Soft tensile all-cotton spunlace cloth and preparation method and application thereof

Abstract

The invention discloses a soft tensile all-cotton spunlace fabric and a preparation method and application thereof, and relates to the technical field of non-woven fabrics. The preparation method of the soft tensile all-cotton spunlace cloth comprises the following steps: S1) carrying out carboxylation modification on the absorbent cotton; then, N, N-dimethyl-1, 3-diaminopropane is used for carrying out tertiary amination modification on the modified product; and finally, carrying out quaternary ammonium salinization to obtain the modified absorbent cotton. (2) mixing the modified absorbent cotton and the pure cotton in proportion, spreading, performing primary spunlace treatment, and drying; degreasing and drying to obtain a degreasing cotton non-woven fabric; s2, alternately laminating the degreasing cotton non-woven fabrics and the cotton paper, wherein the degreasing cotton non-woven fabrics are arranged on the two surfaces of the outermost layer; and carrying out secondary spunlace treatment and drying to obtain the soft tensile all-cotton spunlace cloth. The prepared soft tensile all-cotton spunlace fabric is high in tensile strength, high in liquid absorption and good in softness, and has a certain antibacterial effect.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of non-woven fabrics, in particular to a soft tensile full-cotton spunlace fabric and a preparation method and application thereof. BACKGROUND

[0002] With the improvement of living standards, textiles as a common material for people to contact have higher requirements for their performance and comfort. Among them, as an important non-manufacturing material, full-cotton spunlace non-woven fabric has been widely used due to its pure natural, comfortable, breathable and other advantages. However, there are still deficiencies in the prior art, such as the general tensile strength of full-cotton spunlace fabric, the addition of high-strength synthetic fibers will destroy the full-cotton property of the material, and the method of increasing the spunlace strength will reduce the softness of the full-cotton spunlace fabric.

[0003] In summary, it is of great significance to solve the above problems and prepare a soft tensile full-cotton spunlace fabric. SUMMARY

[0004] The present application relates to the technical field of non-woven fabrics, in particular to a soft tensile full-cotton spunlace fabric and a preparation method and application thereof.

[0005] In order to solve the above technical problems, the present application provides the following technical scheme: A preparation method of a soft tensile full-cotton spunlace fabric, comprising the following steps: S1: (1) Carboxymethyl modification of the absorbent cotton, then tertiary amine modification of the absorbent cotton using N,N-dimethyl-1,3-diaminopropane, and finally quaternary ammonium saltification to obtain modified absorbent cotton; (2) mixing the modified absorbent cotton and pure cotton according to a proportion, laying, one-time spunlace treatment, drying, defatting, and drying again to obtain an absorbent cotton non-woven fabric; S2: alternately stacking the absorbent cotton non-woven fabric and the cotton paper, with the outermost layers being absorbent cotton non-woven fabric on both sides, twice spunlace treatment, and drying to obtain a soft tensile full-cotton spunlace fabric.

[0006] More preferably, in step S2, the number of alternately stacking is greater than or equal to 3 times; the grammage of the absorbent cotton non-woven fabric is 15-50 g / m 2 ; and the grammage of the cotton paper is 15-25 g / m 2 .

[0007] More preferably, in the raw material of the absorbent cotton non-woven fabric, the proportion of the modified absorbent cotton and the pure cotton is (2-3):10.

[0008] More preferably, the preparation method of the modified absorbent cotton is: (1) adding absorbent cotton and chloroacetic acid into a sodium hydroxide solution, stirring at 60-70℃ for 7-8h, washing, acidifying, and drying to obtain carboxyl-modified absorbent cotton; (2) Carboxyl modified absorbent cotton, N, N-dimethyl-1, 3-diaminopropane, N, N'-dicyclohexyl carbodiimide, 4-dimethylamino pyridine are added into tetrahydrofuran and mixed uniformly, stirred at 20-25℃ for 4-5h, filtered, washed, dried to obtain N, N dimethyl modified absorbent cotton; (3) N, N dimethyl modified absorbent cotton, triethylamine, bromoethane are added into aqueous ethanol solution, stirred at 60-65℃ for 30-40h, filtered, washed, dried to obtain modified absorbent cotton.

[0009] More preferably, the carboxyl modified absorbent cotton comprises the following raw materials by mass fraction: 100 parts of absorbent cotton, 9-10 parts of chloroacetic acid, 180-200 parts of 15-20wt% sodium hydroxide solution; The N, N dimethyl modified absorbent cotton comprises the following raw materials by mass fraction: 100 parts of carboxyl modified absorbent cotton, 10-12 parts of N, N-dimethyl-1, 3-diaminopropane, 21-23 parts of N, N'-dicyclohexyl carbodiimide, 11-13 parts of 4-dimethylamino pyridine, 130-150 parts of tetrahydrofuran; The modified absorbent cotton comprises the following raw materials by mass fraction: 100 parts of N, N dimethyl modified absorbent cotton, 10-11 parts of triethylamine, 11-12 parts of bromoethane, 35-40wt% aqueous ethanol solution.

[0010] More preferably, the water pressure of the first water jet treatment is 80-100bar; in the second water jet treatment, the specific process is: first, low pressure water jet treatment with water pressure of 35-50bar, then high pressure water jet treatment with water pressure of 120-150bar.

