TWI693310B - Intrinsic masterbatch for fluorescent fiber, fluorescent fiber and preparation method thereof - Google Patents

Abstract

Provided is an intrinsic masterbatch for a fluorescent fiber that includes about 65 to 80 parts by weight of a base powder, about 1 to 5 parts by weight of a fluorescent colorant, about 10 to 20 parts by weight of a solar resistant agent, and about 9 to 15 parts by weight of an additive, wherein the base powder may include polybutylene terephthalate (PBT). A fluorescent fiber and a preparation method thereof are also provided.

Description

Essential fluorescent fiber masterbatch, fluorescent fiber and preparation method thereof

The invention relates to a textile material, and in particular to an essential fluorescent fiber masterbatch, fluorescent fiber and preparation method thereof.

Under the trend of globalization, the textile industry is facing strong competitive pressure. The textile industry must constantly develop new technologies and diversified products in order to face global competition. More and more people in modern society are active at night, such as night workers (such as police or cleaning staff), cyclists, road runners, etc. In order to improve the safety of night activities, the research and development of protective clothing made of fluorescent fibers has received great attention from the industry.

In view of this, the present invention provides an essential fluorescent fiber masterbatch and a method for preparing fluorescent fiber. The color of the prepared fluorescent fiber falls within the standard EN471 color gamut and the visual whiteness (β) is greater than 0.7. Comply with the specifications of the standard EN471 standard.

The invention provides an essential fluorescent fiber masterbatch, which includes 65 to 80 parts by weight of base powder, 1 to 5 parts by weight of fluorescent colorant, and 10 to 20 parts by weight of sunlight resistance Agent and 9 to 15 parts by weight of additives. In one embodiment, the substrate powder includes polybutylene terephthalate.

。 In an embodiment of the invention, the fluorescent color material includes a fluorescent yellow material, which includes at least one of the structures of formula (1), formula (2), formula (3), and formula (4):

.

In an embodiment of the present invention, the sun-resistant agent includes montmorillonite, titania (TiO ₂ ), silica (SiO ₂ ), barium sulfate (BaSO ₄ ), or a combination thereof.

In an embodiment of the invention, 9 to 15 parts by weight of the additive includes 3 to 5 parts by weight of the second dispersant, 3 to 5 parts by weight of the antioxidant, and 3 to 5 parts by weight of the stabilizer.

The present invention also provides a fluorescent fiber, which is made using the above-mentioned essential fluorescent fiber masterbatch, wherein the color of the fluorescent fiber is fluorescent yellow and meets the specifications of the standard EN471.

The invention also provides a method for preparing a fluorescent fiber, which includes the following steps. 3 to 5 parts by weight of fluorescent colorant, 5 to 15 parts by weight of sunlight resistance agent, 10 to 20 parts by weight of first dispersant, and 60 to 80 parts by weight of water are uniformly mixed to form a mixed liquid. The liquid mixture is subjected to liquid grinding, dispersion and modification steps to obtain a fluorescent color paste modified dispersion liquid with an average particle size of 150-200 nm. 64-87 parts by weight of the substrate powder, 3-80 parts by weight of the modified dispersion of the fluorescent color paste, and 9-15 parts by weight of additives are uniformly mixed. A drying step is carried out to remove water. The kneading granulation step is carried out to form the intrinsic fluorescent fiber masterbatch. 0.5 to 2 parts by weight of the essential fluorescent fiber mother particles and 15 to 25 parts by weight of the carrier are mixed. The melt spinning step is performed to obtain fluorescent fibers.

In an embodiment of the present invention, the above-mentioned liquid grinding, dispersing and modifying steps include grinding at 1,500-2,700 rpm for 30-120 minutes.

In an embodiment of the invention, the substrate powder includes polybutylene terephthalate (PBT).

In an embodiment of the present invention, the carrier includes polyethylene terephthalate (PET).

In an embodiment of the present invention, the spinning temperature of the melt spinning step is in the range of 275°C to 285°C.

Based on the above, the fluorescent fiber prepared by the present invention contributes to the improvement of visual whiteness (β), and its color complies with the specifications of standard EN471. In addition, the average particle diameter of the modified dispersion of fluorescent color paste is controlled between 150nm and 200nm, which can make The color of the prepared fluorescent fiber is closer to the center of the standard EN471 color gamut. In addition, the fluorescent fiber prepared by the present invention has excellent sunlight resistance, fastness to washing and fastness to perspiration, meeting the needs of users.

In order to make the above-mentioned features and advantages of the present invention more obvious and understandable, the embodiments are specifically described below in conjunction with the accompanying drawings for detailed description as follows.

100, 102, 104, 106, 108, 110, 112: steps

FIG. 1 is a flowchart of a method for preparing a fluorescent fiber according to an embodiment of the invention.

