TW202317825A - Aromatic polyester fiber and manufacturing method thereof - Google Patents

Abstract

An aromatic polyester fiber and manufacturing method thereof are provided. The manufacturing method includes the following steps. The aromatic polyester resin is heated and melted. During a spinning process, a yarn is passed through a slow cooling zone at the end of a spinning nozzle. After an oiling agent and a pair of rollers, the yarn is wound on a paper tube. Afterwards, the yarn is rewound on a metal tube, and the oiling agent is applied during the rewinding. Next, a temperature is gradually increased in four stages, and the yarn is subjected to a heat treatment process. Finally, the heat-treated yarn is rewound on a paper tube.

Description

Aromatic polyester fiber and its production method

The present invention relates to a fiber and its manufacturing method, and in particular to an aromatic polyester fiber and its manufacturing method.

In the prior art, aromatic polyester fibers are mainly produced by melt spinning and heat treatment procedures. However, aromatic polyester is a directional molecule. After the fiber is heat-treated, it is easy to cause fibrillation and sticking between fibers, which in turn leads to peeling and fluffing between fibers.

Based on the above, developing a method for producing aromatic polyester fibers to improve the sticking phenomenon between fibers and make the production of aromatic polyester fibers easier to achieve is an important subject of current research.

The invention provides an aromatic polyester fiber and a manufacturing method thereof, which can effectively improve the sticking phenomenon between fibers and make the production of the aromatic polyester fiber easier to achieve.

The production method of the aromatic polyester fiber of the present invention comprises the following steps. The aromatic polyester resin is heated and melted. In the spinning process, the yarn passes through the slow cooling zone set at the end of the spinneret, and after passing through the oiling agent and a pair of rollers, the yarn is wound on the paper tube. Afterwards, the yarn is rewound on a metal tube, and a finish is applied during rewinding. Next, the temperature is gradually raised in four stages, and the yarn is subjected to a heat treatment process. Finally, the heat-treated yarn is rewound on a paper tube.

In an embodiment of the present invention, the temperature of the heating and melting process is 280°C to 320°C.

In an embodiment of the present invention, the temperature of the slow cooling zone is 280°C to 320°C.

In an embodiment of the present invention, the length of the slow cooling zone is 10 mm to 110 mm.

In an embodiment of the present invention, the oiling agent includes polysiloxane oiling agent.

In one embodiment of the present invention, the rewinding tension for rewinding the yarn on the metal tube is 0 to 10 cN.

In an embodiment of the present invention, the temperature is gradually raised in four stages from 220°C to 320°C.

In one embodiment of the present invention, the gradual temperature increase in four stages includes: the first stage, treatment at a temperature of 240°C for 3 hours; the second stage, treatment at a temperature of 265°C for 14 hours; the third stage, treatment at a temperature of 280°C 7 hours; and the fourth stage, treating at a temperature of 300°C for 7 hours.

In an embodiment of the present invention, the time of the heat treatment process is 0.5 hours to 50 hours.

In an embodiment of the present invention, the material of the metal pipe includes iron, copper, aluminum or stainless steel.

The aromatic polyester fiber of the present invention is made by the above-mentioned manufacturing method of the aromatic polyester fiber, the fiber strength of the aromatic polyester fiber is 20 g/d to 25 g/d, and the elongation is 1% to 4%.

Based on the above, the present invention provides an aromatic polyester fiber and a manufacturing method thereof. A slow cooling zone is provided at the end of the spinning end to make the production of the aromatic polyester fiber easier to achieve. In addition, low tension is used for rewinding, and oiling agent is applied during rewinding to greatly improve the sticking phenomenon after heat treatment. On the other hand, through the four-stage gradually heating technology, the fiber strength and elongation can be effectively improved to achieve the effect of optimizing physical properties.

Hereinafter, embodiments of the present invention will be described in detail. However, these embodiments are illustrative, and the present disclosure is not limited thereto.

Herein, a range indicated by "one value to another value" is a general representation which avoids enumerating all values in the range in the specification. Therefore, the description of a specific numerical range covers any numerical value in the numerical range and the smaller numerical range defined by any numerical value in the numerical range, as if the arbitrary numerical value and the smaller numerical range are written in the specification. The value range is the same.

The invention provides a method for producing aromatic polyester fibers, which includes the following steps. The aromatic polyester resin is heated and melted. In the spinning process, the yarn passes through the slow cooling zone set at the end of the spinneret, and after passing through the oiling agent and a pair of rollers, the yarn is wound on the paper tube. Afterwards, the yarn is rewound on a metal tube, and a finish is applied during rewinding. Next, the temperature is gradually raised in four stages, and the yarn is subjected to a heat treatment process. Finally, the heat-treated yarn is rewound on a paper tube.

