High-temperature-resistant fiber fabric and preparation method thereof

Abstract

The invention relates to a high-temperature-resistant fiber fabric and a preparation method, and belongs to the technical field of textiles. The high-temperature-resistant fiber fabric is prepared by taking polypropylene and a self-made monomer additive as raw materials; polypropylene is modified through melt blending, multiple functional groups including sulfonyl, quaternary ammonium salt cations and phosphate groups exist in a monomer additive, the sulfonyl has high polarity and good thermal stability, free rotation and movement of a polypropylene chain segment can be limited, and the heat resistance of the fabric is improved; quaternary ammonium salt cations can attract anions in dye molecules through electrostatic attraction, can also provide carriers for ionization, and directionally migrate and conduct charges under the acting force of an electric field, so that the color fixing and antistatic effects are achieved; the phosphate groups can release phosphorus free radicals after being heated and decomposed, active hydrogen free radicals and hydroxyl free radicals generated in the combustion process can be effectively captured, surface carbonization of combustible materials can be promoted to form a carbon layer, and the fabric has the flame-retardant effect.

Description

Technical Field

[0001] The present invention belongs to the field of textile technology, and in particular relates to a high-temperature resistant fiber fabric and a preparation method thereof. Background Art

[0002] Polypropylene, a thermoplastic copolymer, offers advantages such as ease of processing and modification. However, it suffers from the drawbacks of high-temperature decomposition and insufficient mechanical properties, which limit its application in high-performance applications such as high-temperature environments. With the advancement of materials science, an increasing number of high-performance fibers have been developed. These fibers exhibit excellent high-temperature resistance and flame retardancy, providing a foundation for the preparation of high-performance, high-temperature-resistant fiber fabrics.

[0003] Polypropylene is a lightweight, chemically resistant general-purpose plastic, but its insufficient heat resistance limits its application in high-temperature scenarios. Through melt blending modification, fiber reinforcement technology, nanofiller modification, and high-temperature polymer blending strategies, combined with compatibilizers to optimize interfacial compatibility, the heat resistance, mechanical strength, and thermal-oxidative stability of composite materials can be effectively improved. In the melt blending process, temperature, shear rate, and interface treatment are key control parameters, and equipment such as twin-screw extrusion are required to achieve uniform dispersion of the components. Modified polypropylene fiber fabrics are widely used in high-temperature industrial filtration, lightweight automotive components, fire protection clothing, and new energy fields. Current technical challenges focus on optimizing interfacial compatibility, developing low-cost, high-performance fillers, and improving long-term high-temperature stability. Future trends point to green, intelligent, and multifunctional integration to meet composite requirements under extreme working conditions.

[0004] Based on this, the present invention provides a method for preparing a high-temperature resistant fiber fabric. Summary of the Invention

[0005] The object of the present invention is to provide a high temperature resistant fiber fabric and a preparation method thereof, so as to solve the problems mentioned in the above background technology.

[0006] The purpose of the present invention can be achieved through the following technical solutions:

[0007] A method for preparing a high-temperature resistant fiber fabric comprises the following steps:

[0008] The first step is to mix 2-methylthiopyridine, hydrogen peroxide, sodium tungstate and acetonitrile in a three-necked flask, install a condenser and a thermometer, turn on the magnetic stirring, heat the system to 75-80 ° C, react for 6-8 hours, and then cool to room temperature. Saturated sodium bicarbonate is added to adjust the pH to 7-8, extract with ethyl acetate, combine the organic phases, dry them with anhydrous sodium sulfate, and rotary evaporate to obtain a conjugated heat-resistant monomer;

[0009] In the second step, a conjugated heat-resistant monomer, 3-chloro-1-propanol and acetonitrile were added to a three-necked flask, a condenser and a thermometer were installed, magnetic stirring was turned on, the system was heated to 40-60°C, reacted for 10-12 hours, and then cooled to room temperature. After crystallization, the antistatic monomer was filtered to obtain the crystal.

