Composite short fiber and preparation method thereof

Abstract

The invention relates to a composite staple fiber and a preparation method thereof, belonging to the technical field of textile materials. The invention uses polyethylene terephthalate, a flame retardant and antibacterial agent, a polymerization catalyst, an organic solvent, and viscose fiber as raw materials to prepare a composite staple fiber. The invention first polymerizes polyethylene terephthalate and the flame retardant and antibacterial agent through an esterification reaction to modify the polyethylene terephthalate to obtain a modified polyester, then dissolves the modified polyester in an organic solvent to prepare a spinning solution, and then electrostatically spins the solution to obtain a modified PET fiber. Finally, the modified PET fiber is blended with viscose fiber, and then subjected to oiling, winding, bundling, stretching, heat setting, curling, and cutting to obtain a composite staple fiber. The composite staple fiber of the invention is wrinkle-resistant and wear-resistant, moisture-absorbent and breathable, easy to dye, has good flame retardancy and antibacterial properties, and has a long-lasting effectiveness and is not easily invalidated, and can be widely used in the field of clothing and home textiles.

Description

Technical Field

[0001] The present invention belongs to the technical field of textile materials, and in particular relates to a composite staple fiber and a preparation method thereof. Background Art

[0002] Staple fibers are important raw materials for the textile, clothing, home textile and other industries. Polyester staple fibers are deeply loved by market consumers because of their excellent strength and wear resistance, good elasticity and wrinkle resistance, good heat resistance and other advantages. However, due to the influence of their own chemical properties, polyester fibers still have some defects that limit their use. Polyester fibers have poor moisture absorption and poor air permeability, so wearing polyester fiber clothing in summer often makes people feel stuffy. In addition, polyester fibers themselves do not have antibacterial properties, and lack protective effects on the human body when used in the clothing field. Polyester fibers also have poor flame retardant properties, so when used in the home textile field, polyester fibers lack sufficient safety. Based on this, the present invention provides a composite staple fiber and a preparation method thereof. Summary of the Invention

[0003] The object of the present invention is to provide a composite staple fiber and a preparation method thereof, so as to solve the problems mentioned in the above background technology.

[0004] The purpose of the present invention can be achieved through the following technical solutions:

[0005] A composite staple fiber comprises the following raw materials in parts by weight: 100 parts of polyethylene terephthalate, 1.4-2.2 parts of a flame retardant and antibacterial agent, 0.04-0.06 parts of a polymerization catalyst, 800-1000 parts of an organic solvent, and 45-60 parts of viscose fiber;

[0006] A method for preparing composite short fibers comprises the following steps:

[0007] The first step is to weigh the raw materials according to their mass: 100 parts of polyethylene terephthalate, 1.4-2.2 parts of flame retardant and antibacterial agent, 0.04-0.06 parts of polymerization catalyst, 800-1000 parts of organic solvent, and 45-60 parts of viscose fiber;

[0008] The second step is to mix polyethylene terephthalate, a flame retardant and an antibacterial agent, and a polymerization catalyst, and then heat and polymerize them to obtain a modified polyester;

[0009] The third step is to dissolve the modified polyester in an organic solvent and stir it to prepare a spinning solution, then add the spinning solution into a spinning tube and prepare the modified PET fiber by electrospinning;

[0010] Step 4: The modified PET fiber and the viscose fiber are blended and subjected to oiling, winding, bundling, stretching, heat setting, curling, and cutting to obtain a composite staple fiber;

[0011] Furthermore, the relative molecular mass of the polyethylene terephthalate is 20,000-30,000.

[0012] Furthermore, the polymerization catalyst is antimony acetate.

[0013] Furthermore, the organic solvent is trifluoroacetic acid.

[0014] Furthermore, the heating esterification polymerization in the second step is carried out at a temperature of 260-270° C. and a pressure of 0.02-0.04 KPa for 60-80 minutes.

[0015] Furthermore, the stirring condition in the third step is stirring at a rotation speed of 400-600 rpm for 4 hours.

