A kind of luminous yarn and its preparation method

Abstract

The present invention relates to a luminous yarn and a preparation method thereof, belonging to the technical field of luminous yarns. A preparation method of a luminous yarn comprises the following steps: after mixing luminous powder and deionized water evenly, adding chitosan and carrying out ultrasonic mixing, filtering, freeze-drying, placing in an ethanol solution, adding dihydroxyformyl benzene, heating and stirring, filtering, washing, and drying to obtain modified luminous powder; after subjecting color powder, absolute ethanol and thiomalic acid to ultrasonic treatment, adding oleic acid and an initiator, heating and stirring, centrifuging, washing, and drying to obtain modified color powder; mixing the modified color powder, the modified luminous powder, a functional polymer and a thermoplastic polyester, and carrying out melt spinning to obtain the luminous yarn; the luminous yarn prepared by the present invention has excellent breaking strength and elongation at break.

Description

Technical Field

[0001] The present invention belongs to the technical field of luminous yarns, and relates to a luminous yarn and a preparation method thereof. Background Art

[0002] The luminous yarn made of polyethylene terephthalate as the raw material contains several main components, namely inorganic color powder, luminous powder and thermoplastic resin. This luminous yarn can emit weak light at night or in a dim light environment, having good visual effects. By uniformly mixing the inorganic color powder and the luminous powder in the thermoplastic resin and then through a special processing technology, these components are tightly combined together to form a yarn with luminous function. This luminous yarn not only has excellent physical properties, but also has the advantages of environmental protection, durability and easy processing, and is widely used in the fields of textiles, clothing, decoration, etc.

[0003] As an inorganic filler, the compatibility and dispersibility of the luminous powder and inorganic pigment particles in the polyethylene terephthalate system directly affect the mechanical properties, thermal stability and optical properties of the composite material, etc. The distribution state of the inorganic particles in the interfacial region of the polyethylene terephthalate blend shows a thermodynamically unstable characteristic, and this instability causes the inorganic particles to easily migrate. Further, due to the relatively weak interfacial interaction force between the inorganic particles and the two phases of the blend, even if the inorganic particles are selectively distributed in the interfacial region of the two phases of the blend, it is difficult for them to effectively exert the expected luminous effect, and it is also easy to cause a decrease in the mechanical properties of the luminous yarn. This phenomenon is mainly because the weak interfacial interaction causes the luminous powder particles to be unable to be firmly fixed on the interface, thus unable to fully display their filler characteristics. Summary of the Invention

[0004] The purpose of the present invention is to provide a luminous yarn and a preparation method thereof. The present invention adds rare earth metal luminous powder and introduces inorganic filler color powder, and through organic modification thereof, combines a toughening and compatibilizing polymer to increase its compatibility in the yarn material system. The organic modification selects ultrafine luminous powder and color powder components to be added to the yarn material in the form of covalent bonds and non-covalent bonds, and after melt extrusion, spinning is carried out, and finally a luminous yarn is prepared, endowing the luminous yarn with excellent mechanical properties.

[0005] The purpose of the present invention can be achieved through the following technical solutions:

[0006] A preparation method of a luminous yarn includes the following steps:

[0007] Step 1: Under an inert atmosphere, the luminous powder and deionized water are mixed evenly, then chitosan is added and ultrasonically mixed, and after filtration, freeze-drying is carried out to obtain a composite powder;

[0008] Step 2: Under an inert atmosphere, place the composite powder in an ethanol solution, add dihydroxybenzoylformaldehyde, heat and stir, filter, wash, and then dry to constant weight to obtain the modified luminous powder.

[0009] Step 3: Ultrasonically treat the color powder, absolute ethanol, and thiomalic acid, add oleic acid and an initiator, heat and stir, centrifuge, wash, and then dry to constant weight to obtain the modified color powder.

[0010] Step 4: Mix the modified color powder, modified luminous powder, functional polymer, and thermoplastic polyester in a high-speed mixer, and then place them in a twin-screw extruder for melt spinning to obtain the product.

[0011] As a preferred technical solution of the present invention, the thermoplastic polyester is polyethylene terephthalate.

