CN107541805B - Graphene in-situ polymerization modified polyamide 6 pre-oriented yarn and preparation method thereof - Google Patents
Graphene in-situ polymerization modified polyamide 6 pre-oriented yarn and preparation method thereof Download PDFInfo
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Abstract
The invention provides a graphene in-situ polymerization modified polyamide 6 pre-oriented yarn and a preparation method thereof, wherein the preparation method comprises the following steps: carrying out melt spinning on the graphene in-situ polymerization modified polyamide 6 slice, and cooling to obtain pre-oriented yarn; wherein the winding speed of the spinning is 3500-4500 m/min. The preparation method of the graphene in-situ polymerization modified polyamide 6 pre-oriented yarn provided by the application adopts specific spinning parameters, and has the advantages of convenience, simplicity, easiness in operation and the like. The graphene in-situ polymerization modified polyamide 6 pre-oriented yarn provided by the application can be further subjected to post-treatment, the conventional treatment process is drawing deformation to form a drawing deformation yarn, the drawing strength of the pre-oriented yarn is 4.30-4.45 dN/dTex, the elongation is 35% -45%, and the application prospect is wide.
Description
Technical Field
The invention relates to the technical field of material preparation, in particular to graphene in-situ polymerization modified polyamide 6 pre-oriented yarn and a preparation method thereof.
Background
The polyamide fiber is a synthetic fiber spun by a polymer with a molecular main chain containing an amide group (-CONH). Polyamide 6 (polycaprolactam, PA6) is generally obtained industrially by ring-opening polycondensation of caprolactam.
The polyamide fiber has the advantages of excellent performance, good wear resistance, higher breaking strength, excellent rebound resilience and fatigue resistance, lower hygroscopicity than natural fiber and regenerated fiber, and good dyeing performance. The disadvantage is poor light resistance and reduced intensity under long-term sunlight and ultraviolet lamp irradiation. Because the polyamide fiber has a plurality of excellent properties, the polyamide fiber is widely applied in the fields of civil use, industry and the like, for example, the polyamide fiber is mainly used for manufacturing socks, underwear, shirts, sport shirts and the like in the aspect of clothes, and can be blended with fibers such as cotton, wool, viscose and the like, the blended fabric has good wear resistance, and the polyamide fiber can also be used for manufacturing bedding, outdoor ornaments and cloth for furniture; the method is mainly used for manufacturing tire cord fabrics, conveyor belts, conveyer belts, fishing nets, ropes and the like in the industry, and relates to the fields of transportation, fishery, military industry and the like.
Graphene (Graphene) is a honeycomb-shaped planar thin film formed by carbon atoms in an sp2 hybridization mode, is a quasi-two-dimensional material with the thickness of only one atomic layer, and has the characteristics of high strength and toughness. The theoretical tensile strength and the elastic modulus of the single-layer graphene are 125GPa and 1.1TPa respectively, and the Young modulus is about 42N/m2Therefore, the graphene has obvious reinforcing and toughening effects on the high polymer material. Meanwhile, one of the most important properties of graphene is its unique carrier characteristics and mass-free dirac fermi properties. Its electron mobility can reach 2X 105cm2The electron mobility in silicon is about 140 times that in gallium arsenide, the temperature stability is high, and the conductivity can reach 108Omega/m, and a sheet resistance of about 31 omega/sq (310 omega/m)2) Lower than copper or silver, is the best material to conduct electricity at room temperature.The graphene has large specific surface area (2630 m)2G), thermal conductivity (5000 W.m at room temperature)-1·K-1) 36 times that of silicon, 20 times that of gallium arsenide, and copper (401 W.m at room temperature)-1·K-1) More than ten times. Therefore, the graphene polymer composite material has excellent antistatic and heat-conducting properties.
Chinese patents "batch-type production equipment and preparation method of graphene composite" (CN2017102227140) and "continuous production equipment and preparation method of graphene composite" (CN2017102227155) respectively report different production equipment and preparation methods of graphene in-situ polymerization modified PA 6. The functional graphene in-situ polymerization modified PA6 has good characteristics of reinforcement, toughening, antibiosis, bacteriostasis and ultraviolet resistance, and provides a raw material basis for manufacturing the functional PA6 fiber.
Conventional PA6, crystallization temperature about 160 ℃; the functional graphene in-situ polymerization modified PA6 has a crystallization temperature which is changed to about 190 ℃. Conventional PA6, material thermal conductivity 0.25 W.m-1·K-1The thermal conductivity coefficient of the graphene in-situ polymerization modified PA6 (graphene content is 0.1 wt%) is converted into 0.48 W.m-1·K-1. The change of the thermal property of the material has great influence on the spinning process.