[0016] Furthermore, the electrospinning conditions in the third step are liquid feed rate 12-18 μL / min, spray distance 10-15 cm, spinning voltage 12-16 kV, and spinning temperature 20-30°C.

[0017] Furthermore, the flame retardant and antibacterial agent is prepared by the following steps:

[0018] Step 1, m-aminobenzoic acid, 2-hydroxypyridine-4-carboxaldehyde, triethyl phosphite, citric acid, and cyclopentyl methyl ether were mixed in a three-necked flask, equipped with a condenser and a thermometer, and magnetic stirring was turned on. The mixture was reacted at a temperature of 40-55° C. for 20-30 minutes. After the reaction was completed, a saturated ammonium chloride solution was added to the three-necked flask to quench the reaction, and the organic layer was separated with a separatory funnel. The organic layer was rotary evaporated to remove the solvent and then subjected to silica gel column chromatography to obtain intermediate 1;

[0019]

[0020] Step 2: Mix the intermediate 1, lauryl bromide and acetonitrile in a three-necked flask, install a condenser and a thermometer, start magnetic stirring, and react at a temperature of 40-60° C. for 24 hours. After the reaction is completed, rotary evaporation is performed to obtain the flame retardant and antibacterial agent.

[0021]

[0022] Furthermore, the amount ratio of m-aminobenzoic acid, 2-hydroxypyridine-4-carboxaldehyde, triethyl phosphite, citric acid, and cyclopentyl methyl ether used in step 1 is 0.1-0.12 mol: 0.1 mol: 0.15-0.2 mol: 0.06 mol: 80-100 mL.

[0023] Furthermore, the usage ratio of intermediate 1, lauryl bromide, and acetonitrile used in step 2 is 0.08 mol: 0.1-0.15 mol: 40-60 mL.

[0024] Beneficial effects of the present invention:

[0025] 1) The present invention uses polyethylene terephthalate, a flame retardant and antibacterial agent, a polymerization catalyst, an organic solvent, and viscose fiber as raw materials to prepare a composite staple fiber. The present invention first modifies the polyethylene terephthalate by polymerizing the polyethylene terephthalate and the flame retardant and antibacterial agent through an esterification reaction to obtain a modified polyester, then dissolves the modified polyester in an organic solvent to prepare a spinning solution, and then obtains a modified PET fiber through electrostatic spinning. Finally, the modified PET fiber is blended with viscose fiber and then subjected to oiling, winding, bundling, stretching, heat setting, curling, and cutting to obtain a composite staple fiber. The preparation method of the present invention blends viscose fiber and modified PET fiber to obtain a composite staple fiber. The final composite staple fiber combines the advantages of PET fiber and viscose fiber, has good mechanical strength, excellent elastic recovery ability, excellent wrinkle resistance, and is moisture-absorbent and breathable and easy to dye.

[0026] 2) The present invention uses m-aminobenzoic acid, 2-hydroxypyridine-4-carboxaldehyde and triethyl phosphite as raw materials, and reacts the amino group of m-aminobenzoic acid and the formyl group of 2-hydroxypyridine-4-carboxaldehyde with triethyl phosphite under the catalysis of citric acid through Kabachn ik–Fiel reaction. The intermediate 1 is obtained by a ds reaction, and then the intermediate 1 and lauryl bromide are used as raw materials, and a flame retardant and antibacterial agent is obtained by a quaternary ammonium salt reaction between the pyridine N atom of the intermediate 1 and the lauryl bromide. The flame retardant and antibacterial agent of the present invention contains an aminophosphoric acid ester structure, which can decompose water and non-combustible acid and gas to dilute the oxygen concentration when exposed to the high temperature of the flame and form a heat-insulating and oxygen-isolating protective carbon layer to prevent the group from contacting the external air and oxygen, thereby giving the short fiber good flame retardancy. In addition, the flame retardant and antibacterial agent of the present invention also has a pyridyl quaternary ammonium salt structure, which can adsorb bacterial cell walls and puncture bacterial cell membranes, thereby giving the short fiber good antibacterial properties. In addition, the flame retardant and antibacterial agent of the present invention also has hydroxyl and carboxyl groups, and can be combined with polyethylene terephthalate in the polymer through an esterification reaction, so that the effectiveness time is long-lasting and it is not easy to fail.

