A finishing process for flame-retardant carpet fabric

Abstract

The present invention discloses a finishing process for flame-retardant carpet fabrics, and relates to the field of textile technology. The finishing process for flame-retardant carpet fabrics of the present invention is applicable to wool carpet fabrics, and includes one-time padding, two-time padding, and three-time padding; wherein, the wool carpet fabric is padded with an antioxidant dithiothreitol in the first padding, the wool carpet fabric that is padded once is padded with a carbon nanotube slurry activated with phosphoric acid in the second padding, and the wool carpet fabric that is padded twice is padded with a potassium carbonate solution of silver carbonate, an antibacterial agent, under microwave conditions, to prepare flame-retardant carpet fabrics; the flame-retardant carpet fabrics prepared by the present invention have strong antibacterial, antistatic, and flame retardant properties.

Description

Technical Field

[0001] The invention relates to the technical field of textiles, in particular to a finishing process for flame-retardant velvet carpet fabrics. Background Art

[0002] With the development of economy and the improvement of people's living standard, carpets have been widely used. At present, carpets are mainly made of cotton fiber, animal hair and non-flame retardant fiber yarn. Among them, wool carpets are widely loved by consumers because of their good warmth retention and decorative properties.

[0003] However, wool blankets are extremely flammable and easily generate static electricity during use. In addition, during daily storage, changes in humidity and temperature can easily breed bacteria and cause mildew, greatly reducing the wearing experience of the wool blanket. Therefore, it is necessary to find a finishing process for the wool blanket fabric to make the blanket fabric more antibacterial, antistatic and flame retardant. Summary of the invention

[0004] The purpose of the present invention is to provide a finishing process for flame retardant carpet fabrics to solve the problems existing in the prior art.

[0005] In order to solve the above technical problems, the present invention provides the following technical solutions:

[0006] A post-finishing process for flame-retardant velvet carpet fabric includes primary padding, secondary padding and tertiary padding.

[0007] Furthermore, the first padding is performed by padding the wool carpet fabric with a sodium methoxide solution of dithiothreitol, an antioxidant.

[0008] Furthermore, the secondary padding uses the carbon nanotube slurry activated by phosphoric acid to pad the wool carpet fabric that has been padded once.

[0009] Furthermore, the third padding is performed by padding the wool blanket fabric that has been padded twice with a nitric acid solution of silver carbonate, an antibacterial agent, under microwave conditions.

[0010] Further, the specific steps are as follows:

[0011] (1) One-time padding: Under nitrogen protection, the wool carpet fabric is immersed in a sodium methoxide solution of dithiothreitol with a weight of 9 to 11 times of its weight for 15 to 25 minutes, ultrasonically pressed at 30 to 40 kHz for 4 to 6 minutes, and the impregnated wool carpet fabric is pressed with the liquid to a residual rate of 70 wt%, and then dried at 65 to 75° C. for 5 to 7 hours to prepare a one-time-impregnated wool carpet fabric;

[0012] (2) Secondary impregnation: at 0-4°C and nitrogen protection, the wool carpet fabric impregnated once was immersed in a methanol solution of sodium methoxide in an amount of 8-10 times its mass, stirred at 400-600 r / min for 50-70 min, then cooled to -11--9°C, added with a phosphoric acid-activated carbon nanotube slurry in an amount of 14-16 times its mass, stirred for 20-40 min, then pressed, with a press rate of 70 wt%, and dried at 65-75°C for 5-7 h to prepare a wool carpet fabric impregnated once;

[0013] (3) Three-time impregnation: Under nitrogen protection, the wool carpet fabric that has been impregnated twice is immersed in a nitric acid solution of silver carbonate, an antibacterial agent, with a mass ratio of 12 to 14 times its mass. Then, the catalyst trans-di-(m)-bis[2-(di-o-tolylphosphine)benzyl]acetate dipalladium (II), potassium acetate, and N,N-dimethylacetamide are added in a mass ratio of 1:3.5:0.19 to 1:4.5:0.21, wherein the mass of potassium acetate is 0.08 to 0.1 times that of the wool carpet fabric that has been impregnated twice. The mixture is stirred at 400 to 600 r / min for 50 to 70 min, and microwaved at 110°C at 100 W and in microwave SPS mode for 12 to 14 min. The mixture is then pressed to a residual rate of 70 wt%, and baked at 65 to 75°C for 5 to 7 h to prepare a flame-retardant carpet fabric.