2 is a color diagram of colored yarns prepared in Comparative Examples 1 to 6 and Experimental Examples 1 to 2 of the present invention, where the dotted area is the standard EN471 fluorescent yellow field.

The invention uses the grinding compound processing technology to introduce the sunlight-resistant agent to prepare the fluorescent color paste modified dispersion liquid, and the average particle size of the dispersion in the fluorescent color paste modified dispersion liquid is controlled to 150nm to 200nm by the grinding collision method In this way, intrinsic fluorescent fiber masterbatch and fluorescent fiber complying with standard EN471 are prepared.

The invention provides an essential fluorescent fiber masterbatch, which includes 65 to 80 parts by weight of base powder, 1 to 5 parts by weight of fluorescent colorant, 10 to 20 parts by weight of sunlight resistance agent, and 9 to 15 parts by weight Parts of additives.

In one embodiment, the substrate powder may include polybutylene terephthalate (PBT).

。 In an embodiment, the fluorescent color material includes a fluorescent yellow material, which may include at least one of the structures of formula (1), formula (2), formula (3), and formula (4):

.

In an embodiment, the sun-resistant agent may include montmorillonite, titania (TiO ₂ ), silica (SiO ₂ ), barium sulfate (BaSO ₄ ), or a combination thereof. More specifically, montmorillonite is an intercalated structure, and the color material is inserted between the intercalated layers, which is expected to improve the light fastness without affecting the color. Silicon dioxide has the advantages of low refractive index and low dispersion, and it is expected that after addition, the fluorescent color yellow will not cause color shift due to dispersion. Barium sulfate is a total reflection material for optical detection. It is expected to contribute to the improvement of visual whiteness (β) after addition, and then to move the color to the center of the standard EN417 color gamut.

In one embodiment, 9 to 15 parts by weight of the additive may include 3 to 5 parts by weight The amount of the second dispersant, 3 to 5 parts by weight of antioxidant and 3 to 5 parts by weight of stabilizer.

。 In an embodiment, the second dispersant may include at least one of formula (5), formula (6), and formula (7):

.

。 In an embodiment, the antioxidant may include at least one of the structures of formula (8), formula (9), and formula (10):

.

。 In one embodiment, the stabilizer may include at least one of formula (11), formula (12), and formula (13):

.

The exemplary structures of the components listed above are only for the sake of explanation, and are not intended to limit the present invention. Other structures can also be used for each component, as long as the essential fluorescent fiber masterbatch of the present invention can be prepared.

The present invention also provides a fluorescent fiber, which is made using the above-mentioned essential fluorescent fiber masterbatch, wherein the color of the fluorescent fiber is fluorescent yellow and meets the specifications of the standard EN471. Hereinafter, an exemplary preparation method of the fluorescent fiber of the present invention will be described.

FIG. 1 is a flowchart of a method for preparing a fluorescent fiber according to an embodiment of the invention.

Please refer to FIG. 1. First, in step 100, 3 to 5 parts by weight of fluorescent colorant, 5 to 15 parts by weight of sunlight resistance agent, 10 to 20 parts by weight of first dispersant and 60 to 80 parts by weight The water is mixed evenly to form a mixed liquid. In step 100, Add about 0.01 to 1 part by weight of defoamer as appropriate to remove foam in the mixed liquid. The first dispersant is, for example, commercially available BYK190 (purchased from Germany Walker), and the defoamer is, for example, commercially available BASF-FOAMASTER 333 (purchased from BASF).

Then, in step 102, the mixed liquid is subjected to liquid grinding, dispersion and modification steps to obtain a fluorescent color paste modified dispersion liquid having an average particle size of 150 to 200 nm. In one embodiment, the steps of liquid grinding, dispersion and modification include grinding at a speed of 1,500 to 2,700 rpm for 30 to 120 minutes.

Next, in step 104, 64 to 87 parts by weight of the base powder, 3 to 80 parts by weight of the modified dispersion of fluorescent paste and 9 to 15 parts by weight of additives are uniformly mixed. In one embodiment, the substrate powder includes polybutylene terephthalate (PBT). In an embodiment, 9 to 15 parts by weight of the additive includes 3 to 5 parts by weight of the second dispersant, 3 to 5 parts by weight of the antioxidant, and 3 to 5 parts by weight of the stabilizer.

Next, in step 106, a drying step is performed to remove water. In one embodiment, the drying step may include drying at a temperature of 90°C to 110°C for 12 to 24 hours.

Next, in step 108, a kneading granulation step is performed to form an intrinsic type fluorescent fiber master batch. In one embodiment, the kneading temperature of the kneading granulation step is in the range of 220°C to 250°C.

