A cool-sensation polyester fiber and its preparation method

Abstract

The present invention discloses a cool feeling polyester fiber, characterized in that, according to the weight percentage, it comprises the following raw materials: 10-30 parts of cool feeling regulating additives and 100-220 parts of polyester chips; wherein, the cool feeling regulating additive is composed of an esterification product of mannitol and / or lactitol and at least one of p-aminobenzoic acid and its carboxylic acid derivatives, salicylic acid and its carboxylic acid derivatives. By adjusting the ratio of mannitol and / or lactitol to at least one of p-aminobenzoic acid and its carboxylic acid derivatives, salicylic acid and its carboxylic acid derivatives, a cool feeling regulating additive that can absorb moisture and cool down and absorb ultraviolet rays is obtained, and is added to polyester fibers, which can effectively increase the outward transfer rate of heat emitted by polyester fibers to human bodies, and the fiber has a significant skin-friendly cool feeling; at the same time, the phenomenon of nanoparticle agglomeration is also improved, and due to the principle of like dissolves like, the compatibility and dispersibility in polyester fibers are excellent, and there is no adverse loss to spinning equipment.

Description

Technical Field

[0001] The present invention relates to the textile industry, and particularly to a cool-sensation polyester fiber and a preparation method thereof. Background Art

[0002] Nowadays, with the continuous progress of science and technology and the continuous improvement of living standards, people have new requirements for the performance of clothing. From simply covering the body and keeping warm in the past to paying attention to fashion later, and now people have started to focus on the functionality and environmental protection of fabrics. In recent years, humans have used a large amount of fossil fuels and cut down forests, resulting in a sharp increase in the concentration of gases such as carbon dioxide in the earth's atmosphere, causing the "greenhouse effect" and a rise in the global average temperature. Due to global warming, summers are hotter, and humans have increased the use of refrigeration equipment such as air conditioners, making the "greenhouse effect" more serious and causing a vicious cycle. Against this background, people have put forward requirements for cool-sensation and comfortable clothing, and products with excellent cool-sensation performance have been favored by people.

[0003] In recent years, the types of cool-sensation fibers have become increasingly rich. However, from the mechanism of fiber generating cool-sensation, cool-sensation fibers can be divided into the following two types. One is to design a cross-sectional shape of an irregular fiber such as a flat shape, a three-leaf shape, or a cross shape, improve the moisture absorption and air permeability of the fiber through the microporous structure on the fiber surface, and at the same time utilize the larger specific surface area of the irregular fiber to enhance the capillary effect, promote the conduction of moisture on the fiber, and accelerate the evaporation of human sweat to release heat. The other is to add powders with high thermal conductivity in ordinary fibers, or utilize the high thermal conductivity of the fiber matrix material itself to accelerate the rate of heat dissipation from the human body surface, and then obtain a cool feeling.

[0004] The patent with the publication number CN102031581B discloses a manufacturing method of a super-cool-sensation health-care polyester fiber. In this method, sheet mica and alumina and zinc oxide with high phase change enthalpy and fast heat conduction speed are micronized and ground into powders with a size of 100 - 300 nanometers, and then blended with a fiber-forming polymer for processing to obtain a cool-sensation health-care polyester fiber. However, since mica, jade, etc. are all natural materials, it is difficult to crush them into nanoscale, and they are prone to agglomeration, with poor dispersibility in the polyester melt, and also cause greater pressure on the spinning equipment, which is not conducive to the processing of polyester fibers. In addition, the presence of metal oxides such as alumina and zinc oxide will promote the photo-aging of polyester fibers. Summary of the Invention

[0005] In order to solve the problems such as greater pressure on equipment during the spinning process of traditional cool-sensation polyester fibers and unclear cool-sensation, the present invention provides a cool-sensation polyester fiber and a preparation method thereof. In the cool-sensation polyester fiber, an esterification product of p-aminobenzoic acid and mannitol and / or lactitol is used as an additive, which has no problem of dispersion compatibility, and can also better improve the skin comfort and cooling property of the polyester fiber.