In this embodiment, the temperature of the heating and melting process is, for example, 280° C. to 320° C. The temperature of the slow cooling zone is, for example, 280° C. to 320° C., and the length of the slow cooling zone is, for example, 10 mm to 110 mm, preferably 70 mm. Due to the directionality of aromatic polyester molecules, during the spinning process, after the yarn passes through the spinning port, if the temperature difference is large, the fiber will be cooled rapidly. The invention sets a slow cooling zone at the end of the spinning mouth, which can make the production of the aromatic polyester fiber easier to achieve and improve the spinnability.

In this embodiment, the oiling agent may include polysiloxane oiling agent. The material of the metal tube may include iron, copper, aluminum or stainless steel. The rewinding tension of the yarn on the metal tube is, for example, 0 to 10 cN, preferably 0 to 3 cN. By adopting low-tension rewinding and applying oiling agent during rewinding, the sticking phenomenon of yarn after heat treatment can be greatly improved.

In this embodiment, different from the two-stage temperature raising technology adopted in the conventional technology, four-stage warming treatment conditions are adopted. In more detail, the temperature can be raised gradually from 220°C to 320°C in four stages. For example, it can include: the first stage, treating at 240°C for 3 hours; the second stage, treating at 265°C for 14 hours; the third stage, Treat at a temperature of 280°C for 7 hours; and the fourth stage, treat at a temperature of 300°C for 7 hours. The time of the heat treatment process is about 0.5 hour to 50 hours. Through this four-stage heating technology, the fiber strength and elongation can be effectively improved to achieve the effect of optimizing physical properties. The aromatic polyester fiber produced by the method for producing aromatic polyester fiber of the present invention has a fiber strength of, for example, 20 g/d to 25 g/d, and an elongation of, for example, 1% to 4%.

Hereinafter, the above-mentioned aromatic polyester fiber proposed by the present invention and its manufacturing method will be described in detail by using experimental examples. However, the following experimental examples are not intended to limit the present invention. Experimental example

In order to prove that the aromatic polyester fiber and its manufacturing method proposed by the present invention can effectively improve fiber strength and elongation, and achieve the effect of optimizing physical properties, the following is a special example of this experiment. Preparation of aromatic polyester fiber spinning

The present invention selects Ueno Chemical LCP liquid crystal resin raw material A series, the intrinsic viscosity of the resin is 5 dL/g to 7 dL/g, the melting point temperature is 280°C to 320°C, the resin is dried at 120°C for 8 hours, and the spinneret is long Diameter ratio L/D=2 to 4, a slow cooling zone is set under the spinneret, the length of the slow cooling zone is 10 mm to 110 mm, the temperature of the slow cooling zone is between 280°C and 320°C, and the slow cooling zone is set after the slow cooling zone The yarn is cooled in the side blowing area, the yarn is oiled through the oil nozzle, and then wound by the take-up wheel (GR1, GR2), and then wound by the winding machine, the winding speed of the winding machine is 2,000 m/min to 1,500 m/min . Rewind

The primary fiber is rewound on the metal tube with a low tension < 10cN, preferably below 3cN, through the rewinding machine, and is coated with anti-sticking oil during the rewinding process. The anti-sticking oil here The oil agent contains polysiloxane oil agent, which can avoid the solid state polymerization of the yarn due to the long-term high-temperature process, which will cause the fiber to melt and stick, which will affect the subsequent yarn unwinding. solid state polymerization

In order to improve the strength of the as-spun fiber, after the as-spun fiber is rewound into a metal tube, put it into a nitrogen oven, use 30NL/min to feed it for 30min to 1h, and raise the temperature in stages. The temperature is preferably the yarn melting point temperature Tm-40℃ to Tm -60°C, as the solid-state polymerization time increases, gradually increase the solid-state polymerization temperature, the highest temperature does not exceed 320°C, the solid-state polymerization time, in order to increase the molecular weight of the fiber, that is, the strength and elongation, the maximum temperature is more than 3 hours, more preferably More than 10 hours. In addition, with the increase of temperature and time, the strength and elongation will slow down with the solid-state polymerization reaction, and reach a certain range. In consideration of productivity, the best time for solid-state polymerization is less than 50 hours. After solid-state polymerization, cool down naturally and take it out. yarn. Example 1

In order to adopt the above-mentioned yarn production method, the yarn has not been solid-state polymerized, the as-spun fiber strength is 9.6g/d, and the elongation is 1.8%. Example 2

Using the fiber of Example 1, the yarn undergoes solid state polymerization at 240°C for 3h→265°C for 21h, the fiber strength is 18g/d, and the elongation is 2.99%. Example 3

Using the fiber of Example 1, the yarn undergoes solid state polymerization at 240°C for 3h→265°C for 14h→280°C for 7h, the fiber strength is 21g/d, and the elongation is 3.49%. Example 4

