder is CHHOSPERSE” 330, In the invention, polyamide 6 chips, nano-grade carbon black powder and single carbon black hyperdispersant powder are used as raw materials, and three components are mainly used, and excellent spinnability can be obtained without adding other additives, Among them, the nano-grade carbon black powder of 25-30 nm is preferred to solve the problems of uneven evenness and sharp increase of hairiness caused by spinning jitter caused by spinneret wear in the later stage of long-period spinning production. The addition of the single carbon black super dispersant powder can ensure that there will be no intermittent strip breakage in the extrusion drawing process of the extrusion granulator. In addition, by adding the single carbon black super dispersant powder, the glossiness of the obtained masterbatch can be effectively improved, so that it has a bright black feeling with smooth surface; According to the invention, the proportion of polyamide 6 chips, nano-grade carbon black powder and single carbon black super dispersant powder is strictly controlled, so that the nano-grade carbon black powder has high dispersibility in the carrier polyamide 6 resin; The prepared carbon black masterbatch can be directly applied to the production of black nylon 6 civil filament fiber dimension, with good dyeing effect and continuous spinning production, and the production cycle of spinning components can reach 21-24 days in the spinning process, which is higher than the current mainstream carbon black masterbatch on the market. Furthermore, it can effectively solve the problems of uneven evenness and sharp increase of wool fibers caused by spinning jitter caused by spinneret wear in the later stage of long-period spinning production of masterbatch, and provide a new material choice for continuous production of black nylon 6 civil filament fibers.
The invention relates to a preparation method of carbon black masterbatch for nylon 6 civil filament fiber, which specifically comprises the following steps:
The carbon black masterbatch for nylon 6 civil filament fiber 1s prepared by quantitatiye,. 1702 feeding, melting and plasticizing, screw transmission and shearing, water-cooling granulation, vibration screening and air-blast drying of polyamide 6 chips, nano-grade carbon black powder and single carbon black super dispersant powder in turn.
Further, the quantitative feeding is carried out through the linkage feeding mode of the main feeding position and the side feeding position, Adding polyamide 6 chips through the main feeding position, adding nano-grade carbon black powder and single carbon black hyperdispersant powder through the side feeding position; The feeding speed of the main feeding position and the side feeding position is 20-30 Hz.
Further, the melting and plasticizing process is divided into eleven temperature zones and a machine head temperature zone; The temperature control of each temperature zone is as follows: the first temperature zone is 200-215°C, the second temperature zone is 205-220°C, the third temperature zone is 210-225°C, the fourth, fifth and sixth temperature zones are 220-240°C, the seventh temperature zone is 200-215°C and the eighth temperature zone is 200-215°C.
Further, the rotating speed of the main machine for screw transmission and shearing is 600-825 r/min; The main rotating speed of the water-cooled granulator is 670-730 r/min.
Further, the diameter of the screen hole of the vibration screening is 1-6mm, preferably 1-3mm.
Furthermore, the water content of carbon black masterbatch for nylon 6 civil filament fiber obtained by air-blast drying is 400-450 ppm, the melt index is 4.5-12.9 g/10min, and the relative viscosity is 1.49-2.19.
The carbon black masterbatch prepared according to the preparation method of carbon black masterbatch for nylon 6 civil filament fiber is applied to nylon 6 civil filament fiber.