[0012] As a preferred technical solution of the present invention, in Step 1, the inert atmosphere is a nitrogen atmosphere; the mixing is stirring for 30 - 40 min; the ultrasonic mixing is ultrasonic treatment at a power of 500 - 600 W for 50 - 60 min.

[0013] As a preferred technical solution of the present invention, in Step 1, the mass ratio of the luminous powder, deionized water, and chitosan is 8 - 9:900 - 920:1.0 - 1.2; the luminous powder is strontium aluminate powder.

[0014] As a preferred technical solution of the present invention, in Step 2, the inert atmosphere is a nitrogen atmosphere; the heating and stirring is stirring at a temperature of 62 - 70 °C for 5 - 6 h; the washing is washing three times with absolute ethanol; the drying temperature is 80 °C.

[0015] As a preferred technical solution of the present invention, in Step 2, the dihydroxybenzoylformaldehyde is 1,2 - dihydroxy - 4 - formylbenzene, also known as protocatechuic aldehyde, 3,4 - dihydroxybenzaldehyde; the concentration of the ethanol solution is 80 wt%; the mass ratio of the composite powder, ethanol solution, and dihydroxybenzoylformaldehyde is 10 - 12:70 - 75:2.2 - 2.6.

[0016] As a preferred technical solution of the present invention, in Step 3, the ultrasonic treatment is ultrasonic treatment at a power of 300 - 400 W for 10 - 12 min; the heating and stirring is stirring at a temperature of 35 - 40 °C for 6 - 8 h; the washing is washing three times with absolute ethanol; the drying temperature is 80 °C.

[0017] As a preferred technical solution of the present invention, in step three, the mass ratio of the toner, absolute ethanol, thiomalic acid, oleic acid and initiator is 12-14:60-70:2.8-3.2:3.8-4.0:0.22-0.26; the toner is one or more of cobalt blue pigment, titanium nickel yellow pigment, silicon iron red pigment, cobalt green pigment, copper chromium black pigment, titanium complex brown pigment and titanium iron black pigment; the initiator is ammonium cerium nitrate.

[0018] As a preferred technical solution of the present invention, in step four, the kneading time is 30-40 min; the melting temperature is 260 °C.

[0019] As a preferred technical solution of the present invention, in step four, the functional polymer is ethylene-glycidyl methacrylate copolymer; the mass ratio of the modified toner, modified luminous powder, functional polymer and thermoplastic polyester is 3-4:2.4-3.2:4-5:84-90.

[0020] The present invention discloses a luminous yarn prepared by the above preparation method.

[0021] Advantages of the present invention:

[0022] By adding rare earth metal luminous powder and introducing inorganic filler toner, through its organic modification and combining with toughening and compatibilizing polymers, the compatibility in the yarn material system is increased. The organic modification selects ultrafine luminous powder and toner components to be added into the yarn material in the form of covalent bonds and non-covalent bonds, and after melt extrusion, spinning is carried out, and finally a luminous yarn is prepared, endowing the luminous yarn with excellent mechanical properties. Specific embodiments

[0023] In order to further elaborate on the technical means and effects adopted by the present invention to achieve the predetermined invention purpose, the following combines examples to detail the specific embodiments, structures, features and their effects of the present invention.

[0024] Example 1

[0025] A preparation method of a luminous yarn includes the following steps:

[0026] Step one: Under a nitrogen atmosphere, stir the luminous powder and deionized water for 30 min, then add chitosan and ultrasonicate at 500 W for 50 min, filter and then perform freeze-drying to obtain a composite powder; the mass ratio of the luminous powder, deionized water and chitosan is 8:900:1.0; the luminous powder is strontium aluminate powder.