Using the fiber of Example 1, the yarn undergoes solid state polymerization at 240°C for 3h→265°C for 14h→280°C for 7h→300°C for 7h, the fiber strength is 25.3g/d, and the elongation is 3.82%. Example 5

Using the fiber of Example 1, the yarn undergoes solid state polymerization at 240°C for 3h→265°C for 14h→280°C for 7h→310°C for 12h, the fiber strength is 22.4g/d, and the elongation is 3.62%. Table 1 Results of solid state polymerization test of LCP yarn project Example 1 Example 2 Example 3 Example 4 Example 5 number of lines twenty four twenty four twenty four twenty four twenty four Danny number 200 200 200 200 200 Fineness 8.3 8.3 8.3 8.3 8.3 Strength (g/d) 9.6 18.0 21.0 25.3 22.4 Elongation (%) 1.88 2.99 3.49 3.82 3.62 Solidification conditions -- 240℃3h→265℃21h 240℃3h→265℃14h→280℃7h 240℃3h→265℃14h→280℃7h→300℃7h 240℃3h→265℃14h→280℃7h→310℃12h

It can be seen from the above Table 1 that the strength of the as-spun fibers increased from 9.6 to 18.0 g/d, and the elongation increased from 1.88 to 2.99% after two-stage heating (reference example 2). The as-spun fiber was heated in three stages (reference example 3), the strength increased from 9.6 to 21.0 g/d, and the elongation increased from 1.88 to 3.49%. The as-spun fiber was heated in four stages (reference example 4), the strength increased from 9.6 to 25.3g/d, and the elongation increased from 1.88 to 3.82%. The as-spun fibers were heated up in four stages (reference example 5), the strength increased from 9.6 to 22.4g/d, and the elongation increased from 1.88 to 3.62%. However, because the temperature in the fourth stage is too high, the solidification effect is worse than that of Example 4, that is, the strength and elongation are slightly lowered.

To sum up, the present invention provides an aromatic polyester fiber and a manufacturing method thereof. A slow cooling zone is provided at the end of the spinneret, so that the production of the aromatic polyester fiber is easier to achieve and the spinnability is improved. In addition, low tension is used for rewinding, and oiling agent is applied during rewinding to greatly improve the sticking phenomenon after heat treatment. On the other hand, through the four-stage gradually heating technology, the fiber strength and elongation can be effectively improved to achieve the effect of optimizing physical properties. The aromatic polyester fiber produced by the method for producing aromatic polyester fiber of the present invention has a fiber strength of, for example, 20 g/d to 25 g/d, and an elongation of, for example, 1% to 4%.

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Claims (11)

A method for producing aromatic polyester fibers, comprising: The aromatic polyester resin is heated and melted. In the spinning process, the yarn passes through the slow cooling zone set at the end of the spinneret, and after passing through the oiling agent and a pair of rollers, the yarn is wound on the paper tube superior; rewinding the yarn on a metal tube, applying the oiling agent during rewinding; performing a heat treatment process on the yarn by gradually raising the temperature in four stages; and Rewinding the yarn after the heat treatment process on a paper tube. The method for producing aromatic polyester fibers according to claim 1, wherein the temperature of the heating and melting process is 280°C to 320°C. The method for producing aromatic polyester fibers according to claim 1, wherein the temperature in the slow cooling zone is 280°C to 320°C. The method for producing aromatic polyester fibers according to claim 1, wherein the length of the slow cooling zone is 10 mm to 110 mm. The method for producing aromatic polyester fibers according to claim 1, wherein the oiling agent includes polysiloxane-based oiling agents. The method for producing aromatic polyester fiber according to claim 1, wherein the rewinding tension for rewinding the yarn on the metal tube is 0 to 10 cN. The method for producing aromatic polyester fibers as described in Claim 1, wherein the temperature is gradually raised in four stages from 220°C to 320°C. The manufacturing method of the aromatic polyester fiber as described in Claim 1, wherein carrying out gradual heating in four stages includes: In the first stage, treat at a temperature of 240°C for 3 hours; In the second stage, treat at a temperature of 265°C for 14 hours; In the third stage, treat at a temperature of 280°C for 7 hours; and In the fourth stage, treat at a temperature of 300°C for 7 hours. The method for producing aromatic polyester fibers according to claim 1, wherein the heat treatment process takes 0.5 hours to 50 hours. The method for producing aromatic polyester fibers as claimed in claim 1, wherein the material of the metal tube includes iron, copper, aluminum or stainless steel. An aromatic polyester fiber, made by the method for producing aromatic polyester fiber described in any one of claim 1 to claim 10, the fiber strength of the aromatic polyester fiber is 20 g/d to 25 g/d g/d, the elongation is 1% to 4%.