[0011] More preferably, the preparation method of the cotton paper is: fluorine-containing acrylamide copolymer is configured into a solution, uniformly sprayed on the surface of the water-absorbing cotton paper, dried to obtain the cotton paper; wherein the concentration of the fluorine-containing acrylamide copolymer is 200-300mg / L, and the solvent is 50-70wt% aqueous ethanol solution.

[0012] More preferably, the preparation method of the fluorine-containing acrylamide copolymer comprises the following steps: (1) acrylamide and 2-acrylamido-2-methylpropane sulfonic acid are added into deionized water and stirred uniformly, the pH is adjusted to 6.5±0.3 to obtain a reaction monomer solution A; (2) perfluorooctyl ethyl acrylate and polyethylene glycol monoallyl ether are added into deionized water and stirred uniformly to obtain a reaction monomer solution B; (3) under nitrogen atmosphere, the reaction monomer solution A and the reaction monomer solution B are mixed uniformly, 0.1-0.2wt% initiator is added, stirred at 25-30℃ for 4-4.5h, filtered, washed, dried to obtain the fluorine-containing acrylamide copolymer.

[0013] More preferably, the raw material of the fluorine-containing propylene amide copolymer comprises: 14-16 parts by weight of propylene amide, 2-3 parts by weight of 2-acrylamido-2-methylpropane sulfonic acid, 0.15-0.2 parts by weight of perfluoro octyl ethyl acrylate, 0.3 parts by weight of polyethylene glycol monoallyl ether, and 0.05-0.1 parts by weight of initiator; the molecular weight of the polyethylene glycol monoallyl ether is 400-1000.

[0014] More preferably, the soft tensile full cotton water jet fabric can be functionalized by adding RO pure water or natural plant essence for wet wipe production.

[0015] Compared with the prior art, the present application has the following beneficial effects: the present application uses pure cotton and modified defatted cotton as pure cotton raw material for water jet to obtain defatted cotton non-woven fabric, sprays fluorine-containing propylene amide copolymer solution on the surface of the water-absorbing cotton paper, and then dries to obtain cotton paper, and uses the cotton paper and the defatted cotton non-woven fabric in an alternating stacking manner, and the outermost layer is pure cotton defatted cotton non-woven fabric, which is prepared. The full cotton water jet fabric has high tensile strength, strong liquid absorption, good softness, and certain antibacterial effect.

[0016] The preparation method of the modified defatted cotton is that the hydroxyl group and the vinyl chloride in the defatted cotton are subjected to etherification reaction under alkaline conditions, and the carboxylated defatted cotton is obtained by acidification treatment; further, the carboxyl group of the carboxylated defatted cotton and the primary amine of N,N-dimethyl-1,3-diaminopropane are subjected to coupling reaction under the catalysis of N,N'-dicyclohexyl carbodiimide (DCC) and 4-dimethylamino pyridine (DMAP), to obtain N,N-dimethyl modified defatted cotton; further, the tertiary amine group in the N,N-dimethyl modified defatted cotton is alkylated by bromoethane under the catalysis of triethylamine, to obtain modified defatted cotton containing quaternary ammonium salt. The introduction of the modified defatted cotton can significantly improve the hydrophilicity of the cloth, improve the contact comfort, and endow the cloth with antibacterial function. In addition, the hydroxyl group in the pure cotton fiber is negatively charged, so that the non-woven fabric after water jet treatment is more firm, has low fuzz rate, is more soft, and has higher tensile strength.

[0017] The preparation method of the fluorine-containing acrylamide copolymer is that acrylamide and 2-acrylamido-2-methylpropanesulfonic acid are used as hydrophilic monomers, perfluorooctyl ethyl acrylate is used as a hydrophobic monomer, and polyethylene glycol monoallyl ether is used as an amphiphilic monomer, and the fluorine-containing acrylamide copolymer is obtained after initiation of an initiator. After the fluorine-containing acrylamide copolymer solution is sprayed on the surface of the cotton paper and dried, a discontinuous island-shaped film of a hydrophobic region is formed on the surface of the water-absorbing cotton paper through hydrophobic association, that is, a local hydrophobic region. On the one hand, during the hydroentangling process, the discontinuous hydrophobic region structure can disperse the impact force of water pressure and reduce the loss of cotton paper fibers, and can also avoid excessive hydroentangling to prevent the fibers from being too tightly compacted, thereby preventing the softness of the non-woven fabric from being reduced. On the other hand, the region not covered by the fluorine island retains the capillary channel of the cotton paper, so it does not hinder the liquid absorption, but can hinder the backflow of the liquid, thereby improving the liquid absorption amount. The sulfonic acid group in 2-acrylamido-2-methylpropanesulfonic acid can not only improve the water absorption of the fabric, but also form a bond with the quaternary ammonium salt group used in the pure cotton non-woven fabric, thereby increasing the integrity of the hydroentangled fabric and improving the tensile strength. However, due to the large steric hindrance of perfluorooctyl ethyl acrylate, even if the amount of the monomer is increased, the content of perfluorooctyl ethyl acrylate in the polymer cannot be further increased. Therefore, the polyethylene glycol monoallyl ether with a molecular weight of 400-1000 is used as a second hydrophobic monomer in the present application, which can effectively wet the perfluorooctyl ethyl acrylate monomer, reduce the local segment density, increase the content of perfluorooctyl ethyl acrylate monomer in the polymer, and also participate in the polymerization reaction, thereby improving the wetting and spreading properties of the fluorine-containing acrylamide copolymer and the tensile strength of the fabric. However, the concentration of the fluorine-containing acrylamide copolymer solution needs to be controlled. If the concentration is too low, the hydrophobic association cannot be triggered, and if the concentration is too high, the local hydrophobic region is too large and even merges with each other, which seriously affects the hydroentangling effect and reduces the liquid absorption. Therefore, the mass ratio of perfluorooctyl ethyl acrylate to polyethylene glycol monoallyl ether is controlled to be 3-4:6.