[0006] A cool-sensation polyester fiber, by weight parts, comprises the following raw materials: 10-30 parts of a cool-sensation regulating additive and 100-220 parts of polyester chips; wherein, the cool-sensation regulating additive is composed of an esterification product of mannitol and / or lactitol with at least one of p-aminobenzoic acid and its carboxylic acid derivatives, and salicylic acid and its carboxylic acid derivatives.

[0007] In some embodiments of the present invention, the preparation method of the cool-sensation regulating additive comprises the following steps: dissolving mannitol and / or lactitol with at least one of p-aminobenzoic acid and its carboxylic acid derivatives, and salicylic acid and its carboxylic acid derivatives in an organic solvent, adding a Lewis acid catalyst thereto, heating to 80-100 °C for an esterification reaction, waiting for the reaction to be complete, cooling to room temperature, filtering, extracting with saturated sodium carbonate, and separating liquids, thus obtaining the cool-sensation regulating additive.

[0008] Further, the p-aminobenzoic acid and its carboxylic acid derivatives are at least one of p-aminobenzoic acid, 5-carboxy-isodihydroindole (CAS: 15861-30-0), 4-piperazin-1-yl-benzoic acid (CAS: 85474-75-5), 4-dimethylaminobenzoic acid, 4-(N,N-diethylamino)benzoic acid, 4-amino-2-methylbenzoic acid (CAS: 2486-75-1), 4-amino-3-methoxybenzoic acid (CAS: 2486-69-3), 4-amino-3-nitrobenzoic acid (CAS: 1588-83-6), p-acetamidobenzoic acid (CAS: 556-08-1), 4-hydrazinobenzoic acid (CAS: 619-67-0).

[0009] Further, the salicylic acid and its carboxylic acid derivatives are at least one of salicylic acid, sodium p-aminosalicylate dihydrate, 3-methylsalicylic acid, 3-methoxysalicylic acid, 4-methylsalicylic acid, 4-methoxysalicylic acid, 5-methylsalicylic acid, 5-methoxysalicylic acid, 6-methoxysalicylic acid, 2-hydroxy-3-naphthoic acid, 1,4-dihydroxy-2-naphthoic acid, 3,5-di-tert-butylsalicylic acid, 3,5-diisopropylsalicylic acid, 3-aminosalicylic acid, 5-aminosalicylic acid, gentisic acid, 3-nitrosalicylic acid, 4-nitrosalicylic acid, 3,5-dinitrosalicylic acid.

[0010] Further, the mannitol and / or lactitol and at least one of the p-aminobenzoic acid and its carboxylic acid derivatives and / or the salicylic acid and its carboxylic acid derivatives are added according to a molar ratio of hydroxyl group to carboxyl group of 1:0.2-0.5.

[0011] The reason for limiting the molar ratio of hydroxyl groups to carboxyl groups in the system to 1:0.2 - 0.5 is that the hygroscopic heat release performance of mannitol and / or lactitol is highly correlated with the hydroxyl group structure it contains. If all the hydroxyl groups and carboxylic acids carried by it are reacted to form ester groups, the cool feeling regulation performance of the resulting esterified product will be greatly reduced. Although the existing salicylic acid structure and p-aminobenzoate structure have ultraviolet absorption properties, it is still impossible to achieve good tactile cooling. Therefore, through the analysis of the test results, it is concluded that by optimizing the molar ratio of hydroxyl groups to carboxyl groups in the system to 1:0.2 - 0.5 and applying the resulting product to polyester fibers, better cool feeling performance can be obtained.

[0012] Further, the organic solvent is at least one of chloroform, dimethyl sulfoxide, and toluene.

[0013] Further, the Lewis acid is at least one of aluminum chloride, iron chloride, boron trifluoride, and niobium pentachloride.