[0014] Furthermore, the preparation method of the sodium methoxide solution of dithiothreitol in step (1) is as follows: under nitrogen protection, dithiothreitol and sodium methoxide are mixed in a mass ratio of 1:6 to 1:10, and stirred at 400 to 600 r / min for 50 to 70 min to prepare the sodium methoxide solution of dithiothreitol.

[0015] Furthermore, the preparation method of the phosphoric acid-activated carbon nanotube slurry in step (2) is as follows: carbon nanotubes with a tube length of 30 to 50 nm and a length of 10 to 20 μm are washed with deionized water for 2 to 4 times, dried at 105° C. for 2 h, passed through an 80-mesh sieve and placed in a conical flask, added with a 10% phosphoric acid solution with a mass fraction of 5 to 7 times the mass of the carbon nanotubes, stirred at 1200 to 1400 r / min for 3 to 7 h, ultrasonically dispersed at 30 to 40 kHz for 4 h, then immersed in 20 to 40% propiolic acid with a mass fraction of 5 to 9 times the mass of the carbon nanotubes, continued ultrasonication for 30 min, then added concentrated sulfuric acid with a mass fraction of 0.6 to 1 times the mass of the carbon nanotubes at 40 to 60 drops / min, and continued stirring for 3 to 5 h to prepare a phosphoric acid-activated carbon nanotube slurry.

[0016] Furthermore, the preparation method of the nitric acid solution of silver carbonate in step (3) is as follows: under nitrogen protection conditions, silver carbonate and a nitric acid solution with a mass fraction of 68% are mixed in a mass ratio of 1:3 to 1:7, and stirred at 400 to 600 r / min for 50 to 70 minutes to prepare the nitric acid solution of silver carbonate.

[0017] Compared with the prior art, the beneficial effects achieved by the present invention are:

[0018] The post-finishing process of the flame-retardant carpet fabric of the present invention is suitable for wool carpet fabric, including primary impregnation, secondary impregnation and tertiary impregnation; wherein, the primary impregnation uses an antioxidant dithiothreitol to impregnate the wool carpet fabric, the secondary impregnation uses a phosphoric acid-activated carbon nanotube slurry to impregnate the wool carpet fabric that has been impregnated once, and the tertiary impregnation uses a potassium carbonate solution of silver carbonate, an antibacterial agent, to impregnate the wool carpet fabric that has been impregnated twice under microwave conditions to prepare the flame-retardant carpet fabric.

[0019] The antioxidant dithiothreitol is introduced into the wool carpet fabric by a single impregnation process. The dithiothreitol reduces the disulfide bonds in the wool carpet fabric. After the reduction, the disulfide bonds are broken to form a large number of thiol groups in the wool carpet fabric, making the wool carpet fabric more loose and porous. The phosphoric acid-activated carbon nanotube slurry quickly penetrates into the wool carpet fabric through the pores. The propiolic acid on the phosphoric acid-activated carbon nanotubes reacts with the thiol groups on the wool carpet fabric to form thiophene, thereby enhancing the antibacterial properties of the wool carpet fabric. Phosphoric acid reacts with the hydroxyl groups on dithiothreitol to form phosphate esters, thereby enhancing the flame retardant properties of the flame retardant carpet fabric. Under the action of the potassium carbonate solution of the antibacterial agent silver carbonate, thiophene polymerizes to form polythiophene, thereby forming a conductive path in the wool carpet fabric, thereby enhancing the antistatic properties of the flame retardant carpet fabric. DETAILED DESCRIPTION

[0020] 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 described embodiments 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 creative work are within the scope of protection of the present invention.

[0021] In order to more clearly illustrate the method provided by the present invention, the following examples are used to describe in detail the various index testing methods of the flame retardant carpet fabrics prepared in the following examples as follows:

[0022] Antibacterial property: The flame retardant carpet fabrics prepared in the embodiment and the comparative example with the same mass were tested for antibacterial property according to the GB / T20944 standard method.