[0018] In the hydroentangling process, a stepwise water pressure process is used, that is, low-pressure hydroentangling is performed first to pre-wet and pre-entangle the fabric and prevent the fibers from moving violently, and then high-pressure hydroentangling is performed to effectively improve the overall strength of the fabric. In addition, the defatting process of the present application is arranged after the hydroentangling process. This is because the mechanical properties of the defatted cotton decrease after defatting treatment, and the hydrophilicity is relatively strong, so a larger pressure is required in the hydroentangling process to achieve the same effect, which consumes more energy. In addition, the mixing of defatted cotton in pure cotton fibers also promotes the uniformity of hydroentangling. DETAILED DESCRIPTION

[0019] The technical solutions in the embodiments of the present application will be clearly and completely described below. Obviously, the described embodiments are only a part of the embodiments of the present application, rather than all the embodiments. Based on the embodiments in the present application, all other embodiments obtained by those skilled in the art without creative work fall within the protection scope of the present application.

[0020] It should be noted that the following parts are by weight, and there is no special restriction on the purchase manufacturers of all raw materials involved in the present application, which exemplarily include: chloroacetic acid CAS No. 79-11-8; N,N-dimethyl-1,3-diaminopropane CAS No. 109-55-7; N,N'-dicyclohexyl carbodiimide CAS No. 538-75-0; 4-dimethylamino pyridine CAS No. 1122-58-3; triethylamine CAS No. 121-44-8; bromoethane CAS No. 74-96-4; acrylamide CAS No. 79-06-1; 2-acrylamido-2-methylpropanesulfonic acid CAS No. 15214-89-8; perfluorooctyl ethyl acrylate CAS No. 27905-45-9; polyethylene glycol monoallyl ether with a molecular weight of 800; pure cotton with an impurity content <1%, a fiber length of 30 mm, and a fineness of 1.2 dtex; defatted cotton prepared by a defatting process from pure cotton; water-absorbing cotton paper with a model number of FF-390 and a grammage of 20 g / m 2 Provided by Shenzhen Renshan Technology Co., Ltd.

[0021] In the following examples, parts are mass parts, and the above and other raw materials used but not mentioned are commercially available; wherein, the defatting process is carried out according to the method provided in patent CN113529402A.

[0022] Example 1: A preparation method of a soft and tensile pure cotton water-jet fabric includes the following steps: Step one: preparation of modified defatted cotton: (1) 100 parts of defatted cotton and 9.5 parts of chloroacetic acid are added to 200 parts of 20 wt% sodium hydroxide solution, stirred at 65℃ for 8h, washed, acidified, and dried to obtain carboxyl-modified defatted cotton; (2) 100 parts of carboxyl-modified defatted cotton, 11 parts of N,N-dimethyl-1,3-diaminopropane, 22 parts of N,N'-dicyclohexyl carbodiimide, and 12 parts of 4-dimethylamino pyridine are added to 150 parts of tetrahydrofuran and mixed uniformly, stirred at 25℃ for 4.5h, filtered, washed, and dried to obtain N,N-dimethyl-modified defatted cotton; (3) 100 parts of N,N-dimethyl-modified defatted cotton, 10.5 parts of triethylamine, and 11.5 parts of bromoethane are added to 40 wt% ethanol aqueous solution, stirred at 60℃ for 32h, filtered, washed, and dried to obtain modified defatted cotton; Step two: preparation of fluorine-containing acrylamide copolymer: (1) 15 parts of acrylamide and 2.5 parts of 2-acrylamido-2-methylpropanesulfonic acid were added to 100 parts of deionized water and stirred to obtain a reaction monomer solution A with a pH of 6.5±0.3; (2) 0.18 parts of perfluorooctyl ethyl acrylate and 0.3 parts of polyethylene glycol monoallyl ether were added to 10 parts of deionized water and stirred to obtain a reaction monomer solution B; (3) under a nitrogen atmosphere, the reaction monomer solution A and the hydrophilic reaction monomer solution B were mixed uniformly, 0.1 wt% of an initiator NaHSO3-K2S2O8 (molar ratio of oxidant to reducing agent is 1:2) was added, stirred at 25°C for 4h, filtered, washed, and dried to obtain a fluorine-containing acrylamide copolymer; Step three: preparation of cotton paper: the fluorine-containing acrylamide copolymer was added to a 60 wt% ethanol aqueous solution to prepare a solution with a concentration of 250 mg / L, which was uniformly sprayed on the surface of the water-absorbing cotton paper, and then dried to obtain the cotton paper; Step four: preparation of soft and tensile all-cotton spunlace fabric: S1: the modified defatted cotton and pure cotton were mixed at a mass ratio of 10:2.5, laid flat, and subjected to one-time water jet treatment at a water pressure of 90 bar, dried, defatted, and dried again to obtain a defatted cotton non-woven fabric (with a grammage of 30 g / m 2 ); S2: the defatted cotton non-woven fabric and the cotton paper were alternately stacked (three times of alternating stacking), and the outermost layers were both defatted cotton non-woven fabric; the low-pressure water jet treatment was performed at a water pressure of 40 bar, followed by high-pressure water jet treatment at a water pressure of 130 bar for two-time water jet treatment, and then dried to obtain the soft and tensile all-cotton spunlace fabric.