In the preparation method provided by the invention, each step and parameter in the preparation process are improved, wherein the melting plasticization is divided into eleven temperature zones and a die temperature zone, wherein the die temperature is 70 ‘C higher than the eleven temperature zones, and controlling the temperatures of the die and each temperature zone is beneficial to the high dispersion of carbon black; If the temperature of the die head is too low, it will cause the stay at the outlet of the screw extrusion head to twist and bend, and the discharge is extremely unsmooth. If the die head temperature is separately set at 250-260°C, the stay at the outlet of the screw extrusion head can be smoothly discharged without the phenomenon of strip breakage in the continuous production process, and the carbon black 501702 masterbatch can be stably prepared. At the same time, the temperature of the die should not be too high. On the one hand, too high a temperature will cause waste of energy consumption, on the other hand, it will cause too large temperature fluctuation, and the brace at the outlet of the screw extrusion head will appear large and small strips. The temperature from the seventh temperature zone to the eleventh temperature zone must be gradually decreased, which can ensure that the dispersant will not overheat due to too high temperature after the dispersant 1s fed in the side position, and ensure that the timeliness of the dispersant to soak the carbon black 1s longer, which is beneficial to the high dispersion of the carbon black; Through the above improvement, the final carbon black masterbatch can be used in spinning, which can effectively improve the breaking strength, elongation at break, evenness and other problems of the obtained black nylon 6 civil filament fiber. It can also effectively solve the problems of uneven evenness and sharp increase of wool fibers caused by spinning jitter caused by spinneret wear in the later stage of long-period spinning production of masterbatch, and improve product quality; At the same time, it can effectively improve the production cycle and continuous production of spinning components in the spinning process, and improve the production efficiency and economic benefits.
Example 1 The carbon black masterbatch for nylon 6 civil filament fiber comprises the following components in percentage by weight: 68. 0% of polyamide 6 chips, 30.0% of nano-grade carbon black powder and 2.0% of single carbon black super dispersant powder, and the carbon black masterbatch 1s shown in Fig. 1.
The preparation method of carbon black masterbatch for nylon 6 civil filament fiber specifically comprises the following steps: (1) Quantitative feeding: 68.0% fiber-grade glossy polyamide 6 chips with a particle size of 2 mm are weighed by weight loss and added to the main feeding position of the parallel co-rotating twin-screw extrusion granulator, and the feeding speed of the main feeding position is controlled to be 25 Hz; 30.0% of nano-grade carbon black powder with particle diameter of 25-30 nm and 2.0% of single carbon black hyperdispersant powder are added into the side feeding position of parallel co-rotating twin-screw extruder by weight loss, and the feeding speed of the side feeding position is controlled to be 25 Hz;
(2) Melting plasticization: Melting plasticization is divided into eleven temperature Zones,501702 and die temperature zones, and the temperature of each temperature zone is controlled as follows: the first temperature zone is 215°C; The second stage is 220°C; The third stage is 225°C; 230°C in the fourth, fifth and sixth stages; The seventh stage is 215°C; The eighth stage is 205°C; The ninth stage is 200°C; The tenth stage is 195°C; 185°C in the eleventh stage; Head 255°C; (3) Screw transmission and shearing: the rotating speed of the main machine for screw transmission and shearing is 700 r/min; (4) Water-cooled granulation: the main engine speed of the water-cooled granulation granulator is 700 r/min; (5) Vibration screening: the diameter of the screen hole of vibration screening is 3mm; (6) Air-blast drying: after air-blast drying, the final carbon black masterbatch for nylon 6 civil filament fiber is controlled to have a water content of 400-450 ppm, a melt index of 8.5%
0.5 g/10 min and a relative viscosity of 1.95=20.05.
Example 2 The carbon black masterbatch for nylon 6 civil filament fiber comprises the following components in percentage by weight: 62. 6% of polyamide 6 chips, 35.0% of nano-grade carbon black powder and 2.4% of single carbon black hyperdispersant powder.