[0023] Antistatic property: The flame retardant carpet fabrics prepared in the embodiment and the comparative example with the same mass were tested for antistatic property according to the GB / T12703 standard method.

[0024] Flame retardancy: The flame retardant carpet fabrics prepared in the embodiment and the comparative example with the same mass were tested for flame retardancy according to the GB / T5455 standard method.

[0025] Example 1

[0026] (1) One-time padding: under nitrogen protection, dithiothreitol and sodium methoxide were mixed in a mass ratio of 1:6, and stirred at 400 r / min for 50 min to prepare a dithiothreitol sodium methoxide solution; under nitrogen protection, the wool carpet fabric was immersed in a dithiothreitol sodium methoxide solution with a mass of 9 times that of the wool carpet fabric for 15 min, ultrasonicated at 30 kHz for 4 min, and the impregnated wool carpet fabric was rolled with liquid, with a rolling rate of 70 wt%, and dried at 65 ° C for 5 h to prepare a one-time rolled wool carpet fabric;

[0027] (2) Secondary impregnation: The carbon nanotubes with a tube length of 30 nm and a length of 10 μm were washed twice with deionized water, dried at 105°C for 2 h, passed through an 80-mesh sieve and placed in a conical flask, and a 10% phosphoric acid solution with a mass fraction of 5 times the mass of the carbon nanotubes was added, stirred at 1200 r / min for 3 h, and ultrasonically dispersed at 30 kHz for 4 h, and then immersed in 20% propiolic acid with a mass fraction of 5 times the mass of the carbon nanotubes, and ultrasonicated for 30 min, and then concentrated sulfur with a mass fraction of 0.6 times the mass of the carbon nanotubes was added at 40 drops / min. acid, and continued stirring for 3 hours to prepare a phosphoric acid-activated carbon nanotube slurry; at 0°C and nitrogen protection conditions, the wool carpet fabric that had been once impregnated was immersed in a methanol solution of sodium methoxide that was 8 times its mass, and stirred at 400r / min for 50 minutes, then cooled to -11°C, and a phosphoric acid-activated carbon nanotube slurry that was 14 times the mass of the wool carpet fabric that had been once impregnated was added, and continued stirring for 20 minutes, and then the liquid was squeezed out, and the squeezing rate was 70wt%, and baked at 65°C for 5 hours to prepare a secondary impregnated wool carpet fabric;

[0028] (3) Three-time impregnation: under nitrogen protection, silver carbonate and 68% nitric acid solution were mixed in a mass ratio of 1:3, and stirred at 400 r / min for 50 min to prepare a nitric acid solution of silver carbonate; under nitrogen protection, the wool carpet fabric that had been impregnated twice was immersed in a nitric acid solution of antibacterial agent silver carbonate with a mass ratio of 12 times its mass, and then the catalyst trans-di-(m)-bis[2-(di-o-tolylphosphine)benzyl]acetate dipalladium (II), potassium acetate, and N,N-dimethylacetamide were added in a mass ratio of 1:3.5:0.19, wherein the mass of potassium acetate was 0.08 times that of the wool carpet fabric that had been impregnated twice, stirred at 400 r / min for 50 min, microwaved at 110°C at 100 W and in microwave SPS mode for 12 min, and then liquid pressed to a residual rate of 70wt%, and baked at 65°C for 5 h to prepare a flame-retardant carpet fabric.

[0029] Example 2

[0030] (1) One-time padding: under nitrogen protection, dithiothreitol and sodium methoxide were mixed in a mass ratio of 1:8, and stirred at 500 r / min for 60 min to prepare a dithiothreitol sodium methoxide solution; under nitrogen protection, the wool carpet fabric was immersed in a dithiothreitol sodium methoxide solution with a mass of 10 times that of the wool carpet fabric for 20 min, ultrasonicated at 35 kHz for 5 min, and the impregnated wool carpet fabric was rolled with liquid, with a rolling rate of 70 wt%, and dried at 60°C for 6 h to prepare a one-time-impregnated wool carpet fabric;