[0023] Example 2: a method for preparing a soft and tensile all-cotton spunlace fabric includes the following steps: Step one: preparation of modified defatted cotton: (1) 100 parts of defatted cotton and 9.5 parts of chloroacetic acid were added to 200 parts of a 20 wt% sodium hydroxide solution, stirred at 65°C for 8h, washed, acidified, and dried to obtain carboxyl-modified defatted cotton; (2) 100 parts of the carboxyl-modified defatted cotton, 11 parts of N,N-dimethyl-1,3-diaminopropane, 22 parts of N,N'-dicyclohexyl carbodiimide, and 12 parts of 4-dimethylamino pyridine were added to 150 parts of tetrahydrofuran and stirred uniformly at 25°C for 4.5h, filtered, washed, and dried to obtain N,N-dimethyl-modified defatted cotton; (3) 100 parts of the N,N-dimethyl-modified defatted cotton, 10.5 parts of triethylamine, and 11.5 parts of bromoethane were added to a 40 wt% ethanol aqueous solution and stirred at 60°C for 32h, filtered, washed, and dried to obtain the modified defatted cotton; Step two: preparation of fluorine-containing acrylamide copolymer: (1) 15 parts of acrylamide and 2.5 parts of 2-acrylamido-2-methylpropanesulfonic acid were added to 100 parts of deionized water and stirred to obtain a reaction monomer solution A with a pH of 6.5±0.3; (2) 0.18 parts of perfluorooctyl ethyl acrylate and 0.3 parts of polyethylene glycol monoallyl ether were added to 10 parts of deionized water and stirred to obtain a reaction monomer solution B; (3) under a nitrogen atmosphere, the reaction monomer solution A and the hydrophilic reaction monomer solution B were mixed uniformly, 0.1 wt% of an initiator NaHSO3-K2S2O8 (molar ratio of oxidant to reducing agent is 1:2) was added, stirred at 25°C for 4h, filtered, washed, and dried to obtain a fluorine-containing acrylamide copolymer; Step three: preparation of cotton paper: the fluorine-containing acrylamide copolymer was added to a 60 wt% ethanol aqueous solution to prepare a solution with a concentration of 250 mg / L, which was uniformly sprayed on the surface of the water-absorbing cotton paper, and then dried to obtain the cotton paper; Step four: preparation of soft and tensile all-cotton spunlace fabric: S1: the modified defatted cotton and pure cotton were mixed at a mass ratio of 10:2, laid flat, and subjected to a first water jet treatment at a water pressure of 100 bar, dried, defatted, and dried again to obtain a defatted cotton non-woven fabric (with a grammage of 30 g / m 2 ); S2: the defatted cotton non-woven fabric and the cotton paper were alternately stacked (three times of alternating stacking), and the outermost layers were both defatted cotton non-woven fabric; a low-pressure water jet treatment was first performed at a water pressure of 50 bar, followed by a high-pressure water jet treatment at a water pressure of 120 bar for a second water jet treatment, and then dried to obtain a soft and tensile all-cotton spunlace fabric.