The preparation method of carbon black masterbatch for nylon 6 civil filament fiber specifically comprises the following steps: (1) Quantitative feeding: 62. 6% fiber-grade glossy polyamide 6 chips with a particle size of 3mm are weighed by weight loss and added to the main feeding position of the parallel co-rotating twin-screw extrusion granulator, and the feeding speed of the main feeding position is controlled at 23 Hz; 35.0% of nano-grade carbon black powder with particle diameter of 25-30 nm and 2.0% of single carbon black hyperdispersant powder were added to the side feeding position of parallel co-rotating twin-screw extruder by weight loss, and the feeding speed of the side feeding position was controlled at 27 Hz; (2) Melting plasticization: Melting plasticization is divided into eleven temperature zones and die temperature zones, and the temperature of each temperature zone is controlled as follows: the first temperature zone is 215°C; The second stage is 220°C; The third stage is 225°C; 230°C in the fourth, fifth and sixth stages; The seventh stage is 215°C; The eighth stage is 205°C; The ninth stage is 200°C; The tenth stage is 195°C; 185°C in the eleventh stage; Head 255°C;
(3) Screw transmission and shearing: the rotating speed of the main machine for screw,501702 transmission and shearing is 650 r/min; (4) Water-cooled granulation: the main engine speed of the water-cooled granulation granulator is 685 r/min; (5) Vibration screening: the diameter of the screen hole of vibration screening is 3mm; (6) Air-blast drying: after air-blast drying, the final carbon black masterbatch for nylon 6 civil filament fiber is controlled to have a water content of 400-450 ppm, a melt index of 6.5%
0.5 g/10 min and a relative viscosity of 1.65=20.05.
Example 3 The carbon black masterbatch for nylon 6 civil filament fiber comprises the following components in percentage by weight: 73. 6% of polyamide 6 chips, 25.0% of nano-grade carbon black powder and 1.4% of single carbon black hyperdispersant powder.
The preparation method of carbon black masterbatch for nylon 6 civil filament fiber specifically comprises the following steps: (1) Quantitative feeding: 73. 6% fiber-grade glossy polyamide 6 chips with a particle size of 2mm are weighed by weight loss and added to the main feeding position of the parallel co-rotating twin-screw extrusion granulator, and the feeding speed of the main feeding position is controlled to be 27 Hz; 25. 0% of nano-grade carbon black powder with particle diameter of 25-30 nm and 1. 4% of single carbon black hyperdispersant powder were added to the side feeding position of parallel co-rotating twin-screw extruder by weight loss, and the feeding speed of the side feeding position was controlled at 23 Hz.
(2) Melting plasticization: Melting plasticization is divided into eleven temperature zones and die temperature zones, and the temperature of each temperature zone is controlled as follows: the first temperature zone is 215°C; The second stage is 220°C; The third stage is 225°C; 230°C in the fourth, fifth and sixth stages; The seventh stage is 215°C; The eighth stage is 205°C; The ninth stage is 200°C; The tenth stage is 195°C; 185°C in the eleventh stage; Head 255°C; (3) Screw transmission and shearing: the rotating speed of the main machine for screw transmission and shearing is 750 r/min; (4) Water-cooled granulation: the main engine speed of the water-cooled granulation granulator is 715 r/min; (5) Vibration screening: the diameter of the screen hole of vibration screening is 2mm;
(6) Air-blast drying: after air-blast drying, the final carbon black masterbatch for nylon R50 1702 civil filament fiber is controlled to have a water content of 400-450 ppm, a melt index of 11.0%
0.5 g/10 min and a relative viscosity of 2.05=20.05.
Example 4 The carbon black masterbatch for nylon 6 civil filament fiber comprises the following components in percentage by weight: 57. 0% of polyamide 6 chips, 40.0% of nano-grade carbon black powder and 3.0% of single carbon black hyperdispersant powder.