Then, in step 110, 0.5 to 2 parts by weight of the essential fluorescent fiber mother particles and 15 to 25 parts by weight of the carrier are mixed. In one embodiment, the carrier includes polyethylene terephthalate (PET).

Next, in step 112, a melt spinning step is performed to obtain fluorescent fibers. In one embodiment, the spinning temperature of the melt spinning step is, for example, in the range of 275°C to 285°C. In one embodiment, the fiber specification is 150d/48f, for example. In another embodiment, the fiber size is 75d/48f, for example. In yet another embodiment, the fiber size is 75d/96f, for example.

In one embodiment, the color of the obtained fluorescent fiber is fluorescent yellow and meets the specifications of standard EN471. More specifically, the conventional method is generally to use non-fluorescent fiber masterbatch to make fiber or fabric, and then dye or finish the fiber or fabric to make it have fluorescent color. Fluorescent dyes are not easy to provide, and the fluorescent pigments have poor adhesion to fabrics. Therefore, the fluorescent fibers or fluorescent fabrics obtained by conventional methods will have dyeing uniformity, washing fastness, and durability. Problems with poor properties such as sweat fastness and sunlight fastness. However, the present invention uses intrinsic fluorescent fiber masterbatch to prepare fluorescent fiber. Therefore, the fluorescent fiber of the present invention can have fluorescent color without dyeing and finishing process and is an intrinsic fluorescent fiber. Therefore, the fluorescent fiber of the present invention does not have the problem of poor dyeing uniformity, and has better washing fastness, perspiration fastness and sunlight fastness.

Hereinafter, a plurality of comparative examples and experimental examples will be listed to verify the efficacy of the present invention.

First, in step 100, a mixed solution is prepared according to the formula in Table 1.

Then, in step 102, the mixed liquid is grinded to obtain the modified dispersion of the fluorescent color paste Liquid (abbreviated as color paste). Table 2 shows the average particle size of the color paste, that is, the average particle size of the dispersoid in the modified dispersion of the fluorescent color paste. Depending on the grinding conditions, even if the same sun-resistant agent is used, the average particle size may be different. Color pastes A~G use different sun-resistant agents and grinding conditions, wherein the average particle size of color paste C to color paste G falls within the range of 150-200 nm set by the present invention, and the average of color paste A and color paste B The particle size exceeds the range of 150-200 nm set by the present invention.

Next, proceed to step 104 according to the recipe in Table 3, and then perform steps 106 and 108 to prepare an intrinsic fluorescent fiber masterbatch (abbreviated as masterbatch).

Then, step 110 is performed, and the prepared masterbatch (PBT) is diluted in a carrier (PET), where PBT:PET=1:19. Then, proceed to step 112 to prepare fluorescent fiber (abbreviated as color yarn). The converted effective yarn content of the color yarn is shown in Table 4. In Table 4, Comparative Examples 1 to 4 use unpolished mixed liquid, and the average particle size of the mixed liquid is greater than 1 μm; Comparative Examples 5 to 6 use ground color paste, but the average particle size of the color paste exceeds 150~ set by the present invention The range of 200 nm; experimental examples 1 to 5 use ground color paste, and the average particle size of the color paste falls within the range of 150 to 200 nm set by the present invention.

Next, the prepared fluorescent fiber (abbreviated as colored yarn) is subjected to various tests.

2 is a color diagram of colored yarns prepared in Comparative Examples 1 to 6 and Experimental Examples 1 to 2 of the present invention, where the dotted area is the standard EN471 fluorescent yellow field. Table 5 shows the results of color gamut detection. As shown in FIG. 2 and Table 5, when the polished color paste (Experiment Examples 1-2) is used and the average particle size of the color paste falls within the range of 150-200 nm set by the present invention, the prepared fluorescent fiber The visual whiteness (β) is greater than 0.7 and the color falls within the fluorescent yellow field of EN471, which complies with the standard EN471 for fluorescent yellow. In addition, compared with Comparative Examples 1 to 6, the colors of the fluorescent fibers of Experimental Examples 1 to 2 are closer to the center point of the fluorescent yellow region of the standard EN471.

On the other hand, when the unpolished mixed liquid (Comparative Examples 1 to 4) or the polished color paste (Comparative Examples 5 to 6) is used and the average particle size of the color paste exceeds the range of 150 to 200 nm set by the present invention, Although the color is still at the boundary of the fluorescent yellow field of EN471, its visual whiteness (β) is lower than 0.7, which does not meet the specifications of standard EN471.

Therefore, in the present invention, the average particle size of the fluorescent color paste modified dispersion liquid is controlled between 150 nm and 200 nm, so that the color of the prepared fluorescent fiber can be close to the center point of the fluorescent yellow region of the standard EN471, and Its visual whiteness (β) is higher than 0.7 and meets the EN471 standard, which has unexpected effects.