[0031] (2) Secondary impregnation: The carbon nanotubes with a tube length of 40 nm and a length of 15 μm were washed with deionized water for 3 times, dried at 105°C for 2 h, passed through an 80-mesh sieve and placed in a conical flask, and a 10% phosphoric acid solution with a mass fraction of 6 times the mass of the carbon nanotubes was added, stirred at 1300 r / min for 5 h, ultrasonically dispersed at 35 kHz for 4 h, and then immersed in 30% propiolic acid with a mass fraction of 7 times the mass of the carbon nanotubes, and ultrasonicated for 30 min. Then, concentrated sulfur with a mass fraction of 0.8 times the mass of the carbon nanotubes was added at 50 drops / min. acid, and continued stirring for 4 hours to prepare a phosphoric acid-activated carbon nanotube slurry; at 2°C and nitrogen protection conditions, the wool carpet fabric that had been once impregnated was immersed in a methanol solution of sodium methoxide with a mass of 9 times that of the wool carpet fabric, and stirred at 500r / min for 60 minutes, then cooled to -10°C, and a phosphoric acid-activated carbon nanotube slurry with a mass of 15 times that of the wool carpet fabric that had been once impregnated was added, and continued stirring for 30 minutes, and then the liquid was squeezed out, and the squeezing rate was 70wt%, and dried at 60°C for 6 hours to prepare a secondary impregnated wool carpet fabric;

[0032] (3) Three-time impregnation: under nitrogen protection, silver carbonate and 68% nitric acid solution were mixed in a mass ratio of 1:5, and stirred at 500 r / min for 60 min to prepare a nitric acid solution of silver carbonate; under nitrogen protection, the wool carpet fabric that had been impregnated twice was immersed in a nitric acid solution of antibacterial agent silver carbonate with a mass ratio of 13 times its mass, and then the catalyst trans-di-(m)-bis[2-(di-o-tolylphosphine)benzyl]acetate dipalladium (II), potassium acetate, and N,N-dimethylacetamide were added in a mass ratio of 1:4:0.2, wherein the mass of potassium acetate was 0.09 times that of the wool carpet fabric that had been impregnated twice, stirred at 500 r / min for 60 min, microwaved at 110°C at 100 W and in microwave SPS mode for 13 min, and then liquid pressed to a residual rate of 70 wt%, and dried at 60°C for 6 h to prepare a flame-retardant carpet fabric.

[0033] Example 3

[0034] (1) One-time padding: under nitrogen protection, dithiothreitol and sodium methoxide were mixed in a mass ratio of 1:10, and stirred at 600 r / min for 70 min to prepare a dithiothreitol sodium methoxide solution; under nitrogen protection, the wool carpet fabric was immersed in a dithiothreitol sodium methoxide solution with a mass of 11 times that of the wool carpet fabric for 25 min, ultrasonicated at 40 kHz for 6 min, and the impregnated wool carpet fabric was rolled with liquid, with a rolling rate of 70 wt%, and dried at 75° C. for 7 h to prepare a one-time-impregnated wool carpet fabric;

[0035] (2) Secondary impregnation: The carbon nanotubes with a tube length of 50 nm and a length of 20 μm were washed with deionized water for 4 times, dried at 105°C for 2 h, passed through an 80-mesh sieve and placed in a conical flask, and a 10% phosphoric acid solution with a mass fraction of 7 times the mass of the carbon nanotubes was added, stirred at 1400 r / min for 7 h, ultrasonically dispersed at 40 kHz for 4 h, and then immersed in 40% propiolic acid with a mass fraction of 9 times the mass of the carbon nanotubes, and ultrasonicated for 30 min, and then concentrated sulfuric acid with a mass fraction of 1 times the mass of the carbon nanotubes was added at 60 drops / min. , continue stirring for 5 hours to prepare a phosphoric acid-activated carbon nanotube slurry; at 4°C and nitrogen protection conditions, immerse the wool carpet fabric that has been once rolled in a methanol solution of sodium methoxide with a mass 10 times that of the wool carpet fabric, stir at 600r / min for 70 minutes, then cool to -9°C, add a phosphoric acid-activated carbon nanotube slurry with a mass 16 times that of the wool carpet fabric that has been once rolled, continue stirring for 40 minutes, then perform liquid rolling, the rolling residue rate is 70wt%, and bake at 75°C for 7 hours to prepare a secondary rolled wool carpet fabric;