The preparation method of carbon black masterbatch for nylon 6 civil filament fiber specifically comprises the following steps: (1) Quantitative feeding: 57. 0% of fiber-grade glossy polyamide 6 chips with a particle size of 3mm are weighed by weight loss into the main feeding position of the parallel co-rotating twin-screw extruder, and the feeding speed of the main feeding position is controlled to be 20 Hz;
40. 0% of nano-grade carbon black powder with particle diameter of 25-30 nm and 3. 0% of single carbon black hyperdispersant powder are added to the side feeding position of parallel co-rotating twin-screw extruder by weight loss, and the feeding speed of the side feeding position is controlled at 30 Hz; (2) Melting plasticization: Melting plasticization is divided into eleven temperature zones and die temperature zones, and the temperature of each temperature zone is controlled as follows: the first temperature zone is 200°C; The second stage is 205°C; The third stage is 210°C; 220°C in the fourth, fifth and sixth stages; The seventh stage is 200°C; The eighth stage is 200°C; The ninth stage is 195°C; 190°C in the tenth stage; 180°C in the eleventh stage; Head 250°C; (3) Screw transmission and shearing: the rotating speed of the main machine for screw transmission and shearing is 600 r/min; (4) Water-cooled granulation: the rotating speed of the main machine of the water-cooled granulation granulator is 670 r/min; (5) Vibration screening: the diameter of the screen hole of vibration screening is 1mm; (6) Air-blast drying: after air-blast drying, the final carbon black masterbatch for nylon 6 civil filament fiber is controlled to have a water content of 400-450 ppm, a melt index of 4.5 +
0.5 g/10 min and a relative viscosity of 1.45=20.05.
Example 5 The carbon black masterbatch for nylon 6 civil filament fiber comprises the following components in percentage by weight: 79. 0% of polyamide 6 chips, 20.0% of nano-grade carbon 50 1702 black powder and 1.0% of single carbon black hyperdispersant powder.
The preparation method of carbon black masterbatch for nylon 6 civil filament fiber specifically comprises the following steps: (1) Quantitative feeding: 79. 0% of fiber-grade glossy polyamide 6 chips with a particle size of 3mm are weighed by weight loss into the main feeding position of the parallel co-rotating twin-screw extruder, and the feeding speed of the main feeding position is controlled at 30 Hz;
20. 0% of nano-grade carbon black powder with particle diameter of 25-30 nm and 1. 0% of single carbon black hyperdispersant powder were added to the side feeding position of parallel co-rotating twin-screw extruder by weight loss, and the feeding speed of the side feeding position was controlled at 20 Hz.
(2) Melting plasticization: Melting plasticization is divided into eleven temperature zones and die temperature zones, and the temperature of each temperature zone is controlled as follows: the first temperature zone is 217°C; The second stage is 210°C; The third stage is 215°C; 240°C in the fourth, fifth and sixth stages; The seventh stage is 210°C; The eighth stage is 215°C; The ninth stage is 205°C; The tenth stage is 200°C; 190°C in the eleventh stage; Head 260°C; (3) Screw transmission and shearing: the main engine speed of screw transmission and shearing is 825 r/min; (4) Water-cooled granulation: the main engine speed of the water-cooled granulation granulator is 730 r/min; (5) Vibration screening: the diameter of the screen hole of vibration screening is 3mm; (6) Air-blast drying: after air-blast drying, the final carbon black masterbatch for nylon 6 civil filament fiber is controlled to have a water content of 400-450 ppm, a melt index of 12.5%
0.5 g/10 min and a relative viscosity of 2.15=0.05.
Comparative example 1 The preparation method of carbon black masterbatch for nylon 6 civil filament fiber specifically comprises the following steps:
66. 0% fiber-grade glossy polyamide 6 chips with a particle size of 2mm are weighed by weight loss into the main feeding position of the parallel co-rotating twin-screw extrusion granulator, and the feeding speed of the main feeding position is controlled to be 25Hz; 30.0% of carbon black powder with a particle size of 25-30 nm and 4.0% of single carbon black hyperdispersant powder were added to the side feeding position of parallel co-rotating 59 1702 twin-screw extruder granulator by weight loss, and the feeding speed of the side feeding position was controlled at 25Hz.
Melt plasticizing: melt plasticizing is divided into eleven temperature zones and die temperature zones, and the temperature control of each temperature zone is the same as in Example 1.