[0010] The third step is to add antistatic monomer, phosphorus trichloride, triethylamine, anhydrous magnesium chloride and acetonitrile into a three-necked flask, install a condenser and a thermometer, turn on magnetic stirring, heat the system to 70-75°C, react for 2-3 hours, then heat to 80-85°C, react for 19-21 hours, cool to room temperature, wash with water, dry with anhydrous magnesium sulfate, and elute with silica gel after rotary evaporation to obtain the monomer additive;

[0011] In the fourth step, the polypropylene, monomer additives, antioxidant and trinonylphenyl phosphite are mixed evenly and then added into a twin-screw extruder for melt extrusion, and then melt-spun into fibers, which are then woven and shaped to obtain high-temperature resistant fiber fabrics.

[0012] Furthermore, the mass fraction of hydrogen peroxide in the first step is 30-40%.

[0013] Furthermore, in the first step, the mass ratio of 2-methylthiopyridine, hydrogen peroxide, sodium tungstate and acetonitrile is 12.5-15:51-81:0.7-1.7:150-170.

[0014] Furthermore, the mass ratio of the conjugated heat-resistant monomer, 3-chloro-1-propanol and acetonitrile in the second step is 12-14:7.5-8.5:125-140.

[0015] Furthermore, in the third step, the mass ratio of the antistatic monomer, phosphorus trichloride, triethylamine, anhydrous magnesium chloride and acetonitrile is 14-17:3-3.6:8-9:0.2-0.5:100-125.

[0016] Furthermore, the melt extrusion temperature in the fourth step is 220-250°C.

[0017] Furthermore, in the fourth step, the mass ratio of the monomer additive, polypropylene, antioxidant and trisnonylphenyl phosphite is 19-21:100-110:0.1-0.5:0.1-0.5.

[0018] A method for preparing a high-temperature resistant fiber fabric, comprising preparing the high-temperature resistant fiber fabric by any of the above-mentioned preparation steps.

[0019] Beneficial effects of the present invention:

[0020] 1) The present invention uses 2-methylthiopyridine and hydrogen peroxide as raw materials and sodium tungstate as a catalyst to carry out an oxidation reaction to obtain a conjugated heat-resistant monomer containing a sulfone group; pyridine in the conjugated heat-resistant monomer and the chlorine atom in 3-chloro-1-propanol undergo a quaternary ammonium salt reaction to obtain an antistatic monomer; phosphorus trichloride and the antistatic monomer are then used as raw materials and triethylamine is used as an acid-binding agent to carry out a phosphation reaction to obtain a monomer additive; finally, the monomer additive is used to modify polypropylene to obtain a high-temperature resistant fiber fabric.

[0021] 2) The conjugated heat-resistant monomer of the present invention contains multiple sulfone groups. The sulfone group has strong polarity and high electron-withdrawing properties. This strong polarity causes the sulfone group to produce strong dipole-dipole interactions with atoms on adjacent molecular chains, greatly increasing the resistance to molecular chain movement. At the same time, the double bond energy formed by the oxygen atom and the sulfur atom of the sulfone group is high. The sulfone group itself has high rigidity and thermal stability. When added to polypropylene as an additive, it restricts the free rotation and movement of the polypropylene chain segments, requiring higher temperatures for chain segment movement, thereby significantly improving the heat resistance of the fabric.

[0022] 3) The antistatic monomer obtained by the quaternary ammonium salt reaction of the present invention can provide carriers for ionization. The quaternary ammonium salt cations in the monomer can migrate directionally under the action of the electric field to conduct charge, and the counter-anions migrate synchronously in the opposite direction to maintain charge balance, thereby achieving the antistatic effect of the fabric. In addition, the quaternary ammonium salt ions have a positive charge, while the dye molecules have a negative charge in the aqueous solution. The two are attracted to each other through electrostatic attraction, so that the dye molecules are more firmly attached to the surface or inside of the fiber, reducing the shedding of the dye during washing and other processes, thereby achieving a color fixing effect on the fabric.