[0027] Step 2: Under a nitrogen atmosphere, place the composite powder in an ethanol solution, add dihydroxybenzoylbenzene, stir at 62 °C for 5 h, filter, wash three times with absolute ethanol, and then dry at 80 °C to constant weight to obtain modified luminous powder; the dihydroxybenzoylbenzene is 1,2-dihydroxy-4-formylbenzene; the concentration of the ethanol solution is 80 wt%; the mass ratio of the composite powder, ethanol solution, and dihydroxybenzoylbenzene is 10:70:2.2;

[0028] Step 3: Ultrasonic the color powder, absolute ethanol, and thiomalic acid at a power of 300 W for 10 min, then add oleic acid and initiator, stir at 35 °C for 6 h, centrifuge, wash three times with absolute ethanol, and dry at 80 °C to constant weight to obtain modified color powder; the mass ratio of the color powder, absolute ethanol, thiomalic acid, oleic acid, and initiator is 12:60:2.8:3.8:0.22; the initiator is ammonium cerium nitrate; the color powder is titanium nickel yellow pigment;

[0029] Step 4: Mix the modified color powder, modified luminous powder, functional polymer, and thermoplastic polyester in a high-speed mixer for 30 min, and then melt-spin in a twin-screw extruder at 260 °C to obtain the product; the functional polymer is ethylene-glycidyl methacrylate copolymer; the mass ratio of the modified color powder, modified luminous powder, functional polymer, and thermoplastic polyester is 3:2.4:4:84.

[0030] Example 2

[0031] A preparation method of a luminous yarn includes the following steps:

[0032] Step 1: Under a nitrogen atmosphere, stir the luminous powder and deionized water for 35 min, add chitosan, ultrasonic at a power of 550 W for 55 min, filter, and then perform freeze-drying to obtain a composite powder; the mass ratio of the luminous powder, deionized water, and chitosan is 8.5:910:1.1; the luminous powder is strontium aluminate powder;

[0033] Step 2: Under a nitrogen atmosphere, place the composite powder in an ethanol solution, add dihydroxybenzoylbenzene, stir at 66 °C for 5.5 h, filter, wash three times with absolute ethanol, and then dry at 80 °C to constant weight to obtain modified luminous powder; the dihydroxybenzoylbenzene is 1,2-dihydroxy-4-formylbenzene; the concentration of the ethanol solution is 80 wt%; the mass ratio of the composite powder, ethanol solution, and dihydroxybenzoylbenzene is 11:72:2.4;

[0034] Step 3: Ultrasonic the toner, absolute ethanol and thiomalic acid at a power of 350 W for 11 min, then add oleic acid and initiator and stir at 38 °C for 7 h, centrifuge, wash three times with absolute ethanol, and dry to constant weight at 80 °C to obtain modified toner; the mass ratio of the toner, absolute ethanol, thiomalic acid, oleic acid and initiator is 13:65:3:3.9:0.24; the initiator is ammonium cerium nitrate; the toner is titanium nickel yellow pigment;

[0035] Step 4: Mix the modified toner, modified luminous powder, functional polymer and thermoplastic polyester in a high-speed mixer for 35 min, and then melt-spin in a twin-screw extruder at 260 °C to obtain; the functional polymer is ethylene-glycidyl methacrylate copolymer; the mass ratio of the modified toner, modified luminous powder, functional polymer and thermoplastic polyester is 3.5:2.8:4.5:87.

[0036] Example 3

[0037] A preparation method of luminous yarn includes the following steps:

[0038] Step 1: Under a nitrogen atmosphere, stir the luminous powder and deionized water for 40 min, then add chitosan and ultrasonic at a power of 600 W for 60 min, filter and then freeze-dry to obtain composite powder; the mass ratio of the luminous powder, deionized water and chitosan is 9:920:1.2; the luminous powder is strontium aluminate powder;

[0039] Step 2: Under a nitrogen atmosphere, place the composite powder in an ethanol solution, add 1,2-dihydroxy-4-formylbenzene and stir at 70 °C for 6 h, filter, wash three times with absolute ethanol, and dry to constant weight at 80 °C to obtain modified luminous powder; the 1,2-dihydroxy-4-formylbenzene is 1,2-dihydroxy-4-formylbenzene; the concentration of the ethanol solution is 80 wt%; the mass ratio of the composite powder, ethanol solution and 1,2-dihydroxy-4-formylbenzene is 12:75:2.6;