Screw transmission and shearing: the main engine speed of screw transmission and shearing is the same as that of Example 1; Water-cooled granulation: the main engine speed of the water-cooled granulation granulator is the same as that of Example 1; Vibration screening: The diameter of the screen hole of vibration screening 1s the same as that of Example 1; Blow drying: the control of water content, melt index and relative viscosity of carbon black masterbatch for nylon 6 civil filament fiber is the same as that in Example 1.
During the preparation of the carbon black masterbatch mentioned above, high-frequency intermittent strip breakage will occur during the extrusion and drawing process, which will cause abnormal production and make it impossible to stably prepare the carbon black masterbatch.
Comparative example 2 The preparation method of carbon black masterbatch for nylon 6 civil filament fiber specifically comprises the following steps:
69. 5% fiber-grade glossy polyamide 6 chips with a particle size of 2mm are weighed by weight loss into the main feeding position of the parallel co-rotating twin-screw extrusion granulator, and the feeding speed of the main feeding position is controlled at 25Hz; 30.0% of nano-grade particles with the particle size of 25-30 nm Meter-grade carbon black powder and 0. 5% single carbon black super dispersant powder were weighed into the side feeding position of parallel co-rotating twin-screw extruder granulator by weight loss, and the feeding speed of the side feeding position was controlled at 25Hz.
Melting plasticizing: Melting plasticizing 1s divided into eleven temperature zones and die temperature zones, and the temperature control of each temperature zone is the same as in Example 1.
Screw transmission and shearing: the main engine speed of screw transmission and shearing, 1702 is the same as that of Example 1; Water-cooled granulation: the main engine speed of the water-cooled granulation granulator is the same as that of Example 1; Vibration screening: The diameter of the screen hole of vibration screening is the same as that of Example 1; Blow drying: the control of water content, melt index and relative viscosity of carbon black masterbatch for nylon 6 civil filament fiber is the same as that in Example 1.
During the preparation of the carbon black masterbatch mentioned above, high-frequency intermittent strip breakage will occur during the extrusion and drawing process, which will cause abnormal production and make it impossible to stably prepare the carbon black masterbatch.
Comparative example 3 The preparation method of carbon black masterbatch for nylon 6 civil filament fiber specifically comprises the following steps:
70. 0% fiber-grade bright polyamide 6 chips with a particle size of 2mm were weighed by weight loss and added with parallel co-rotating twin screws.
Rod extrudes the main feeding position of granulator, and the feeding speed of the main feeding position is controlled to be 25Hz; 30.0% carbon black powder with a particle size of 25-30 nm of nanometer level is added to the side feeding position of the parallel co-rotating twin-screw extruder granulator by weight loss, and the feeding speed of the side feeding position is controlled to be 25Hz; Melting plasticization: melting plasticization is divided into eleven temperature zones and die temperature zones, and the temperature control of each temperature zone is the same as in Example 1; Screw transmission and shearing: the main engine speed of screw transmission and shearing is the same as that of Example 1; Water-cooled granulation: the main engine speed of the water-cooled granulation granulator is the same as that of Example 1; Vibration screening: The diameter of the screen hole of vibration screening is the same as that of Example 1; Blow drying: water content, melt index and relative content of carbon black masterbatch for nylon 6 civil filament fiber. LU501702 The viscosity was controlled as in Example 1.
During the preparation of the carbon black masterbatch mentioned above, high-frequency intermittent strip breakage will occur during the extrusion and drawing process, which will cause abnormal production and make it impossible to stably prepare the carbon black masterbatch.