In view of the above, the present invention is particularly proposed.
Disclosure of Invention
The first purpose of the invention is to provide a preparation method of graphene in-situ polymerization modified polyamide 6 pre-oriented yarn, which adopts specific spinning parameters aiming at the material and has the advantages of convenience, simplicity, easy operation and the like.
The second purpose of the invention is to provide the graphene in-situ polymerization modified polyamide 6 pre-oriented yarn prepared by the preparation method of the graphene in-situ polymerization modified polyamide 6 pre-oriented yarn, the pre-oriented yarn can be further post-processed, the conventional processing technology is drawing deformation to form a drawing deformation yarn, the drawing strength of the pre-oriented yarn is 4.30-4.45 dN/dTex, the elongation is 35% -45%, and the application prospect is wide.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
a preparation method of graphene in-situ polymerization modified polyamide 6 pre-oriented yarn comprises the following steps:
carrying out melt spinning on the graphene in-situ polymerization modified polyamide 6 slice, and cooling to obtain pre-oriented yarn;
wherein the winding speed of the spinning is 3500-4500 m/min; preferably, the winding speed is 3700 to 4300 m/min.
Preferably, in the spinning process, the screw temperature is 270-276 ℃, the spinning box temperature is 270-280 ℃, and the spinning box pressure is 130-200 bar.
Preferably, the cooling temperature is 30-60 ℃, the humidity is 85-95%, and the wind speed is 0.18-0.25 m/s.
Preferably, the cooling is performed by a cross-blow or a circular-blow operation.
Preferably, the device of cross-blowing comprises a spinneret plate, a heating plate and a blowing plate, wherein the spinneret plate is horizontally arranged, and the heating plate and the blowing plate are arranged on one side of the spinneret plate in parallel and are perpendicular to the spinneret plate.
Preferably, an upper oil level is arranged at a position 600-800 mm below the spinneret plate, and the amount of the upper oil is controlled to be 0.5-2%.
Preferably, the height of the heating plate is 25-60% of the total height of the side blowing device, and the rest part of the heating plate is hollow.
Preferably, the relative viscosity of the graphene in-situ polymerization modified polyamide 6 slice is 2.45-2.75, the water content is less than 0.04 wt%, and the graphene content is 0.05-0.7 wt%.
Preferably, the stretching is performed at a high speed by matching a tension roller with a winding head.
The graphene in-situ polymerization modified polyamide 6 pre-oriented yarn prepared by the preparation method of the graphene in-situ polymerization modified polyamide 6 pre-oriented yarn.
Compared with the prior art, the invention has the beneficial effects that:
(1) the preparation method of the graphene in-situ polymerization modified polyamide 6 pre-oriented yarn provided by the application adopts specific spinning parameters, and has the advantages of convenience, simplicity, easiness in operation and the like.
(2) The graphene in-situ polymerization modified polyamide 6 pre-oriented yarn provided by the application can be further subjected to post-treatment, the conventional treatment process is drawing deformation to form a drawing deformation yarn, the drawing strength of the pre-oriented yarn is 4.30-4.45 dN/dTex, the elongation is 35% -45%, and the application prospect is wide.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are some embodiments of the present invention, and other drawings can be obtained by those skilled in the art without creative efforts.
Fig. 1 is a front view of a three-view device of a side blowing device according to an embodiment of the present invention;
fig. 2 is a left side view of a three-view device of a side blowing device according to an embodiment of the present invention;
fig. 3 is a top view of a three-view device of a side blowing device according to an embodiment of the present invention.
Reference numerals:
1-a blowing plate; 2-heating the plate; 3-spinneret plate.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below with reference to the accompanying drawings and the detailed description, but those skilled in the art will understand that the following described embodiments are some, not all, of the embodiments of the present invention, and are only used for illustrating the present invention, and should not be construed as limiting the scope of the present invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention. The examples, in which specific conditions are not specified, were conducted under conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are not indicated by the manufacturer, and are all conventional products available commercially.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplicity of description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
In the description of the present invention, it should be noted that, unless otherwise explicitly specified or limited, the terms "mounted," "connected," and "connected" are to be construed broadly, e.g., as meaning either a fixed connection, a removable connection, or an integral connection; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The specific meanings of the above terms in the present invention can be understood in specific cases to those skilled in the art.