[0040] Step 3: Ultrasonic the toner, absolute ethanol and thiomalic acid at a power of 400 W for 12 min, then add oleic acid and initiator and stir at 40 °C for 8 h, centrifuge, wash three times with absolute ethanol, and dry to constant weight at 80 °C to obtain modified toner; the mass ratio of the toner, absolute ethanol, thiomalic acid, oleic acid and initiator is 14:70:3.2:4.0:0.26; the initiator is ammonium cerium nitrate; the toner is titanium nickel yellow pigment;

[0041] Step 4: Place the modified toner, modified luminous powder, functional polymer, and thermoplastic polyester in a high-speed mixer and knead for 40 minutes, then place them in a twin-screw extruder and melt-spin at 260 °C to obtain; the functional polymer is ethylene-glycidyl methacrylate copolymer; the mass ratio of the modified toner, modified luminous powder, functional polymer, and thermoplastic polyester is 4:3.2:5:90.

[0042] Comparative Example 1

[0043] Compared with Example 3, the difference in Comparative Example 1 is that chitosan is not used, and the other components, preparation steps, and parameters are the same.

[0044] Comparative Example 2

[0045] Compared with Example 3, the difference in Comparative Example 2 is that benzaldehyde is used instead of dihydroxymethylbenzene, and the other components, preparation steps, and parameters are the same.

[0046] Comparative Example 3

[0047] Compared with Example 3, the difference in Comparative Example 3 is that thiomalic acid is not used, and the other components, preparation steps, and parameters are the same.

[0048] Comparative Example 4

[0049] Compared with Example 3, the difference in Comparative Example 4 is that oleic acid is not used, and the other components, preparation steps, and parameters are the same.

[0050] Comparative Example 5

[0051] Compared with Example 3, the difference in Comparative Example 5 is that the functional polymer is not used, and the other components, preparation steps, and parameters are the same.

[0052] Comparative Example 6

[0053] Compared with Example 3, the difference in Comparative Example 6 is that dihydroxymethylbenzene is not used, and the other components, preparation steps, and parameters are the same.

[0054] The luminous yarns prepared in Examples 1-3 and Comparative Examples 1-6 were respectively tested for the following properties, and the test results are shown in Table 1.

[0055] Mechanical property test: According to GB / T14344-2022;

[0056] Table 1

[0057] Breaking strength (cN / dtex) Elongation at break (%) Example 1 3.15 32.6 Example 2 3.17 32.7 Example 3 3.21 32.9 Comparative Example 1 2.53 24.5 Comparative Example 2 2.61 25.8 Comparative Example 3 2.77 26.1 Comparative Example 4 2.64 24.4 Comparative Example 5 2.48 23.8 Comparative Example 6 2.51 24.2

[0058] As can be seen from the test results in Table 1, compared with Comparative Examples 1-6, the luminous yarns prepared in Examples 1-3 of the present invention have excellent breaking strength and elongation at break. Through comparative analysis, it can be seen that this is because in the present invention, hydrogen bonds and electrostatic adsorption are used to form a complex of chitosan and luminous powder. While increasing its active hydroxyl groups, the complex can form physical crosslinks and chemical bond connections with dihydroxyformylbenzene, improving the thermal stability of the luminous powder, and at the same time improving its dispersibility and compatibility in the thermoplastic polyester system, thereby improving the breaking strength and elongation at break of the yarn material. Then, through the interaction between the metal ions of the color powder and thiomalic acid, thiomalic acid is attached to the surface of the color powder and undergoes a chemical grafting reaction with oleic acid, introducing more active carboxyl groups and hydrophobic long carbon chain structures to the surface of the color powder. The long carbon chain structure promotes the fluidity of the color powder in the thermoplastic polyester system, improves the hydrophobicity, and its long carbon chain can also be embedded between the molecular chains of the thermoplastic polyester resin, improving the interfacial bonding force and promoting compatibility. Finally, the modified luminous powder, modified color powder, polymer, and thermoplastic polyester are melt-extruded. The epoxy groups of the polymer can form covalent bond connections with the hydroxyl and carboxyl groups of the modified luminous powder and modified color powder, and physical adsorption crosslinks can also be formed between the hydroxyl and carboxyl groups, improving the structural compactness and mechanical properties of the yarn material. In addition, the polymer can also play a toughening and compatibilizing role, significantly improving the compatibility and dispersibility of the luminous powder and color powder in the thermoplastic polyester system.