Performance test:
1. referring to fig. 1, it is a physical diagram of carbon black masterbatches prepared according to the method provided by the present invention, and the physical parameters of carbon black masterbatches prepared according to examples 1 to 5 are shown in table 1: Table 1 Physical parameters of carbon black masterbatch EE es No. content weight content Relative viscosity (%) (2) (ppm) (g/10min) |Example1| 30 | 13596 | 400 | 86 | 195 |
2. Apply carbon black masterbatch to spinning black nylon 6 civil filament fiber.
The carbon black masterbatches prepared according to Examples 1 to 5 of the present invention and Comparative Example 3 are directly used to spin black nylon 6 civil filament fibers (product specification: HOY BR 45D/12F, the base material used for spinning is glossy polyamide 6 chips), and the addition ratio of carbon black masterbatches, spinning component cycle and color discrimination M rate of hosiery of each practical example and comparative example are shown in Table 2. The physical properties of black nylon 6 civil filament fibers produced by carbon black masterbatch of each example and comparative example are shown in Table 3. The black nylon 6 civil filament fiber produced by the carbon black masterbatch of Example 1 is shown in Fig. 2. The spinning performance of black nylon 6 civil filament fiber produced by carbon black masterbatch in Example 1 is shown in Table 4 and Fig. 3. From the visual data in Fig. 3, the pressure of the solution after the pump rises slowly, and it can be seen that the dispersion of carbon black in the resin is very good, especially in the later period of use of the assembly, the pressure rises steadily, and the average daily pressure rises by 1.4bar in the so 1702 whole cycle, which shows that during the long-term spinning process, carbon black does not agglomerate and enrich on a large scale on the filter screen of the spinning assembly, so the service life of the spinning assembly is long, The carbon black masterbatch obtained in Comparative Example 1-2 is unstable and cannot be used for direct spinning black nylon 6 civil filament fiber; Table 2 Addition ratio of carbon black masterbatch, spinning component cycle and M rate of garter color judgment No.
Masterbatch addition | Component period | _ M-rate of color ratio (%) (day) judgment of garter belt 0 ample 4
Fxample 3
Example 3
Table 3 Physical properties of black nylon 6 civil filament fiber produced by carbon black LU501702 masterbatch C ; Exampl | Exampl | Exampl | Exampl | Exampl omparafl ve el e2 e3 e4 es example 3 5039 | 5035 | 5033 | 5039 | 5022 | 49.87 Fibre number Fracture strength
81.03 | 8151 | 8222 | 8192 | 8199 | 8158 Elongation at break £ venness | CV% | 068 | 072 | 078 | 077 | 08 | 078 | Boiling wate Hung water % 723 | 755 | 752 | 767 | 7.59 7.47 shrinkage re Front CORTE 03 03 03 03 03 03 shoulder point ss te point Rear conver 03 03 03 03 03 94 shoulder point
Table 4 Spinning performance of black nylon 6 civil filament fiber produced by carbon black, U50 1702 masterbatch Number of break (time) Number of Float (time) Cre [ss “ey [ao aw ao Cao “ew [a [0 ao [ww oo [ww [2 [0 10% day day Te 12T day pe) day eo day Te 15T day pi je 6% day Te 7 day 187 day M 19 day pa je day dy Te Pa oo] ay 24 day To “hes | ar ee | It can be seen from Table 2 that the life cycle of the carbon black masterbatch prepared according to the preparation methods of each example in the present invention in the spinning assembly is more than 21 days, up to 24 days at the highest, which is much higher than that of the mainstream imported carbon black masterbatch currently on the market, which is less than 15 days.
From Table 3, Table 4 and Fig. 3, it can be seen that the carbon black masterbatch prepared according to the preparation methods of each example of the present invention has excellent performance in the spinning process, and the daily average times of broken ends and floating filaments are far lower than 5.5 times and 3.5 times of the mainstream imported carbon black masterbatch currently on the market, which provides a new material choice for the continuoys, 59 1702 production of black nylon 6 civil filament fibers.
The above description is only an example of the present invention, and it does not limit the patent scope of the present invention. Any equivalent structure or equivalent process transformation made by using the content of the present invention, or directly or indirectly applied in other related technical fields, are equally included in the patent protection scope of the present invention.