A preparation method of graphene in-situ polymerization modified polyamide 6 pre-oriented yarn comprises the following steps:
carrying out melt spinning on the graphene in-situ polymerization modified polyamide 6 slice, and cooling to obtain pre-oriented yarn;
wherein the winding speed of the spinning is 3500-4500 m/min; preferably, the winding speed is 3700 to 4300 m/min.
The PA6 melt spinning process is mainly as follows: melting the polyamide polymer; pressurizing the melt by a specific device, extruding the melt from a spinneret plate 3 to form melt trickle, cooling and solidifying to form nascent fiber; then winding the fiber on a yarn receiving mechanism. To meet the performance requirements of the finished fiber, the nascent fiber needs further post-treatment steps of stretching, sizing, deforming and the like. In the actual production process, the series of post-treatments can occur before the primary fiber winding (i.e. one-step method) or after the primary fiber winding (i.e. two-step method).
When the polyamide is melted and spun, the temperature control, the spinning speed and the stretching ratio all have obvious influence on the fiber forming. When the spinning speed is more than 4000m/min, the orientation degree and the crystallinity degree of the fiber are improved, and the anisotropic expansion of the fiber is obviously reduced, so that better bobbin forming is obtained, and at the moment, pre-oriented yarn (POY) is obtained. The POY fiber can be further post-processed, and the common processing technology is drawing deformation, namely drawing deformation yarn (DTY).
The preparation method of the graphene in-situ polymerization modified polyamide 6 pre-oriented yarn provided by the application adopts specific spinning parameters, and has the advantages of convenience, simplicity, easiness in operation and the like. Due to the good antistatic property of the graphene in-situ polymerization modified PA6, in the POY fiber spinning process, a textile auxiliary with antistatic property does not need to be added. Other chemical fiber oil agents for spinning are used according to the requirements of the common PA6 spinning process.
Preferably, in the spinning process, the screw temperature is 270-276 ℃, the spinning box temperature is 270-280 ℃, and the spinning box pressure is 130-200 bar.
Preferably, the cooling temperature is 30-60 ℃, the humidity is 85-95%, and the wind speed is 0.18-0.25 m/s.
Preferably, the cooling is performed by a cross-blow or a circular-blow operation.
In order to delay the crystallization speed of the graphene in-situ polymerization modified PA6, the temperature of the fiber cooling device needs to be adjusted to 30-60 ℃ by side blowing or circular blowing, the humidity is 85% -95%, and the wind speed is 0.18-0.25 m/s.
Preferably, the device of cross-blowing includes spinneret 3, hot plate 2 and blowing board 1, spinneret 3 is placed horizontally, hot plate 2 with blowing board 1 parallel arrangement in one side of spinneret 3, with spinneret 3 is perpendicular.
Preferably, the height of the metal baffle is 25-60% of the total height of the side-blowing cooling device, and the rest part of the metal baffle is hollow.
In order to further adjust the fiber cooling speed, the height of the metal baffle is 25-60% of the total height of the side-blowing cooling device, and the rest part is still hollow.
Preferably, the relative viscosity of the graphene in-situ polymerization modified polyamide 6 slice is 2.45-2.75, the water content is less than 0.04 wt%, and the graphene content is 0.05-0.7 wt%.
Preferably, the stretching is performed at a high speed by matching a tension roller with a winding head.
Preferably, the position 600 mm-800 mm below the spinneret plate 3 is used as an oil applying position, and the oil applying amount is controlled to be 0.5% -2%.
The graphene in-situ polymerization modified polyamide 6 pre-oriented yarn prepared by the preparation method of the graphene in-situ polymerization modified polyamide 6 pre-oriented yarn.
Example 1
The spinning in-situ polymerized graphene modified PA6 chip has the relative viscosity of 2.72, the water content of the chip is 0.02 wt%, and the graphene content is 0.05 wt%.
The position 600mm below the spinneret plate 3 is the upper oil level, and the upper oil level is controlled to be 2%.
Example 2
The spinning in-situ polymerized graphene modified PA6 slice has the relative viscosity of 2.65, the water content of the slice is 0.03 wt%, and the graphene content is 0.1 wt%.
The position 650mm below the spinneret plate 3 is the upper oil level, and the upper oil level is controlled to be 1.2%.
Example 3
The spinning in-situ polymerized graphene modified PA6 slice has the relative viscosity of 2.65, the water content of the slice is 0.03 wt%, and the graphene content is 0.3 wt%.