[0024] Example 3: a method for preparing a soft and tensile all-cotton spunlace fabric includes the following steps: Step one: preparation of modified defatted cotton: (1) 100 parts of defatted cotton and 9.5 parts of chloroacetic acid were added to 200 parts of a 20 wt% sodium hydroxide solution and stirred at 65°C for 8h, washed, acidified, and dried to obtain carboxyl-modified defatted cotton; (2) 100 parts of the carboxyl-modified defatted cotton, 11 parts of N,N-dimethyl-1,3-diaminopropane, 22 parts of N,N'-dicyclohexyl carbodiimide, and 12 parts of 4-dimethylamino pyridine were added to 150 parts of tetrahydrofuran and stirred at 25°C for 4.5h, filtered, washed, and dried to obtain N,N-dimethyl-modified defatted cotton; (3) 100 parts of the N,N-dimethyl-modified defatted cotton, 10.5 parts of triethylamine, and 11.5 parts of bromoethane were added to a 40 wt% ethanol aqueous solution and stirred at 60°C for 32h, filtered, washed, and dried to obtain the modified defatted cotton; Step two: preparation of fluorine-containing acrylamide copolymer: (1) 15 parts of acrylamide and 2.5 parts of 2-acrylamido-2-methylpropanesulfonic acid were added to 100 parts of deionized water and stirred to obtain a reaction monomer solution A with a pH of 6.5±0.3; (2) 0.18 parts of perfluorooctyl ethyl acrylate and 0.3 parts of polyethylene glycol monoallyl ether were added to 10 parts of deionized water and stirred to obtain a reaction monomer solution B; (3) under a nitrogen atmosphere, the reaction monomer solution A and the hydrophilic reaction monomer solution B were mixed uniformly, 0.1wt% of an initiator NaHSO3-K2S2O8 (molar ratio of oxidant to reducing agent is 1:2) was added, stirred at 25°C for 4h, filtered, washed and dried to obtain a fluorine-containing acrylamide copolymer; Step three: preparation of cotton paper: the fluorine-containing acrylamide copolymer was added to a 60wt% ethanol aqueous solution to prepare a solution with a concentration of 250mg / L, which was uniformly sprayed on the surface of the water-absorbing cotton paper and dried to obtain the cotton paper; Step four: preparation of soft and tensile all-cotton spunlace fabric: S1: the modified defatted cotton and pure cotton were mixed at a mass ratio of 10:3, laid flat, and subjected to a first water jet treatment at a water pressure of 80bar and dried; defatted and dried again to obtain a defatted cotton non-woven fabric (with a grammage of 30g / m 2 ); S2: the defatted cotton non-woven fabric and the cotton paper were alternately stacked (the number of alternating layers was three), and the outermost layer was defatted cotton non-woven fabric on both sides; a second water jet treatment was performed by first performing a low-pressure water jet treatment at a water pressure of 35bar and then performing a high-pressure water jet treatment at a water pressure of 150bar, and then dried to obtain a soft and tensile all-cotton spunlace fabric.

[0025] Comparative Example 1: based on Example 1, the defatted cotton was not modified, and the rest of the process remained unchanged, as follows: Step one: preparation of fluorine-containing acrylamide copolymer: (1) 15 parts of acrylamide and 2.5 parts of 2-acrylamido-2-methylpropanesulfonic acid were added to 100 parts of deionized water and stirred to obtain a reaction monomer solution A with a pH of 6.5±0.3; (2) 0.18 parts of perfluorooctyl ethyl acrylate and 0.3 parts of polyethylene glycol monoallyl ether were added to 10 parts of deionized water and stirred to obtain a reaction monomer solution B; (3) under a nitrogen atmosphere, the reaction monomer solution A and the hydrophilic reaction monomer solution B were mixed uniformly, 0.1wt% of an initiator NaHSO3-K2S2O8 (molar ratio of oxidant to reducing agent is 1:2) was added, stirred at 25°C for 4h, filtered, washed and dried to obtain a fluorine-containing acrylamide copolymer; Step two: preparation of cotton paper: the fluorine-containing acrylamide copolymer was added to a 60wt% ethanol aqueous solution to prepare a solution with a concentration of 250mg / L, which was uniformly sprayed on the surface of the water-absorbing cotton paper and dried to obtain the cotton paper; Step three: preparation of soft and tensile all-cotton water-jet fabric: S1: mix modified defatted cotton and pure cotton at a mass ratio of 10:2.5, lay flat, set the water pressure to 90 bar for one water jet treatment, dry, defat, and dry again to obtain defatted cotton non-woven fabric (gram weight of 30 g / m 2 ); S2: alternately stack the defatted cotton non-woven fabric and cotton paper (alternately stack three times), and the outermost two sides are both defatted cotton non-woven fabric; first, perform low-pressure water jet treatment at a water pressure of 40 bar, then perform high-pressure water jet treatment at a water pressure of 130 bar for two water jet treatments, and dry to obtain soft and tensile all-cotton water-jet fabric.

[0026] Comparative Example 2: based on Example 1, without adding polyethylene glycol monomethallyl ether, and the rest of the process remains unchanged, as follows: Step one: preparation of modified defatted cotton: (1) add 100 parts of defatted cotton and 9.5 parts of chloroacetic acid to 200 parts of 20 wt% sodium hydroxide solution, stir at 65°C for 8h, wash, acidify, and dry to obtain carboxyl-modified defatted cotton; (2) add 100 parts of carboxyl-modified defatted cotton, 11 parts of N,N-dimethyl-1,3-diaminopropane, 22 parts of N,N'-dicyclohexyl carbodiimide, and 12 parts of 4-dimethylamino pyridine to 150 parts of tetrahydrofuran and mix uniformly, stir at 25°C for 4.5h, filter, wash, and dry to obtain N,N-dimethyl-modified defatted cotton; (3) add 100 parts of N,N-dimethyl-modified defatted cotton, 10.5 parts of triethylamine, and 11.5 parts of bromoethane to 40 wt% ethanol aqueous solution, stir at 60°C for 32h, filter, wash, and dry to obtain modified defatted cotton; Step two: preparation of fluorine-containing acrylamide copolymer: (1) add 15 parts of acrylamide and 2.5 parts of 2-acrylamido-2-methylpropanesulfonic acid to 100 parts of deionized water and stir uniformly, adjust the pH to 6.5±0.3 to obtain reaction monomer solution A; (2) add 0.18 parts of perfluorooctyl ethyl acrylate and 0.3 parts of sodium dodecyl sulfate to 10 parts of deionized water and stir uniformly to obtain reaction monomer solution B; (3) under a nitrogen atmosphere, mix reaction monomer solution A and hydrophilic reaction monomer solution B uniformly, add 0.1 wt% of initiator NaHSO3-K2S2O8 (molar ratio of oxidizing agent to reducing agent is 1:2), stir at 25°C for 4h, filter, wash, and dry to obtain fluorine-containing acrylamide copolymer; Step three: preparation of cotton paper: add fluorine-containing acrylamide copolymer to 60 wt% ethanol aqueous solution to prepare a solution with a concentration of 250 mg / L, uniformly spray it on the surface of water-absorbing cotton paper, and dry to obtain cotton paper; Step four: preparation of soft and tensile all-cotton water-jet fabric: S1: mix modified defatted cotton and pure cotton at a mass ratio of 10:2.5, lay flat, set the water pressure to 90 bar for one hydroentanglement treatment, dry, defat, and dry again to obtain defatted cotton non-woven fabric (gram weight of 30 g / m 2 ); S2: alternately stack the defatted cotton non-woven fabric and the cotton paper (alternately stack three times), and the outermost layer is defatted cotton non-woven fabric on both sides; first, perform low-pressure hydroentanglement treatment at a water pressure of 40 bar, then perform high-pressure hydroentanglement treatment at a water pressure of 130 bar for two hydroentanglement treatments, and dry to obtain soft and tensile all-cotton hydroentangled fabric.