Table 6 shows the test results of sunlight fastness. As shown in Table 6, the colored yarn of Comparative Example 1 has no fastness to sunlight due to the absence of a sun-resistant agent. Although the colored yarns of Comparative Examples 2 to 4 are added with a sunlight-resistant agent, they are made of a mixed solution with a larger particle size, so Comparative Examples 2 to 4 are also faster in sunlight resistance than Experimental Examples 1 to 5. The fastness is poor. On the other hand, the colored yarns of Experimental Examples 1 to 5 all have a considerable degree of fastness to sunlight. Meet the needs of users.

Table 7 shows the test results of fastness to washing and perspiration. As shown in Table 7, the colored yarns of Comparative Examples 4 to 6 and Experimental Examples 1 to 5 all have a considerable degree of fastness to washing and perspiration, which meets the needs of users.

In summary, the fluorescent fiber prepared by the present invention is an intrinsic fluorescent fiber The dimension also contributes to the improvement of visual whiteness (β), so its color complies with the standard of EN471. In addition, the average particle size of the fluorescent color paste modified dispersion liquid is controlled between 150nm and 200nm, so that the color of the prepared fluorescent fiber is closer to the center point of the standard EN471 color gamut. In addition, the fluorescent fiber prepared by the present invention has excellent sunlight resistance, fastness to washing and fastness to perspiration, meeting the needs of users.

Although the present invention has been disclosed as above with examples, it is not intended to limit the present invention. Any person with ordinary knowledge in the technical field can make some changes and modifications without departing from the spirit and scope of the present invention. The scope of protection of the present invention shall be subject to the scope defined in the appended patent application.

100, 102, 104, 106, 108, 110, 112: steps

Claims (9)

An essential fluorescent fiber masterbatch, including: 65 to 80 parts by weight of base powder, which includes polybutylene terephthalate (PBT); 1 to 5 parts by weight of fluorescent colorant; 10 to 20 parts by weight of sun-resistant agent; and 9 to 15 parts by weight of additives, wherein the additives include 3 to 5 parts by weight of second dispersant, 3 to 5 parts by weight of antioxidant and 3 to 5 parts by weight of Stabilizer. The essential fluorescent fiber masterbatch as described in item 1 of the patent application scope, wherein the fluorescent color material includes a fluorescent yellow material, which includes formula (1), formula (2), formula (3) and formula ( 4) At least one of the structures:

. The essential fluorescent fiber masterbatch as described in item 1 of the patent application scope, wherein the sunlight-resistant agent includes montmorillonite, titania (TiO ₂ ), silica (SiO ₂ ), and barium sulfate (BaSO ₄ ) or a combination thereof. A fluorescent fiber made of the essential fluorescent fiber masterbatch according to any one of claims 1 to 3, wherein the color of the fluorescent fiber is fluorescent yellow and complies with the standard EN471 specification. A method for preparing fluorescent fiber, comprising: adding 3 to 5 parts by weight of fluorescent colorant, 5 to 15 parts by weight of sunlight resistance agent, 10 to 20 parts by weight of first dispersant, and 60 to 80 parts by weight of water Mix uniformly to form a mixed solution; perform liquid grinding, dispersion and modification steps on the mixed solution to obtain a modified dispersion of fluorescent color paste with an average particle size of 150 to 200 nm; 64 to 87 parts by weight of the substrate The powder, 3 to 80 parts by weight of the fluorescent color paste modified dispersion and 9 to 15 parts by weight of the additive are uniformly mixed, wherein the additive includes 3 to 5 parts by weight of the second dispersant and 3 to 5 parts by weight Parts of antioxidants and 3 to 5 parts by weight of stabilizers; a drying step to remove water; a mixing granulation step to form intrinsic fluorescent fiber masterbatch; 0.5 to 2 parts by weight of the intrinsic fluorescent The optical fiber masterbatch and 15 to 25 parts by weight of the carrier are mixed; and the melt spinning step is performed to obtain the fluorescent fiber. The method for preparing a fluorescent fiber as described in item 5 of the patent application range, wherein the steps of liquid grinding, dispersion and modification include grinding at a speed of 1,500 to 2,700 rpm for 30 to 120 minutes. The method for preparing a fluorescent fiber as described in item 5 of the patent application scope, wherein the substrate powder includes polybutylene terephthalate (PBT). The preparation method of the fluorescent fiber as described in item 5 of the patent application scope, wherein the carrier includes polyethylene terephthalate (PET). The method for preparing a fluorescent fiber as described in item 5 of the patent application range, wherein the spinning temperature of the melt spinning step is in the range of 275°C to 285°C.

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