The position 700mm below the spinneret plate 3 is used as an upper oil level, and the upper oil level is controlled to be 0.8%.
Example 4
The in-situ polymerized graphene modified PA6 chip for spinning has the relative viscosity of 2.45, the water content of the chip is 0.02 wt%, and the graphene content is 0.7 wt%.
The part 800mm below the spinneret plate 3 is used as an upper oil level, and the upper oil level is controlled to be 0.5 percent.
The comparative example is substantially the same as example 1 except that the spinning speed is 4000 m/min.
Experimental examples tensile Strength and elongation testing
The graphene in-situ polymerization modified PA6 pre-oriented yarns provided in examples 1-4 and comparative examples of the present application were subjected to tensile strength and elongation tests, and the test results are shown in Table 1.
TABLE 1 tensile Strength and elongation test results
| Serial number | Tensile Strength (dN/dTex) | Elongation (%) |
| Example 1 | 4.31 | 43 |
| Example 2 | 4.38 | 40 |
| Example 3 | 4.30 | 45 |
| Example 4 | 4.45 | 35 |
| Comparative example | 4.33 | 42 |
Experimental results show that the graphene in-situ polymerization modified PA6 pre-oriented yarn provided by the application has good performance, the tensile strength is 4.30-4.45 dN/dTex, the elongation is 35% -45%, the pre-oriented yarn can be further post-processed, and the conventional processing technology is tensile deformation and becomes tensile deformation yarn. The comparative examples show that the spinning speed has a significant influence on the properties of the pre-oriented yarn.
In summary, the preparation method of the graphene in-situ polymerization modified polyamide 6 pre-oriented yarn provided by the application adopts specific spinning parameters, and has the advantages of convenience, simplicity, easiness in operation and the like. The graphene in-situ polymerization modified polyamide 6 pre-oriented yarn provided by the application can be further subjected to post-treatment, the conventional treatment process is drawing deformation to form a drawing deformation yarn, the drawing strength of the pre-oriented yarn is 4.30-4.45 dN/dTex, the elongation is 35% -45%, and the application prospect is wide.
While particular embodiments of the present invention have been illustrated and described, it will be appreciated that the above embodiments are merely illustrative of the technical solution of the present invention and are not restrictive; those of ordinary skill in the art will understand that: modifications may be made to the above-described embodiments, or equivalents may be substituted for some or all of the features thereof without departing from the spirit and scope of the present invention; the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention; it is therefore intended to cover in the appended claims all such alternatives and modifications that are within the scope of the invention.
Claims (3)
1. A preparation method of graphene in-situ polymerization modified polyamide 6 pre-oriented yarn is characterized by comprising the following steps:
carrying out melt spinning on the graphene in-situ polymerization modified polyamide 6 slice, and cooling to obtain pre-oriented yarn;
wherein the winding speed of the spinning is 3700-4300 m/min;
in the spinning process, the temperature of a screw is 270-276 ℃, the temperature of a spinning box is 270-280 ℃, and the pressure of the spinning box is 130-200 bar;
the cooling temperature is 30-60 ℃, the humidity is 85% -95%, and the wind speed is 0.18-0.25 m/s;
the relative viscosity of the graphene in-situ polymerization modified polyamide 6 slice is 2.45-2.75, the water content is less than 0.04 wt%, and the graphene content is 0.05-0.7 wt%;
the cooling is performed by adopting side blowing or circular blowing;
the side blowing device comprises a spinneret plate, a heating plate and a blowing plate, wherein the spinneret plate is horizontally arranged, and the heating plate and the blowing plate are arranged on one side of the spinneret plate in parallel and are perpendicular to the spinneret plate;
setting an upper oil level at a position 600-800 mm below the spinneret plate, wherein the upper oil level is controlled to be 0.5-2%;
the height of the heating plate is 25-60% of the total height of the side blowing device, and the rest part of the heating plate is hollow.
2. The method for preparing the graphene in-situ polymerization modified polyamide 6 pre-oriented yarn according to claim 1, wherein the stretching is performed at a high speed by matching a tension roller with a winding head.
3. The graphene in-situ polymerization modified polyamide 6 pre-oriented yarn prepared by the preparation method of the graphene in-situ polymerization modified polyamide 6 pre-oriented yarn according to claim 1 or 2.
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| CN112851958A (en) * | 2020-12-31 | 2021-05-28 | 常州恒利宝纳米新材料科技有限公司 | Graphene in-situ polymerization semi-aromatic polyamide and preparation method thereof |
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