[0036] (3) Three-time impregnation: under nitrogen protection, silver carbonate and 68% nitric acid solution were mixed in a mass ratio of 1:7, and stirred at 600 r / min for 70 min to prepare a nitric acid solution of silver carbonate; under nitrogen protection, the wool carpet fabric that had been impregnated twice was immersed in a nitric acid solution of antibacterial agent silver carbonate with a mass ratio of 14 times its mass, and then the catalyst trans-di-(m)-bis[2-(di-o-tolylphosphine)benzyl]acetate dipalladium (II), potassium acetate, and N,N-dimethylacetamide were added in a mass ratio of 1:4.5:0.21, wherein the mass of potassium acetate was 0.1 times that of the wool carpet fabric that had been impregnated twice, stirred at 600 r / min for 70 min, microwaved at 110°C at 100 W and in microwave SPS mode for 14 min, and then liquid pressed to a residual rate of 70 wt%, and baked at 75°C for 7 h to prepare a flame-retardant carpet fabric.

[0037] Comparative Example 1

[0038] The difference between Comparative Example 1 and Example 2 is that the wool carpet fabric is impregnated with the carbon nanotube slurry activated by phosphoric acid, and then the carpet fabric is impregnated with the potassium carbonate solution of silver carbonate, an antibacterial agent, under microwave conditions. The remaining preparation steps are the same as in Example 2.

[0039] Comparative Example 2

[0040] The difference between Comparative Example 2 and Example 2 is that the wool carpet fabric is impregnated with an antioxidant dithiothreitol, then impregnated with a carbon nanotube slurry, and then impregnated with an antibacterial agent silver carbonate potassium carbonate solution under microwave conditions to prepare the carpet fabric. The remaining preparation steps are the same as Example 2.

[0041] Comparative Example 3

[0042] The difference between Comparative Example 3 and Example 2 is that only the antioxidant dithiothreitol is used to pad the wool carpet fabric, and then the antibacterial agent silver carbonate potassium carbonate solution is used to pad the carpet fabric under microwave conditions. The remaining preparation steps are the same as Example 2.

[0043] Comparative Example 4

[0044] The difference between Comparative Example 4 and Example 2 is that only the antioxidant dithiothreitol is used to pad the wool carpet fabric, and then the carbon nanotube slurry activated by phosphoric acid is used to pad the flame retardant carpet fabric. The remaining preparation steps are the same as those in Example 2.

[0045] Effect example

[0046] Table 1 below shows the analysis results of the antibacterial property, antistatic property and flame retardancy of the flame retardant carpet fabrics prepared by using Examples 1 to 3 of the present invention and Comparative Examples 1 to 4.

[0047] Table 1

[0048]

[0049] It can be found from Table 1 that the flame-retardant carpet fabrics prepared in Examples 1, 2 and 3 have strong antibacterial, antistatic and flame retardant properties; from the comparison of the experimental data of Examples 1, 2, 3 and Comparative Example 1, it can be found that the flame-retardant carpet fabric is prepared by impregnating the wool carpet fabric with the antioxidant dithiothreitol, which can form thiophene and phosphate ester, and the flame-retardant carpet fabric prepared has strong antibacterial, antistatic and flame retardant properties; from the experimental data of Examples 1, 2, 3 and Comparative Examples 2 and 3, it can be found that the flame-retardant carpet fabric is prepared by impregnating the carbon nanotube slurry activated by phosphoric acid, which can form thiophene and phosphate ester, and the antibacterial, antistatic and flame retardant properties are strong; from the experimental data of Examples 1, 2, 3 and Comparative Example 4, it can be found that the flame-retardant carpet fabric is prepared by impregnating the potassium carbonate solution of the antibacterial agent silver carbonate under microwave conditions, which can form polythiophene, and the flame-retardant carpet fabric prepared has strong antistatic properties.

[0050] It will be apparent to those skilled in the art that the invention is not limited to the details of the exemplary embodiments described above and that the invention can be implemented in other specific forms without departing from the spirit or essential features of the invention. Therefore, the embodiments should be considered in all respects as exemplary and non-limiting, and the scope of the invention is defined by the appended claims rather than the foregoing description, and it is intended that all variations within the meaning and scope of the equivalent elements of the claims be included in the invention. Any marking in a claim should not be considered as limiting the claim to which it relates.