[0027] 3) The composite staple fiber of the present invention is wrinkle-resistant and wear-resistant, moisture-absorbent and breathable, easy to dye, has good flame retardancy and antibacterial properties, and has a long-lasting effectiveness and is not easy to fail, and can be widely used in the field of clothing and home textiles. DETAILED DESCRIPTION

[0028] The following will be combined with the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the embodiments described are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without making any creative efforts shall fall within the scope of protection of the present invention.

[0029] Example 1

[0030] A flame retardant and antibacterial agent is prepared by the following steps:

[0031] Step 1: 0.1 mol m-aminobenzoic acid, 0.1 mol 2-hydroxypyridine-4-carboxaldehyde, 0.15 mol triethyl phosphite, 0.06 mol citric acid, and 80 mL cyclopentyl methyl ether were mixed in a three-necked flask, equipped with a condenser and a thermometer, and magnetic stirring was turned on. The mixture was reacted at 40° C. for 20 min. After the reaction was completed, a saturated ammonium chloride solution was added to the three-necked flask to quench the reaction, and the organic layer was separated with a separatory funnel. The organic layer was evaporated to remove the solvent and then subjected to silica gel column chromatography to obtain intermediate 1;

[0032] Step 2: Mix 0.08 mol intermediate 1, 0.1 mol lauryl bromide, and 40 mL acetonitrile in a three-necked flask, install a condenser and a thermometer, turn on magnetic stirring, and react at a temperature of 40°C for 24 hours. After the reaction is completed, rotary evaporation is performed to obtain the flame retardant and antibacterial agent.

[0033] Example 2

[0034] A flame retardant and antibacterial agent is prepared by the following steps:

[0035] Step 1: 0.11 mol m-aminobenzoic acid, 0.1 mol 2-hydroxypyridine-4-carboxaldehyde, 0.175 mol triethyl phosphite, 0.06 mol citric acid, and 90 mL cyclopentyl methyl ether were mixed in a three-necked flask, equipped with a condenser and a thermometer, and magnetic stirring was turned on. The mixture was reacted at 48° C. for 25 min. After the reaction was completed, a saturated ammonium chloride solution was added to the three-necked flask to quench the reaction, and the organic layer was separated with a separatory funnel. The organic layer was evaporated to remove the solvent and then subjected to silica gel column chromatography to obtain intermediate 1;

[0036] Step 2: Mix 0.08 mol intermediate 1, 0.125 mol lauryl bromide, and 50 mL acetonitrile in a three-necked flask, install a condenser and a thermometer, turn on magnetic stirring, and react at a temperature of 50°C for 24 hours. After the reaction is completed, rotary evaporation is performed to obtain the flame retardant and antibacterial agent.

[0037] Example 3

[0038] A flame retardant and antibacterial agent is prepared by the following steps:

[0039] Step 1: 0.12 mol m-aminobenzoic acid, 0.1 mol 2-hydroxypyridine-4-carboxaldehyde, 0.2 mol triethyl phosphite, 0.06 mol citric acid, and 100 mL cyclopentyl methyl ether were mixed in a three-necked flask, equipped with a condenser and a thermometer, and magnetic stirring was turned on. The mixture was reacted at 55° C. for 30 min. After the reaction was completed, a saturated ammonium chloride solution was added to the three-necked flask to quench the reaction, and the organic layer was separated with a separatory funnel. The organic layer was evaporated to remove the solvent and then subjected to silica gel column chromatography to obtain intermediate 1;

[0040] Step 2: Mix 0.08 mol intermediate 1, 0.15 mol lauryl bromide, and 60 mL acetonitrile in a three-necked flask, install a condenser and a thermometer, turn on magnetic stirring, and react at a temperature of 60°C for 24 hours. After the reaction is completed, rotary evaporation is performed to obtain the flame retardant and antibacterial agent.