Claims (10)

CLAIMS LU501702
1. A carbon black masterbatch for nylon 6 civil filament fiber, which is characterized by comprising the following components in percentage by weight: 57-79% of polyamide 6 chips, 20-40% of nano-grade carbon black powder and 1-3% of single carbon black hyperdispersant powder.
2. The carbon black masterbatch for nylon 6 civil filament fiber according to claim 1, which is characterized in that the polyamide 6 chips are fiber-grade bright polyamide 6 chips or semi-dull polyamide 6 chips, and are granular.
3. The carbon black masterbatch for nylon 6 civil filament fiber according to claim 1, which is characterized in that the particle size of the nano-grade carbon black powder is 25-30 nm.
4. The carbon black masterbatch for nylon 6 civil filament fiber according to claim 1, which is characterized in that the single type carbon black hyperdispersant powder is CLIOSPERSE” 20
5. A preparation method of carbon black masterbatch for nylon 6 civil filament fiber according to any one of claims 1-4, which is characterized by specifically comprising the following steps: polyamide 6 chips, nano-grade carbon black powder and single carbon black super dispersant powder were sequentially subjected to quantitative feeding, melting plasticization, screw transmission and shearing, water-cooling granulation, vibration screening and air drying to prepare carbon black master particles for nylon 6 civil filament fibers.
6. The preparation method of carbon black masterbatch for nylon 6 civil filament fiber according to claim 5, which is characterized in that the quantitative feeding is carried out through the linkage feeding mode of the main feeding position and the side feeding position; adding polyamide 6 chips through the main feeding position, adding nano-grade carbon black powder and single carbon black hyperdispersant powder through the side feeding position; the feeding speed of the main feeding position and the side feeding position is 20-30 Hz.
7. The preparation method of carbon black masterbatch for nylon 6 civil filament fiber according to claim 5, which is characterized in that the melting and plasticizing process is divided into eleven temperature zones and a machine head temperature zone; the temperature control of each temperature zone is as follows: the first temperature zone is 200-215°C, the second temperature zone is 205-220°C, the third temperature zone is 210-225°C, the fourth, fiffh, 501702 and sixth temperature zones are 220-240°C, the seventh temperature zone is 200-215°C, the eighth temperature zone is 200-215°C, and the ninth temperature zone is 195-205°C.
8. The preparation method of carbon black masterbatch for nylon 6 civil filament fiber according to claim 5, which is characterized in that the rotating speed of the main machine for screw transmission and shearing is 600-825 r/min; the main engine speed of the water-cooled granulator is 670-730 r/min.
9. The preparation method of carbon black masterbatch for nylon 6 civil filament fiber according to claim 5, which is characterized in that the moisture content of carbon black masterbatch for nylon 6 civil filament fiber after air-blast drying is 400-450 ppm, the melt index is 4.5-12.9 g/10 min, and the relative viscosity is 1.49-2.19.
10. An application of the carbon black masterbatch prepared according to the preparation method of the carbon black masterbatch for nylon 6 civil filament fiber in any one of claims 7-9 in nylon 6 civil filament fiber.
PATENTANSPRÜCHE LU501702
1. Fin RuB-Masterbatch für Nylon 6-Zivilfilamentfasern, das dadurch gekennzeichnet ist, dass es die folgenden Komponenten in Gewichtsprozent umfasst: 57-79% Polyamid 6-Chips, 20-40% nanoskaligen RuBpulver und 1-3% einfaches RuB-Superdispergiermittelspulver.
2. Das RuB-Masterbatch für Nylon 6-Zivilfilamentfasern nach Anspruch 1, das dadurch gekennzeichnet ist, dass die Polyamid 6-Chips Fiber-graduale helle Polyamid 6-Chips oder halbstumpfe Polyamid 6-Chips sind und kôrnig sind.
3. Das RuB-Masterbatch für Nylon 6-Zivilfilamentfasern nach Anspruch 1, das dadurch gekennzeichnet ist, dass die TeilchengrôBe des nanoskaligen RuBpulvers 25-30 nm beträgt.