[0014] Further, the added mass of the Lewis acid accounts for 2 - 5% of the total mass of mannitol and / or lactitol and at least one of p-aminobenzoic acid and its carboxylic acid derivatives, and salicylic acid and its carboxylic acid derivatives.

[0015] The preparation method of the above-mentioned cool feeling polyester fiber comprises the following steps: melting and blending the cool feeling temperature regulating additive and polyester chips in a screw extruder, and then obtaining the cool feeling polyester fiber through spinning, winding, drawing, and crimping.

[0016] Further, the spinning temperature is 270 - 290 °C, the spinning speed is 1000 - 1200 m / min; the draw ratio is 3.8 - 4.2 times.

[0017] Further, the cross-section of the cool feeling polyester fiber of the present invention can be any cross-section of known melt spinning, such as circular, triangular, trilobal, hollow, flat, L-shaped, T-shaped, W-shaped, polygonal, dogbone-shaped, etc., and the fineness of its single filament is 0.8 denier to 10 denier.

[0018] Beneficial effects: Compared with the prior art, the cool feeling polyester fiber provided by the present invention has the following advantages: By adjusting the ratio of mannitol and / or lactitol and at least one of p-aminobenzoic acid and its carboxylic acid derivatives, and salicylic acid and its carboxylic acid derivatives, a cool feeling regulating additive that can both absorb moisture and cool down and absorb ultraviolet rays is obtained. When added to polyester fibers, it can effectively improve the outward heat transfer rate of the heat emitted by the human body by the polyester fibers, and the skin-friendly cool feeling of the fibers is obvious; at the same time, it also improves the non-existence of nanoparticle aggregation phenomenon, and due to the principle of similar solubility, it has excellent compatibility and dispersibility in polyester fibers and has no adverse loss to the spinning equipment. Specific embodiments

[0019] The present invention will be further described in detail below in conjunction with examples. It should be noted that the following examples and comparative examples are examples of the present invention, only for illustrating the present invention, and not for limiting the present invention. Without departing from the gist or scope of the present invention, other combinations and various improvements within the concept of the present invention can be made.

[0020] The preparation of the cool feeling regulating additive used in the examples is exemplarily described as follows:

[0021] Cool feeling regulating additive #1

[0022] Dissolve 18.2 g (0.1 mol) of mannitol and 16.44 g (0.12 mol) of p-aminobenzoic acid in 100 ml of chloroform, add 0.69 g of aluminum chloride thereto, heat to 100 °C for an esterification reaction. After the reaction is complete, cool to room temperature, and obtain the cool feeling regulating additive #1 through filtration, extraction with saturated sodium carbonate, and liquid separation.

[0023] Cool feeling regulating additive #2

[0024] Dissolve 18.2 g (0.1 mol) of mannitol and 37.08 g (0.18 mol) of 4-piperazin-1-yl-benzoic acid in 100 ml of chloroform, add 1.66 g of aluminum chloride thereto, heat to 90 °C for an esterification reaction. After the reaction is complete, cool to room temperature, and obtain the cool feeling regulating additive #2 through filtration, extraction with saturated sodium carbonate, and liquid separation.

[0025] Cool feeling regulating additive #3

[0026] Dissolve 18.2 g (0.1 mol) of mannitol and 57.9 g (0.30 mol) of 4-(N,N-diethylamino)benzoic acid in 100 ml of chloroform, add 3.81 g of aluminum chloride thereto, heat to 100 °C for an esterification reaction. After the reaction is complete, cool to room temperature, and obtain the cool feeling regulating additive #3 through filtration, extraction with saturated sodium carbonate, and liquid separation.

[0027] Cool feeling regulating additive #4

[0028] The process is the same as that of the cool feeling regulating additive #1, except that p-aminobenzoic acid is replaced with an equimolar amount of salicylic acid.

[0029] Cool feeling regulating additive #5

[0030] The process is the same as that of the cool feeling regulating additive #3, except that 4-(N,N-diethylamino)benzoic acid is replaced with an equimolar amount of 3,5-diisopropylsalicylic acid.