[0041] Example 4

[0042] A composite staple fiber, comprising the following raw materials in parts by mass: 100 parts of polyethylene terephthalate, 1.4 parts of the flame retardant and antibacterial agent obtained in Example 1, 0.04 parts of antimony acetate, 800 parts of trifluoroacetic acid, and 45 parts of viscose fiber;

[0043] A method for preparing composite short fibers comprises the following steps:

[0044] The first step is to weigh 100 parts of polyethylene terephthalate, 1.4 parts of the flame retardant and antibacterial agent obtained in Example 1, 0.04 parts of antimony acetate, 800 parts of trifluoroacetic acid, and 45 parts of viscose fiber according to their mass parts;

[0045] Step 2: polyethylene terephthalate, the flame retardant and antibacterial agent obtained in Example 1, and antimony acetate are mixed and reacted at a temperature of 260° C. and a pressure of 0.02 KPa for 60 minutes to obtain a modified polyester;

[0046] The modified polyester was dissolved in trifluoroacetic acid and stirred at 400 rpm for 4 h to prepare a spinning solution. The spinning solution was then added to a spinning tube and modified PET fibers were prepared by electrospinning. The electrospinning conditions were as follows: a liquid feed rate of 12 μL / min, a spray distance of 10 cm, a spinning voltage of 12 kV, and a spinning temperature of 20°C.

[0047] In the fourth step, the modified PET fiber and the viscose fiber are blended and then subjected to oiling, winding, bundling, stretching, heat setting, curling and cutting to obtain a composite staple fiber.

[0048] The relative molecular weight specification of the polyethylene terephthalate used in this embodiment is 20,000-30,000.

[0049] Example 5

[0050] A composite staple fiber, comprising the following raw materials in parts by mass: 100 parts of polyethylene terephthalate, 1.8 parts of the flame retardant and antibacterial agent obtained in Example 2, 0.05 parts of antimony acetate, 900 parts of trifluoroacetic acid, and 52 parts of viscose fiber;

[0051] A method for preparing composite short fibers comprises the following steps:

[0052] The first step is to weigh 100 parts of polyethylene terephthalate, 1.8 parts of the flame retardant and antibacterial agent obtained in Example 2, 0.05 parts of antimony acetate, 900 parts of trifluoroacetic acid, and 52 parts of viscose fiber according to their mass ratio;

[0053] Step 2: polyethylene terephthalate, the flame retardant and antibacterial agent obtained in Example 2, and antimony acetate were mixed and reacted at a temperature of 265° C. and a pressure of 0.03 KPa for 70 minutes to obtain a modified polyester;

[0054] The modified polyester was dissolved in trifluoroacetic acid and stirred at 500 rpm for 4 h to prepare a spinning solution. The spinning solution was then added to a spinning tube and modified PET fibers were prepared by electrospinning. The electrospinning conditions were as follows: a liquid feed rate of 16 μL / min, a spray distance of 12.5 cm, a spinning voltage of 14 kV, and a spinning temperature of 25°C.

[0055] In the fourth step, the modified PET fiber and the viscose fiber are blended and then subjected to oiling, winding, bundling, stretching, heat setting, curling and cutting to obtain a composite staple fiber.

[0056] The relative molecular weight specification of the polyethylene terephthalate used in this embodiment is 20,000-30,000.

[0057] Example 6

[0058] A composite staple fiber, comprising the following raw materials in parts by mass: 100 parts of polyethylene terephthalate, 2.2 parts of the flame retardant and antibacterial agent obtained in Example 3, 0.06 parts of antimony acetate, 1000 parts of trifluoroacetic acid, and 60 parts of viscose fiber;

[0059] A method for preparing composite short fibers comprises the following steps:

[0060] The first step is to weigh 100 parts of polyethylene terephthalate, 2.2 parts of the flame retardant and antibacterial agent obtained in Example 3, 0.06 parts of antimony acetate, 1000 parts of trifluoroacetic acid, and 60 parts of viscose fiber according to their mass ratio;