4. Das RuB-Masterbatch für Nylon 6-Zivilfilamentfasern nach Anspruch 1, das dadurch gekennzeichnet ist, dass das einfache RuB3-Superdispergiermittelspulver CLIOSPERSE 35, ist.
5. Ein Verfahren zur Herstellung von RuB-Masterbatch für Nylon 6-Zivilfilamentfasern nach einem der Ansprüche 1 bis 4, das dadurch gekennzeichnet ist, dass es insbesondere die folgenden Schritte umfasst: Polyamid 6-Chips, nanoskaliges RuBpulver und einfaches Ruf3-Superdispermittelspulver wurden nacheinander einer quantitativen Beschickung, einer Schmelzplastifizierung, einer Schneckenübertragung und Scherung, einer Granulierung mit Wasserkühlung, einer Vibrationssiebung und einer Gebläsewindtrocknung unterzogen, um RuB-Masterbatch für Nylon 6-Zivilfilamentfasern herzustellen.
6. Das Verfahren zur Herstellung von RuB-Masterbatch für Nylon 6-Zivilfilamentfasern nach Anspruch 5, das dadurch gekennzeichnet ist, dass die quantitative Beschickung durch den Kopplungsbeschickungsmodus der Hauptbeschickungsposition und der Seitenbeschickungsposition durchgeführt wird; Zugabe von Polyamid 6-Chips durch die Hauptbeschickungposition, Zugabe von nanoskaligem RuBpulver und einfachem RuB-Hyperdispermittelspulver durch die Seitenbeschickungsposition; die Beschickungsgeschwindigkeit der Haupt- und Seitenbeschickungsposition betragt 20-30 Hz.
7. Das Verfahren zur Herstellung von RuB-Masterbatch für Nylon 6-Zivilfilamentfasern nach Anspruch 5, das dadurch gekennzeichnet ist, dass der Schmelz- und Plastifizierungsprozess in elf Temperaturzonen und eine Maschinenkopf-Temperaturzone unterteilt ist; die
Temperaturregelung jeder Temperaturzone ist wie folgt: die erste Temperaturzone beträgt 50 1702 200-215°C, die zweite Temperaturzone beträgt 205-220°C, die dritte Temperaturzone beträgt 210-225°C, die vierte, die fünfte und die sechste Temperaturzonen betragen 220-240°C, die siebte Temperaturzone beträgt 200-215‘C, die achte Temperaturzone beträgt 200-215°C und die neunte Temperaturzone beträgt 195-205°C.
8. Das Verfahren zur Herstellung von RuB-Masterbatch für Nylon 6-Zivilfilamentfasern nach Anspruch 5, das dadurch gekennzeichnet ist, dass die Drehgeschwindigkeit der Hauptmaschine für Schneckenübertragung und Scherung 600-825 U/min beträgt; die Hauptmotordrehzahl des Granulators mit Wasserkühlung 670-730 U/min beträgt.
9. Das Verfahren zur Herstellung von RuB-Masterbatch für Nylon 6-Zivilfilamentfasern nach Anspruch 5, das dadurch gekennzeichnet ist, dass der Feuchtigkeitsgehalt von RuB-Masterbatch für Nylon 6-Zivilfilamentfasern nach dem Gebläsewindtrocknung 400-450 ppm beträgt, der Schmelzindex 4,5-12,9 g/10 min beträgt und die relative Viskosität 1,49-2,19 beträgt.
10. Eine Anwendung des RuB-Masterbatches, hergestellt nach dem Herstellungsverfahren des RuB-Masterbatches für Nylon 6-Zivilfilamentfasern in einem der Anspriiche 7 bis 9, in Nylon 6-Zivilfilamentfasern.
LU501702A 2022-03-23 2022-03-23 Carbon Black Masterbatch for Nylon 6 Civil Filament Fiber, Preparation and Application Thereof LU501702B1 (fr)

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