[0031] Cool feeling regulating additive #6

[0032] Dissolve 34.4 g (0.1 mol) of lactitol and 27.18 g (0.18 mol) of 4-amino-2-methylbenzoic acid in 100 ml of dimethyl sulfoxide, add 1.85 g of iron(III) chloride thereto, heat to 80 °C for esterification reaction. After the reaction is complete, cool to room temperature, and obtain the cooling sensation regulating additive #6 through filtration, extraction with saturated sodium carbonate, and liquid separation.

[0033] Cooling sensation regulating additive #7

[0034] Dissolve 34.4 g (0.1 mol) of lactitol and 64.44 g (0.36 mol) of p-acetamidobenzoic acid in 150 ml of dimethyl sulfoxide, add 4.94 g of iron(III) chloride thereto, heat to 90 °C for esterification reaction. After the reaction is complete, cool to room temperature, and obtain the cooling sensation regulating additive #7 through filtration, extraction with saturated sodium carbonate, and liquid separation.

[0035] Cooling sensation regulating additive #8

[0036] Dissolve 34.4 g (0.1 mol) of lactitol and 45.36 g (0.27 mol) of 5-methoxysalicylic acid in 200 ml of dimethyl sulfoxide, add 3.19 g of iron(III) chloride thereto, heat to 100 °C for esterification reaction. After the reaction is complete, cool to room temperature, and obtain the cooling sensation regulating additive #8 through filtration, extraction with saturated sodium carbonate, and liquid separation.

[0037] Cooling sensation regulating additive #9

[0038] Dissolve 34.4 g (0.1 mol) of lactitol and 91.8 g (0.45 mol) of 1,4-dihydroxy-2-naphthoic acid in 200 ml of toluene, add 6.3 g of boron trifluoride thereto, heat to 100 °C for esterification reaction. After the reaction is complete, cool to room temperature, and obtain the cooling sensation regulating additive #9 through filtration, extraction with saturated sodium carbonate, and liquid separation.

[0039] Cooling sensation regulating additive #10

[0040] The process is the same as that of the cooling sensation regulating additive #9, except that the molar amount of 1,4-dihydroxy-2-naphthoic acid used is 0.54 mol.

[0041] Example 1

[0042] Melt and blend 30 parts of the cooling sensation regulating additive #1 and 100 parts of polyester chips in a screw extruder, and then obtain the cooling sensation polyester fiber through spinning at 270 °C (speed: 1000 m / min), winding, drawing (3.8 times), and crimping.

[0043] Example 2

[0044] 25 parts of cool feeling regulating additive #2 and 130 parts of polyester chips were melt-blended in a screw extruder, and then spun at 270 °C (speed: 1000 m / min), wound, drawn (3.8 times), and crimped to obtain cool feeling polyester fibers.

[0045] Example 3

[0046] 20 parts of cool feeling regulating additive #3 and 150 parts of polyester chips were melt-blended in a screw extruder, and then spun at 275 °C (speed: 1100 m / min), wound, drawn (4.0 times), and crimped to obtain cool feeling polyester fibers.

[0047] Example 4

[0048] 15 parts of cool feeling regulating additive #4 and 180 parts of polyester chips were melt-blended in a screw extruder, and then spun at 275 °C (speed: 1100 m / min), wound, drawn (4.0 times), and crimped to obtain cool feeling polyester fibers.

[0049] Example 5

[0050] 10 parts of cool feeling regulating additive #5 and 220 parts of polyester chips were melt-blended in a screw extruder, and then spun at 280 °C (speed: 1200 m / min), wound, drawn (4.2 times), and crimped to obtain cool feeling polyester fibers.

[0051] Example 6

[0052] Same as Example 5, except that cool feeling regulating additive #5 was replaced with cool feeling regulating additive #6.

[0053] Example 7

[0054] Same as Example 5, except that cool feeling regulating additive #5 was replaced with cool feeling regulating additive #7.