[0061] Step 2: polyethylene terephthalate, the flame retardant and antibacterial agent obtained in Example 3, and antimony acetate were mixed and reacted at a temperature of 270° C. and a pressure of 0.04 kPa for 80 minutes to obtain a modified polyester;

[0062] The modified polyester was dissolved in trifluoroacetic acid and stirred at 600 rpm for 4 h to prepare a spinning solution. The spinning solution was then added to a spinning tube and modified PET fibers were prepared by electrospinning. The electrospinning conditions were as follows: a liquid feed rate of 18 μL / min, a spray distance of 15 cm, a spinning voltage of 16 kV, and a spinning temperature of 30°C.

[0063] In the fourth step, the modified PET fiber and the viscose fiber are blended and then subjected to oiling, winding, bundling, stretching, heat setting, curling and cutting to obtain a composite staple fiber.

[0064] The relative molecular weight specification of the polyethylene terephthalate used in this embodiment is 20,000-30,000.

[0065] Comparative Example 1

[0066] A composite staple fiber comprising the following raw materials in parts by mass: 100 parts of polyethylene terephthalate, 1000 parts of trifluoroacetic acid, and 60 parts of viscose fiber;

[0067] A method for preparing composite short fibers comprises the following steps:

[0068] The first step is to weigh 100 parts of polyethylene terephthalate, 1000 parts of trifluoroacetic acid, and 60 parts of viscose fiber according to their mass ratios;

[0069] In the second step, polyethylene terephthalate was dissolved in trifluoroacetic acid and stirred at 600 rpm for 4 h to prepare a spinning solution. The spinning solution was then added to a spinning tube and PET fibers were prepared by electrospinning. The electrospinning conditions were as follows: a liquid feed rate of 18 μL / min, a spray distance of 15 cm, a spinning voltage of 16 kV, and a spinning temperature of 30°C.

[0070] In the third step, the PET fiber and the viscose fiber are blended and subjected to oiling, winding, bundling, stretching, heat setting, curling and cutting to obtain a composite staple fiber.

[0071] The relative molecular weight specification of the polyethylene terephthalate used in this embodiment is 20,000-30,000.

[0072] Comparative Example 2

[0073] This comparative example is a commercially available PET flame-retardant antibacterial fiber.

[0074] The composite staple fibers of Examples 4-6 and Comparative Example 1 were tested together with the commercially available flame-retardant antibacterial polyester of Comparative Example 2 for performance. The limited oxygen index was tested according to the national standard GB / T 5454-1997 "Textiles Burning Performance Test Oxygen Index Method", and the antibacterial rates of Escherichia coli and Staphylococcus aureus were tested according to the national standard GB / T 20944.3-2008 "Evaluation of Antibacterial Properties of Textiles Part 3: Oscillation Method". The test results are shown in Table 1:

[0075] Table 1

[0076] project Limited oxygen index% Escherichia coli inhibition rate% Staphylococcus aureus inhibition rate % Example 4 28.16 99.76 99.13 Example 5 29.79 99.94 99.40 Example 6 30.14 99.96 99.45 Comparative Example 1 20.13 2.77 3.14 Comparative Example 2 25.48 86.15 85.31

[0077] It can be seen from Table 1 that the limiting oxygen index and antibacterial rate of the composite staple fiber of the present invention in Examples 4-6 are higher than those of the commercially available PET antibacterial flame retardant fiber, indicating that the composite staple fiber of the present invention has good flame retardancy and antibacterial properties, while the composite staple fiber in Comparative Example 1 has poor performance because the flame retardant and antibacterial agent of the present invention is not used. In summary, the composite staple fiber of the present invention has good flame retardancy and antibacterial properties and can be widely used in the field of clothing and home textiles.