[0027] Comparative Example 3: based on Example 1, exchange the ratio of perfluorooctyl ethyl acrylate and polyethylene glycol monomethallyl ether, and the rest of the process remains unchanged, as follows: Step one: preparation of modified defatted cotton: (1) add 100 parts of defatted cotton and 9.5 parts of chloroacetic acid to 200 parts of 20 wt% sodium hydroxide solution, stir at 65°C for 8h, wash, acidify, and dry to obtain carboxyl-modified defatted cotton; (2) add 100 parts of carboxyl-modified defatted cotton, 11 parts of N,N-dimethyl-1,3-diaminopropane, 22 parts of N,N'-dicyclohexyl carbodiimide, and 12 parts of 4-dimethylamino pyridine to 150 parts of tetrahydrofuran and mix uniformly, stir at 25°C for 4.5h, filter, wash, and dry to obtain N,N-dimethyl-modified defatted cotton; (3) add 100 parts of N,N-dimethyl-modified defatted cotton, 10.5 parts of triethylamine, and 11.5 parts of bromoethane to 40 wt% ethanol aqueous solution, stir at 60°C for 32h, filter, wash, and dry to obtain modified defatted cotton; Step two: preparation of fluorine-containing acrylamide copolymer: (1) add 15 parts of acrylamide and 2.5 parts of 2-acrylamido-2-methylpropanesulfonic acid to 100 parts of deionized water and stir uniformly, adjust the pH to 6.5±0.3 to obtain reaction monomer solution A; (2) add 0.3 parts of perfluorooctyl ethyl acrylate and 0.18 parts of polyethylene glycol monomethallyl ether to 10 parts of deionized water and stir uniformly to obtain reaction monomer solution B; (3) under a nitrogen atmosphere, mix reaction monomer solution A and hydrophilic reaction monomer solution B uniformly, add 0.1 wt% of initiator NaHSO3-K2S2O8 (molar ratio of oxidizing agent to reducing agent is 1:2), stir at 25°C for 4h, filter, wash, and dry to obtain fluorine-containing acrylamide copolymer; Step three: preparation of cotton paper: add fluorine-containing acrylamide copolymer to 60 wt% ethanol aqueous solution to prepare a solution with a concentration of 250 mg / L, uniformly spray it on the surface of water-absorbing cotton paper, and dry to obtain cotton paper; Step four: preparation of soft and tensile all-cotton hydroentangled fabric S1: mix modified defatted cotton and pure cotton at a mass ratio of 10:2.5, lay flat, set the water pressure to 90 bar for one hydroentanglement treatment, dry, defat, and dry again to obtain defatted cotton non-woven fabric (gram weight of 30 g / m 2 ); S2: alternately stack the defatted cotton non-woven fabric and the cotton paper (alternately stack three times), and the outermost layer is defatted cotton non-woven fabric on both sides; first, perform low-pressure hydroentanglement treatment at a water pressure of 40 bar, then perform high-pressure hydroentanglement treatment at a water pressure of 130 bar for two hydroentanglement treatments, and dry to obtain soft and tensile all-cotton hydroentangled fabric.