[0023] 4) The monomer additive of the present invention contains phosphate groups, which release phosphoric acid when decomposed by heat. Phosphorus radicals such as metaphosphoric acid can effectively capture the active hydrogen radicals and hydroxyl radicals generated during the combustion process, inhibiting the combustion chain reaction and thus preventing the spread of flames. In addition, phosphate substances can also promote carbonization of the combustible surface, forming a dense protective carbon layer, which can further block heat and oxygen, making the fabric flame-retardant. DETAILED DESCRIPTION

[0024] The following is a clear and complete description of the technical solutions of the embodiments of this application. Obviously, the embodiments described are part of the embodiments of this application, not all of them. Based on the embodiments in this specification, all other embodiments obtained by ordinary technicians in this field without making any creative efforts are within the scope of protection requested by this application.

[0025] The sources of all raw materials in the present invention are not particularly limited and can be purchased from the market or prepared according to conventional methods known to those skilled in the art.

[0026] Example 1

[0027] A high-temperature resistant fiber fabric is made by the following steps.

[0028] The first step is to mix 12.5g of 2-methylthiopyridine, 51g of 40% hydrogen peroxide, 0.7g of sodium tungstate and 150g of acetonitrile in a three-necked flask, install a condenser and a thermometer, turn on magnetic stirring, heat the system to 75°C, react for 6 hours, and then cool to room temperature. Saturated sodium bicarbonate is added to adjust the pH to 7, and the mixture is extracted with ethyl acetate. The organic phases are combined and dried over anhydrous sodium sulfate, and then rotary evaporated to obtain a conjugated heat-resistant monomer.

[0029] In the second step, 12 g of conjugated heat-resistant monomer, 7.5 g of 3-chloro-1-propanol and 125 g of acetonitrile were added to a three-necked flask, a condenser and a thermometer were installed, magnetic stirring was turned on, the system was heated to 40°C, reacted for 10 hours, and then cooled to room temperature. After crystallization, the antistatic monomer was filtered to obtain the crystal.

[0030] The third step is to add 14g of antistatic monomer, 3g of phosphorus trichloride, 8g of triethylamine, 100g of acetonitrile and 0.2g of anhydrous magnesium chloride into a three-necked flask, install a condenser, a thermometer and a tail gas absorption device, turn on magnetic stirring, heat the system to 70°C, react for 2h, then heat to 80°C, react for 19h, cool to room temperature, wash with water, dry with anhydrous magnesium sulfate, and elute with silica gel after rotary evaporation to obtain a monomer additive;

[0031] Step 4: 100g of polypropylene, 19g of monomer additive, 0.1g of antioxidant 1010 and 0.1g of trinonylphenyl phosphite were mixed evenly and added into a twin-screw extruder for melt extrusion. The fibers were made by melt spinning, and then woven and shaped to obtain high-temperature resistant fiber fabrics.

[0032] A method for preparing a high-temperature resistant fiber fabric, wherein the high-temperature resistant fiber fabric is prepared by the above-mentioned preparation steps.

[0033] Example 2

[0034] A high-temperature resistant fiber fabric is made by the following steps.

[0035] The first step is to mix 13.75g of 2-methylthiopyridine, 66g of 35% hydrogen peroxide, 1.2g of sodium tungstate and 160g of acetonitrile in a three-necked flask, install a condenser and a thermometer, turn on magnetic stirring, heat the system to 78°C, react for 7h, and then cool to room temperature. Saturated sodium bicarbonate is added to adjust the pH to 7.5, extract with ethyl acetate, combine the organic phases, dry them with anhydrous sodium sulfate, and rotary evaporate to obtain a conjugated heat-resistant monomer;

[0036] In the second step, 13 g of conjugated heat-resistant monomer, 8 g of 3-chloro-1-propanol and 132.5 g of acetonitrile were added to a three-necked flask, a condenser and a thermometer were installed, magnetic stirring was turned on, the system was heated to 50 ° C, reacted for 11 hours, and then cooled to room temperature. After the crystals were precipitated, they were filtered to obtain the antistatic monomer;