[0055] Example 8

[0056] Same as Example 5, except that cool feeling regulating additive #5 was replaced with cool feeling regulating additive #8.

[0057] Example 9

[0058] Same as Example 5, except that cool feeling regulating additive #5 was replaced with cool feeling regulating additive #9.

[0059] Example 10

[0060] Same as Example 5, except that cool feeling regulating additive #5 was replaced with cool feeling regulating additive #10.

[0061] Comparative Example 1

[0062] Same as Example 5, except that the cool feeling regulating additive #5 is replaced with an equal amount of mannitol.

[0063] Comparative Example 2

[0064] Same as Example 5, except that the cool feeling regulating additive #5 is replaced with an equal amount of 3,5 - diisopropyl salicylic acid.

[0065] Comparative Example 3

[0066] Same as Example 6, except that the cool feeling regulating additive #6 is replaced with an equal amount of lactitol.

[0067] Comparative Example 4

[0068] Same as Example 6, except that the cool feeling regulating additive #6 is replaced with an equal amount of 4 - amino - 2 - methylbenzoic acid.

[0069] Comparative Example 5

[0070] Same as Example 6, except that the cool feeling regulating additive #6 is not added.

[0071] Performance Test

[0072] Hygroscopicity: According to the standard GB / T9995 - 1997 "Textile materials - Moisture regain - Oven - drying method", measure the moisture regain of the fiber, control the fabric specimen to be exposed in an environment with a temperature fluctuation range of ±2°C, and set the temperature of the constant - temperature oven to (105 ± 2)°C, and the drying time is 60 min;

[0073] Moisture permeability: Refer to the standard GB / T 12704.1 - 2009 "Textiles - Test method for moisture permeability of fabrics - Part 1: Moisture absorption method" for measurement, control the circulating air flow speed to be 0.3 - 0.5 m / s, and the relative humidity control accuracy is ±2%;

[0074] Contact cool feeling performance: Test using a KES - QM cool feeling performance tester. Refer to the standard GB / T35263 - 2017. Prepare 3 specimens with the same surface density of 10 cm × 10 cm for each fabric and place them in a standard atmosphere to equilibrate for more than 24 h. The test results are averaged. The test index is the cool feeling coefficient Q max , that is, the peak value reached by the heat release in 0.2 s, Q max The larger the Q value, the cooler the human body feels when contacting the fabric; conversely, the warmer it feels.

[0075] The test results are shown in Table 1:

[0076] Table 1 Performance test results of the fibers obtained in Examples 1 - 10 and Comparative Examples 1 - 5

[0077]

[0078] As can be seen from the data in Table 1, the cool-sensation polyester fiber provided by the present invention has excellent moisture absorption and moisture permeability, thus achieving an ideal contact cool-sensation. By comparing the results of Example 10 with those of Examples 1-9, it can be found that when more hydroxyl groups of the used lactitol are reacted, the prepared cool-sensation regulating additive is added to the polyester fiber, and both the moisture permeability and the cool-sensation coefficient decrease. It can be seen that the amount of hydroxyl groups contained in the cool-sensation regulating additive has a great influence on the contact cool-sensation of the cool-sensation polyester fiber. The results of Comparative Examples 1-4 show that when mannitol or lactitol or salicylic acid derivative or p-aminobenzoic acid derivative is used alone, the contact cool-sensation of the obtained polyester fiber is inferior to that of the polyester fiber obtained in Examples 1-10. From this, it can be inferred that the product of mannitol and / or lactitol and at least one compound among p-aminobenzoic acid and its carboxylic acid derivatives, salicylic acid and its carboxylic acid derivatives improves the cool-sensation of the polyester fiber to a much greater extent than the improvement effect of a single component.

[0079] The above are only the preferred embodiments of the present invention, and do not impose any limitations on the present invention. Any simple modification, change, and equivalent transformation made to the above embodiments according to the technical essence of the present invention still belong to the protection scope of the technical solution of the present invention.