[0059] The above are only the preferred embodiments of the present invention, and do not impose any form of limitation on the present invention. Although the present invention has been disclosed above with preferred embodiments, it is not intended to limit the present invention. Any person skilled in the art can make some changes or modifications to the above-disclosed technical content to obtain equivalent embodiments with equivalent changes. However, as long as it does not depart from the technical content of the present invention, any indirect modification, equivalent change, and modification made to the above embodiments based on the technical essence of the present invention still fall within the scope of the technical solution of the present invention.

Claims

1. A method for preparing a luminous yarn, characterized in that, The preparation method includes the following steps: Step 1: Under an inert atmosphere, mix the luminous powder and deionized water, then add chitosan and mix by ultrasound. After filtration, perform freeze-drying to obtain a composite powder; Step 2: Under an inert atmosphere, place the composite powder in an ethanol solution, add 1,2-dihydroxy-4-formylbenzene and stir while heating. After filtration and washing, dry to constant weight to obtain a modified luminous powder; Step 3: Ultrasonically treat the color powder, absolute ethanol and thiomalic acid, then add oleic acid and an initiator and stir while heating. After centrifugation and washing, dry to constant weight to obtain a modified color powder; Step 4: Mix the modified color powder, modified luminous powder, functional polymer and thermoplastic polyester in a high-speed mixer, and then place them in a twin-screw extruder for melt spinning to obtain the product. The functional polymer is ethylene-glycidyl methacrylate copolymer. The mass ratio of the modified color powder, modified luminous powder, functional polymer and thermoplastic polyester is 3-4: 2.4-3.2: 4-5: 84-90.

2. The preparation method of a kind of luminous yarn according to claim 1, characterized in that: In Step 1, the inert atmosphere is a nitrogen atmosphere; the mixing is stirring for 30-40 min; the ultrasonic mixing is ultrasonic mixing at a power of 500-600 W for 50-60 min.

3. The preparation method of a luminous yarn according to claim 1, characterized in that: In Step 1, the mass ratio of the luminous powder, deionized water and chitosan is 8-9: 900-920: 1.0-1.2; the luminous powder is strontium aluminate powder.

4. The preparation method of a luminous yarn according to claim 1, characterized in that: In Step 2, the inert atmosphere is a nitrogen atmosphere; the heating and stirring is stirring at a temperature of 62-70 °C for 5-6 h; the washing is washing three times with absolute ethanol; the drying temperature is 80 °C.

5. The preparation method of a luminous yarn according to claim 1, characterized in that: In Step 2, the 1,2-dihydroxy-4-formylbenzene is 1,2-dihydroxy-4-formylbenzene; the concentration of the ethanol solution is 80 wt%; the mass ratio of the composite powder, ethanol solution and 1,2-dihydroxy-4-formylbenzene is 10-12: 70-75: 2.2-2.

6.

6. The preparation method of a kind of luminous yarn according to claim 1, characterized in that: In Step 3, the ultrasonic treatment is ultrasonic treatment at a power of 300-400 W for 10-12 min; the heating and stirring is stirring at a temperature of 35-40 °C for 6-8 h; the washing is washing three times with absolute ethanol; the drying temperature is 80 °C.

7. The preparation method of a kind of luminous yarn according to claim 1, characterized in that: In Step 3, the mass ratio of the color powder, absolute ethanol, thiomalic acid, oleic acid and initiator is 12-14: 60-70: 2.8-3.2: 3.8-4.0: 0.22-0.26; the color powder is one or more of cobalt blue pigment, titanium nickel yellow pigment, silicon iron red pigment, cobalt green pigment, copper chromium black pigment, titanium complex brown pigment and titanium iron black pigment; the initiator is ammonium cerium nitrate.

8. The preparation method of a luminous yarn according to claim 1, characterized in that: In Step 4, the mixing time is 30-40 min; the melting temperature is 260 °C.

9. A luminous yarn prepared by the preparation method according to any one of claims 1 to 8.