[0028] Comparative Example 4: Based on Example 1, the concentration of fluorine-containing acrylamide copolymer is increased, and the rest of the process remains unchanged, as follows: Step one: preparation of modified defatted cotton: (1) add 100 parts of defatted cotton and 9.5 parts of chloroacetic acid to 200 parts of 20 wt% sodium hydroxide solution, stir at 65°C for 8h, wash, acidify, and dry to obtain carboxyl-modified defatted cotton; (2) add 100 parts of carboxyl-modified defatted cotton, 11 parts of N,N-dimethyl-1,3-diaminopropane, 22 parts of N,N'-dicyclohexyl carbodiimide, and 12 parts of 4-dimethylamino pyridine to 150 parts of tetrahydrofuran and mix uniformly, stir at 25°C for 4.5h, filter, wash, and dry to obtain N,N-dimethyl-modified defatted cotton; (3) add 100 parts of N,N-dimethyl-modified defatted cotton, 10.5 parts of triethylamine, and 11.5 parts of bromoethane to 40 wt% ethanol aqueous solution, stir at 60°C for 32h, filter, wash, and dry to obtain modified defatted cotton; Step two: preparation of fluorine-containing acrylamide copolymer: (1) add 15 parts of acrylamide and 2.5 parts of 2-acrylamido-2-methylpropanesulfonic acid to 100 parts of deionized water and stir uniformly to obtain reaction monomer solution A; (2) add 0.18 parts of perfluorooctyl ethyl acrylate and 0.3 parts of polyethylene glycol monoallyl ether to 10 parts of deionized water and stir uniformly to obtain reaction monomer solution B; (3) under a nitrogen atmosphere, mix reaction monomer solution A and hydrophilic reaction monomer solution B uniformly, add 0.1 wt% of initiator NaHSO3-K2S2O8 (molar ratio of oxidizing agent to reducing agent is 1:2), stir at 25°C for 4h, filter, wash, and dry to obtain fluorine-containing acrylamide copolymer; Step three: preparation of cotton paper: add fluorine-containing acrylamide copolymer to 60 wt% ethanol aqueous solution to prepare a solution with a concentration of 600 mg / L, uniformly spray the solution on the surface of the water-absorbing cotton paper, and dry to obtain cotton paper; Step four: preparation of soft and tensile all-cotton hydroentangled fabric S1: mix modified defatted cotton and pure cotton at a mass ratio of 10:2.5, lay flat, set the water pressure to 90 bar for one hydroentanglement treatment, dry; defat, dry again, to obtain defatted cotton non-woven fabric (the grammage is 30 g / m 2 S2: alternately stack the defatted cotton non-woven fabric and the cotton paper (the number of alternately stacking is three times), and the outermost layer is defatted cotton non-woven fabric on both sides; first, low-pressure hydroentanglement treatment with a water pressure of 40 bar, then high-pressure hydroentanglement treatment with a water pressure of 130 bar for two hydroentanglement treatments, and dry to obtain soft and tensile all-cotton hydroentanglement fabric.

[0029] Performance test one: test the partial performance of the sample of example 1 according to GB / T 40276-2021, and the experimental data is shown in Table one: Table one

[0030] As shown in Table one, the defatted cotton non-woven fabric is obtained by using pure cotton and modified defatted cotton as pure cotton raw material for hydroentanglement, the cotton paper is obtained by spraying and drying the fluorine-containing acrylamide copolymer solution on the surface of the water-absorbing cotton paper, and the all-cotton hydroentanglement fabric is prepared by alternately stacking the cotton paper and the defatted cotton non-woven fabric and using pure cotton defatted cotton non-woven fabric as the outermost layer. The all-cotton hydroentanglement fabric has high tensile strength, strong liquid absorption, good softness, and certain antibacterial effect.

[0031] Performance test two: (1) test the breaking strength of the samples of each example and the comparative examples according to GB / T 24218.3-2010, the sample width is 50 mm, and the tensile rate is 100 mm / min; (2) test the absorption amount of the samples of each example and the comparative examples according to GB / T 24218.6-2010, the sample size is 100 mm*100 mm; the experimental data is shown in Table two.

[0032] Table two

[0033] As shown in Table two, the defatted cotton in comparative example 1 is not modified, the hydrophilicity is reduced, and the chemical bond is lacking, so the breaking strength is reduced, and the liquid absorption amount is reduced; in comparative example 2, polyethylene glycol monomethallyl ether is not added, due to the lack of polyethylene glycol monomethallyl ether wetting effect, the steric hindrance is large, and under the same amount of perfluoroalkyl ethyl acrylate, it is difficult for sodium dodecyl sulfonate to promote the increase of the polymer content, so the breaking strength is reduced, and the liquid absorption amount is reduced; in comparative example 3, the ratio of perfluoroalkyl ethyl acrylate and polyethylene glycol monomethallyl ether is exchanged, and the performance is obviously not as good as that of example 1; in comparative example 4, the concentration of fluorine-containing acrylamide copolymer is increased, the local hydrophobic region is too large, and even merges with each other, which seriously affects the hydroentanglement effect, the breaking strength is greatly reduced, and the liquid absorption amount is reduced. ​

[0034] It should be pointed out finally that the above only describes the preferred embodiments of the present application and is not intended to limit the present application. Although the present application has been described in detail with reference to the foregoing embodiments, those skilled in the art can still modify the technical solutions described in the foregoing embodiments or make equivalent replacements to some technical features. Any modification, equivalent replacement, improvement, etc. made within the spirit and principle of the present application shall be included in the protection scope of the present application.