Claims

1. A cool feeling polyester fiber, characterized in that: The invention comprises the following raw materials in parts by weight: 10-30 parts of a cooling agent and 100-220 parts of polyester chips; wherein the cooling agent is composed of an esterification product of mannitol and / or lactitol and at least one of p-aminobenzoic acid and its carboxylic acid derivatives, salicylic acid and its carboxylic acid derivatives; The mannitol and / or lactitol and at least one of p-aminobenzoic acid and its carboxylic acid derivatives and / or salicylic acid and its carboxylic acid derivatives are added according to a molar ratio of hydroxyl group to carboxyl group of 1:0.2-0.5; The preparation method of the cool feeling polyester fiber comprises the following steps: melt-blending a cool feeling regulating additive and polyester chips in a screw extruder, and then spinning, winding, drawing and curling to obtain the cool feeling polyester fiber.

2. The cool polyester fiber according to claim 1, characterized in that: The preparation method of the cooling sensation regulating additive comprises the following steps: dissolving mannitol and / or lactitol and at least one of p-aminobenzoic acid and its carboxylic acid derivatives, salicylic acid and its carboxylic acid derivatives in an organic solvent, adding a Lewis acid catalyst thereto, heating to 80-100° C. for esterification reaction, cooling to room temperature after the reaction is complete, filtering, extracting with saturated sodium carbonate, and separating the liquids to obtain the cooling sensation regulating additive.

3. The cool polyester fiber according to claim 2, characterized in that: The p-aminobenzoic acid and its carboxylic acid derivatives are at least one of p-aminobenzoic acid, 5-carboxy-isoindoline, 4-(piperazine-1-yl)benzoic acid, 4-dimethylaminobenzoic acid, 4-(N,N-diethylamino)benzoic acid, 4-amino-2-methylbenzoic acid, 4-amino-3-methoxybenzoic acid, 4-amino-3-nitrobenzoic acid, p-acetylaminobenzoic acid, and 4-hydrazinobenzoic acid.

4. The cool polyester fiber according to claim 2, characterized in that: The salicylic acid and its carboxylic acid derivatives are at least one of salicylic acid, sodium p-aminosalicylate dihydrate, 3-methylsalicylic acid, 3-methoxysalicylic acid, 4-methylsalicylic acid, 4-methoxysalicylic acid, 5-methylsalicylic acid, 5-methoxysalicylic acid, 6-methoxysalicylic acid, 2-hydroxy-3-naphthoic acid, 1,4-dihydroxy-2-naphthoic acid, 3,5-di-tert-butylsalicylic acid, 3,5-diisopropylsalicylic acid, 3-aminosalicylic acid, 5-aminosalicylic acid, gentisic acid, 3-nitrosalicylic acid, 4-nitrosalicylic acid, and 3,5-dinitrosalicylic acid.

5. The cool polyester fiber according to claim 2, characterized in that: The organic solvent is at least one of chloroform, dimethyl sulfoxide and toluene.

6. The cool polyester fiber according to claim 2, characterized in that: The Lewis acid is at least one of aluminum chloride, ferric chloride, boron trifluoride and niobium pentachloride.

7. The cool feeling polyester fiber according to claim 6, characterized in that: The added mass of the Lewis acid accounts for 2-5% of the total mass of the mannitol and / or lactitol and at least one of p-aminobenzoic acid and its carboxylic acid derivatives, salicylic acid and its carboxylic acid derivatives.

8. The method for preparing the cool polyester fiber according to any one of claims 1 to 7, characterized in that: The method comprises the following steps: melt-blending a cooling feeling regulating additive and polyester chips in a screw extruder, and then spinning, winding, drawing and curling to obtain cooling feeling polyester fibers.

9. The method for preparing the cool polyester fiber according to claim 8, characterized in that: The spinning temperature is 270-290° C., the spinning speed is 1000-1200 m / min; and the drafting multiple is 3.8-4.2 times.

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