Claims

1. A finishing process for flame retardant carpet fabric, characterized in that: The method comprises a first immersion, a second immersion and a third immersion, wherein the first immersion uses a sodium methoxide solution of dithiothreitol, an antioxidant, to immerse the wool carpet fabric, the second immersion uses a carbon nanotube slurry activated by phosphoric acid to immerse the wool carpet fabric that has been immersed once, and the third immersion uses a nitric acid solution of silver carbonate, an antibacterial agent, to immerse the wool carpet fabric that has been immersed twice under microwave conditions; The specific steps of the post-finishing process of the flame-retardant carpet fabric are as follows: (1) One-time padding: Under nitrogen protection, the wool carpet fabric is immersed in a sodium methoxide solution of dithiothreitol with a weight of 9 to 11 times its weight for 15 to 25 minutes, and the wool carpet fabric is ultrasonically pressed at 30 to 40 kHz for 4 to 6 minutes, with a rolling rate of 70 wt%. The wool carpet fabric is then dried at 65 to 75 °C for 5 to 7 hours to prepare a one-time padding wool carpet fabric. (2) Secondary impregnation: at 0-4°C and nitrogen protection, immerse the wool carpet fabric that has been impregnated once in a methanol solution of sodium methoxide at a volume of 8-10 times its mass, stir at 400-600 r / min for 50-70 min, then cool to -11--9°C, add a 14-16-times-mass phosphoric acid-activated carbon nanotube slurry, continue stirring for 20-40 min, and then perform liquid pressing, with a residual rate of 70 wt%, and bake at 65-75°C for 5-7 h to prepare a wool carpet fabric that has been impregnated twice; (3) Three-time padding: Under nitrogen protection, the wool carpet fabric that has been padded twice is immersed in a nitric acid solution of silver carbonate, an antibacterial agent, in an amount of 12 to 14 times its mass. Then, a catalyst of trans-di-(m)-bis[2-(di-o-tolylphosphine)benzyl]acetate dipalladium(II), potassium acetate, and N,N-dimethylacetamide are added in a mass ratio of 1:3.5:0.19 to 1:4.5:0.21, wherein the mass of potassium acetate is 0.08 to 0.1 times that of the wool carpet fabric that has been padded twice. The mixture is stirred at 400 to 600 r / min for 50 to 70 min, and microwaved at 110°C at 100 W and in microwave SPS mode for 12 to 14 min. The mixture is then rolled to a residual rate of 70 wt%. The mixture is then dried at 65 to 75°C for 5 to 7 h to prepare a flame-retardant carpet fabric. The preparation method of the sodium methoxide solution of dithiothreitol in step (1) is as follows: under nitrogen protection, dithiothreitol and sodium methoxide are mixed in a mass ratio of 1:6 to 1:10, and stirred at 400 to 600 r / min for 50 to 70 min to prepare the sodium methoxide solution of dithiothreitol; The preparation method of the phosphoric acid-activated carbon nanotube slurry in step (2) is as follows: washing carbon nanotubes with a tube length of 30-50 nm and a length of 10-20 μm with deionized water for 2-4 times, drying at 105° C. for 2 h, passing through an 80-mesh sieve and placing in a conical flask, adding a 10% phosphoric acid solution with a mass fraction of 5-7 times the mass of the carbon nanotubes, stirring at 1200-1400 r / min for 3-7 h, ultrasonically dispersing at 30-40 kHz for 4 h, then immersing in 20-40% propiolic acid with a mass fraction of 5-9 times the mass of the carbon nanotubes, continuing ultrasonication for 30 min, then dripping concentrated sulfuric acid with a mass fraction of 0.6-1 times the mass of the carbon nanotubes at 40-60 drops / min, and continuing stirring for 3-5 h to prepare a phosphoric acid-activated carbon nanotube slurry; The preparation method of the nitric acid solution of silver carbonate in step (3) is as follows: under nitrogen protection conditions, silver carbonate and a nitric acid solution with a mass fraction of 68% are mixed in a mass ratio of 1:3 to 1:7, and stirred at 400 to 600 r / min for 50 to 70 min to prepare the nitric acid solution of silver carbonate.

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