Claims

1. A method for preparing a soft, tensile-resistant, all-cotton spunlace fabric, characterized in that: Includes the following steps: S1: (1) Carboxylation modification of degreased cotton; then N,N-dimethyl-1,3-diaminopropane is used to modify it into a tertiary amine; finally, it is quaternized to obtain modified degreased cotton; (2) Modified degreased cotton and pure cotton are mixed in proportion, laid flat, hydroentangled once, and dried; degreased and dried again to obtain degreased cotton nonwoven fabric; S2: Alternately layer degreased cotton nonwoven fabric and cotton paper, with the outermost layer consisting of degreased cotton nonwoven fabric on both sides; perform secondary hydroentangling treatment and drying to obtain soft, tensile-resistant all-cotton hydroentangled fabric.

2. The method for preparing a soft, tensile-resistant, all-cotton spunlace fabric according to claim 1, characterized in that: In step S2, the alternating layering is performed ≥3 times; the basis weight of the degreased cotton nonwoven fabric is 15~50 g / m². 2 The weight of cotton paper is 15~25g / m³. 2 .

3. The method for preparing a soft, tensile-resistant, all-cotton spunlace fabric according to claim 1, characterized in that: The raw materials of the degreased cotton nonwoven fabric are modified degreased cotton and pure cotton in a ratio of (2~3):

10.

4. The method for preparing a soft, tensile-resistant, all-cotton spunlace fabric according to claim 1, characterized in that: The preparation method of modified degreased cotton is as follows: (1) Add degreased cotton and chloroacetic acid to sodium hydroxide solution, stir at 60~70℃ for 7~8h, wash, acidify and dry to obtain carboxyl modified degreased cotton; (2) Add carboxyl modified degreased cotton, N,N-dimethyl-1,3-diaminopropane, N,N'-dicyclohexylcarbodiimide and 4-dimethylaminopyridine to tetrahydrofuran and mix evenly, stir at 20~25℃ for 4~5h, filter, wash and dry to obtain N,N-dimethyl modified degreased cotton; (3) Add N,N-dimethyl modified degreased cotton, triethylamine and bromoethane to an ethanol aqueous solution, stir at 60~65℃ for 30~40h, filter, wash and dry to obtain modified degreased cotton.

5. The method for preparing a soft, tensile-resistant, all-cotton spunlace fabric according to claim 1, characterized in that: The carboxyl-modified degreased cotton comprises the following raw materials, by mass: 100 parts degreased cotton, 9-10 parts chloroacetic acid, and 180-200 parts 15-20 wt% sodium hydroxide solution; The N,N-dimethyl modified degreased cotton comprises the following raw materials, by mass parts: 100 parts carboxyl modified degreased cotton, 10-12 parts N,N-dimethyl-1,3-diaminopropane, 21-23 parts N,N'-dicyclohexylcarbodiimide, 11-13 parts 4-dimethylaminopyridine, and 130-150 parts tetrahydrofuran; The modified degreased cotton comprises the following raw materials, by mass: 100 parts N,N-dimethyl modified degreased cotton, 10-11 parts triethylamine, 11-12 parts bromoethane, and 35-40 wt% ethanol aqueous solution.

6. The method for preparing a soft, tensile-resistant, all-cotton spunlace fabric according to claim 1, characterized in that: The water pressure for the first hydroentangling treatment is 80~100 bar; the specific process for the second hydroentangling treatment is as follows: first, low-pressure hydroentangling treatment at a water pressure of 35~50 bar, and then high-pressure hydroentangling treatment at a water pressure of 120~150 bar.

7. The method for preparing a soft, tensile-resistant, all-cotton spunlace fabric according to claim 1, characterized in that: The method for preparing the cotton paper is as follows: a fluoroacrylamide copolymer is prepared into a solution, uniformly sprayed onto the surface of absorbent cotton paper, and dried to obtain cotton paper; wherein, the concentration of the fluoroacrylamide copolymer is 200~300mg / L, and the solvent is a 50~70wt% aqueous ethanol solution.

8. The method for preparing a soft, tensile-resistant, all-cotton spunlace fabric according to claim 1, characterized in that: The preparation method of the fluorinated acrylamide copolymer includes the following steps: (1) Add acrylamide and 2-acrylamido-2-methylpropanesulfonic acid to deionized water and stir evenly, adjust the pH to 6.5±0.3 to obtain reaction monomer solution A; (2) Add perfluorooctyl ethyl acrylate and polyethylene glycol monoallyl ether to deionized water and stir evenly to obtain reaction monomer solution B; (3) Under a nitrogen atmosphere, mix reaction monomer solution A and reaction monomer solution B evenly, add 0.1~0.2wt% of initiator, stir at 25~30℃ for 4~4.5h, filter, wash and dry to obtain fluorinated acrylamide copolymer.

9. The method for preparing a soft, tensile-resistant, all-cotton spunlace fabric according to claim 1, characterized in that: The raw materials for the fluorinated acrylamide copolymer include, by weight, 14-16 parts acrylamide, 2-3 parts 2-acrylamido-2-methylpropanesulfonic acid, 0.15-0.2 parts perfluorooctyl ethyl acrylate, 0.3 parts polyethylene glycol monoallyl ether, and 0.05-0.1 parts initiator; wherein the polyethylene glycol monoallyl ether has a molecular weight of 400-1000.

10. A soft, tensile-resistant, all-cotton spunlace fabric, characterized in that: The soft, tensile-resistant spunlace cotton fabric is prepared by the preparation method according to any one of claims 1 to 9.

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