[0078] The above is a detailed introduction to a composite staple fiber and a preparation method thereof provided by the present invention. Specific examples are used herein to illustrate the principles and implementation methods of the present invention. The description of the above embodiments is only used to help understand the method of the present invention and its core ideas, including the best way, and also enables any technician in this field to practice the present invention, including the manufacture and use of any device or system, and the implementation of any combination method. It should be pointed out that for ordinary technicians in this technical field, the present invention can also be improved and modified without departing from the principles of the present invention. In particular, as long as there is no structural conflict, the various features in the embodiments disclosed in the present invention can be combined with each other in any way. The reason why these combinations are not exhaustively described in this specification is simply for the sake of omitting space and saving resources. Therefore, the present invention is not limited to the specific embodiments disclosed herein, but includes all technical solutions that fall within the scope of the claims.

Claims

1. A composite short fiber, characterized in that: The invention comprises the following raw materials in parts by weight: 100 parts of polyethylene terephthalate, 1.4-2.2 parts of flame retardant and antibacterial agent, 0.04-0.06 parts of polymerization catalyst, 800-1000 parts of organic solvent, and 45-60 parts of viscose fiber; Wherein, the flame retardant and antibacterial agent is prepared by the following steps: Step 1, m-aminobenzoic acid, 2-hydroxypyridine-4-carboxaldehyde, triethyl phosphite, citric acid, and cyclopentyl methyl ether are mixed in a container, stirred evenly, and reacted at a temperature of 40-55° C. for 20-30 minutes to obtain intermediate 1; Step 2: Mix the intermediate 1, lauryl bromide, and acetonitrile in a container, stir evenly, and react at a temperature of 40-60° C. for 24 hours to obtain the flame retardant and antibacterial agent.

2. A composite short fiber according to claim 1, characterized in that: The amount ratio of m-aminobenzoic acid, 2-hydroxypyridine-4-carboxaldehyde, triethyl phosphite, citric acid, and cyclopentyl methyl ether used in step 1 is 0.1-0.12 mol: 0.1 mol: 0.15-0.2 mol: 0.06 mol: 80-100 mL.

3. The composite short fiber according to claim 1, characterized in that: The amount ratio of intermediate 1, lauryl bromide and acetonitrile used in step 2 is 0.08 mol: 0.1-0.15 mol: 40-60 mL.

4. A method for preparing a composite short fiber according to any one of claims 1 to 3, characterized in that: The method comprises the following preparation steps: The first step is to weigh the raw materials according to their mass: 100 parts of polyethylene terephthalate, 1.4-2.2 parts of flame retardant and antibacterial agent, 0.04-0.06 parts of polymerization catalyst, 800-1000 parts of organic solvent, and 45-60 parts of viscose fiber; The second step is to mix polyethylene terephthalate, a flame retardant and an antibacterial agent, and a polymerization catalyst, and then heat and polymerize them to obtain a modified polyester; The third step is to dissolve the modified polyester in an organic solvent and stir it to prepare a spinning solution, then add the spinning solution into a spinning tube and prepare the modified PET fiber by electrospinning; In the fourth step, the modified PET fiber and the viscose fiber are blended and then subjected to oiling, winding, bundling, stretching, heat setting, curling and cutting to obtain a composite staple fiber.

5. The method for preparing composite short fibers according to claim 4, characterized in that: The relative molecular mass of the polyethylene terephthalate is 20,000 to 30,000.

6. The method for preparing composite short fibers according to claim 4, characterized in that: The polymerization catalyst is antimony acetate.

7. The method for preparing composite short fibers according to claim 4, wherein: The organic solvent is trifluoroacetic acid.

8. The method for preparing composite short fibers according to claim 4, characterized in that: The conditions for the heating esterification polymerization in the second step are to react at a temperature of 260-270° C. and a pressure of 0.02-0.04 KPa for 60-80 minutes.

9. The method for preparing composite short fibers according to claim 4, characterized in that: The stirring condition in the third step is stirring at a rotation speed of 400-600 rpm for 4 hours.

10. The method for preparing composite short fibers according to claim 4, characterized in that: The electrospinning conditions in the third step are as follows: liquid feed rate 12-18 μL / min, spray distance 10-15 cm, spinning voltage 12-16 kV, and spinning temperature 20-30°C.

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