[0037] The third step is to add 15.5g of antistatic monomer, 3.3g of phosphorus trichloride, 8.5g of triethylamine, 112.5g of acetonitrile and 0.35g of anhydrous magnesium chloride into a three-necked flask, install a condenser, a thermometer and a tail gas absorption device, turn on magnetic stirring, heat the system to 73°C, react for 2.5h, then heat to 83°C, react for 20h, cool to room temperature, wash with water, dry with anhydrous magnesium sulfate, and elute with silica gel after rotary evaporation to obtain a monomer additive;

[0038] Step 4: 105g of polypropylene, 20g of monomer additive, 0.3g of antioxidant 1076 and 0.3g of trinonylphenyl phosphite were mixed evenly and added into a twin-screw extruder for melt extrusion. The fibers were made by melt spinning, and then woven and shaped to obtain high-temperature resistant fiber fabrics.

[0039] A method for preparing a high-temperature resistant fiber fabric, wherein the high-temperature resistant fiber fabric is prepared by the above-mentioned preparation steps.

[0040] Example 3

[0041] A high-temperature resistant fiber fabric is made by the following steps.

[0042] The first step is to mix 15g of 2-methylthiopyridine, 81g of 30% hydrogen peroxide, 1.7g of sodium tungstate and 170g of acetonitrile in a three-necked flask, install a condenser and a thermometer, turn on magnetic stirring, heat the system to 80°C, react for 8h, and then cool to room temperature. Saturated sodium bicarbonate is added to adjust the pH to 8, and the mixture is extracted with ethyl acetate. The organic phases are combined and dried over anhydrous sodium sulfate, and then rotary evaporated to obtain a conjugated heat-resistant monomer.

[0043] In the second step, 14 g of conjugated heat-resistant monomer, 8.5 g of 3-chloro-1-propanol and 140 g of acetonitrile were added to a three-necked flask, a condenser and a thermometer were installed, magnetic stirring was turned on, the system was heated to 60°C, reacted for 12 hours, and then cooled to room temperature. After crystallization, the antistatic monomer was filtered to obtain;

[0044] The third step is to add 17g of antistatic monomer, 3.6g of phosphorus trichloride, 9g of triethylamine, 125g of acetonitrile and 0.5g of anhydrous magnesium chloride into a three-necked flask, install a condenser, a thermometer and a tail gas absorption device, turn on magnetic stirring, heat the system to 75°C, react for 3h, then heat to 85°C, react for 21h, cool to room temperature, wash with water, dry with anhydrous magnesium sulfate, and elute with silica gel after rotary evaporation to obtain a monomer additive;

[0045] Step 4: 110 g of polypropylene, 21 g of monomer additive, 0.5 g of antioxidant 3114 and 0.5 g of trinonylphenyl phosphite were mixed evenly and added into a twin-screw extruder for melt extrusion. The fibers were made by melt spinning, and then woven and shaped to obtain high-temperature resistant fiber fabrics.

[0046] A method for preparing a high-temperature resistant fiber fabric, wherein the high-temperature resistant fiber fabric is prepared by the above-mentioned preparation steps.

[0047] Comparative Example 1

[0048] 105g of polypropylene and 0.3g of antioxidant 1076 trinonylphenyl phosphite were mixed evenly and added into a twin-screw extruder for melt extrusion. Polypropylene fibers were prepared by melt spinning, and then woven and shaped to obtain polypropylene fabrics.

[0049] Experimental Example 1

[0050] The polypropylene fabrics in Examples 1 to 3 and Comparative Example 1 were respectively subjected to performance tests. The heat resistance of each group of fabrics was tested with reference to GB / T 13767-1992 "Test method for heat resistance of textiles", and the dimensional change rate of each group of fabrics was recorded; the antistatic performance of each group of fabrics was tested with reference to GB / T 12703.1-2021 "Test method for electrostatic properties of textiles", and the electrostatic half-life of each group of fabrics was recorded; the color fastness grade of each group of fabrics was tested with reference to GB / T 23976.1-2009 "Textiles - Test for colour fastness", and the flame retardant properties of each group of fabrics were tested with reference to GB / T 5454-1997 "Textiles - Test for burning behaviour", and the limiting oxygen index IOR of each group of fabrics was recorded. The test results are shown in Table 1.

[0051] Table 1

[0052] project Dimensional change rate (%) Electrostatic half-life (s) Color fastness grade Limiting oxygen index IOR (%) Example 1 1.44 3.18 5 27.76 Example 2 1.35 2.96 5 28.13 Example 3 1.52 3.07 5 27.69 Comparative Example 1 3.77 15.81 4 20.63

[0053] As can be seen from Table 1, compared with Comparative Example 1, Examples 1 to 3 have higher dimensional change rates and faster half-lives, indicating that the heat resistance and antistatic properties of the high-temperature resistant fiber fabric are better. At the same time, the color fixing performance and flame retardant properties of Examples 1 to 3 are also better than those of Comparative Example 1. Combined with Comparative Example 1, it can be seen that polypropylene and monomer additives can effectively improve the heat resistance, antistatic performance, color fixing performance and flame retardant properties of polypropylene fabrics.

[0054] The above embodiments are merely intended to facilitate understanding of the methods and core concepts of the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the general principles defined herein may be implemented in other embodiments without departing from the spirit or scope of the present invention. Therefore, the present invention is not limited to the embodiments shown herein, but is intended to be construed in the widest manner consistent with the principles and novel features disclosed herein.

Claims

1. A method for preparing a high temperature resistant fiber fabric, characterized in that: The following steps are involved: Preparation of a monomer additive: obtaining a conjugated heat-resistant monomer by an oxidation reaction between 2-methylthiopyridine and hydrogen peroxide, obtaining an antistatic monomer by a quaternary ammonium salt reaction between the conjugated heat-resistant monomer and 3-chloro-1-propanol, and obtaining a monomer additive by a phosphate esterification reaction between the antistatic monomer, phosphorus trichloride and triethylamine; Preparation of high temperature resistant fiber fabric: polypropylene, monomer additives, antioxidants and plasticizers are blended, melt-extruded, melt-spun, woven and shaped to obtain the high temperature resistant fiber fabric.

2. The method for preparing a high temperature resistant fiber fabric according to claim 1, characterized in that: The mass fraction of hydrogen peroxide is 30-40%.

3. The method for preparing a high temperature resistant fiber fabric according to claim 1, characterized in that: The mass ratio of 2-methylthiopyridine to hydrogen peroxide is 12.5-15:51-81.

4. The method for preparing a high temperature resistant fiber fabric according to claim 1, characterized in that: The mass ratio of the conjugated heat-resistant monomer to 3-chloro-1-propanol is 12-14:7.5-8.

5.

5. The method for preparing a high temperature resistant fiber fabric according to claim 1, characterized in that: The mass ratio of the antistatic monomer to phosphorus trichloride is 14-17:3-3.

6.

6. The method for preparing a high temperature resistant fiber fabric according to claim 1, characterized in that: The antioxidants are antioxidant 1010, antioxidant 1076 and antioxidant 1330.

7. The method for preparing a high temperature resistant fiber fabric according to claim 1, characterized in that: The plasticizer is trinonylphenyl phosphite.

8. The method for preparing a high temperature resistant fiber fabric according to claim 1, characterized in that: The mass ratio of the monomer additive, polypropylene, antioxidant and plasticizer is 19-21:100-110:0.1-0.5:0.1-0.

5.

9. The method for preparing a high temperature resistant fiber fabric according to claim 1, characterized in that: The melt extrusion temperature condition is 220 to 250°C.

10. A high temperature resistant fiber fabric, characterized in that: The high temperature resistant fiber fabric is prepared by the preparation method described in any one of claims 1 to 9.