A method for preparing antibacterial soft fabric

Abstract

The invention relates to the technical field of fabrics, and discloses a method for preparing an antibacterial and compliant fabric. The invention uses p-aminostyrene, dicyandiamide, didodecylamine and the like as raw materials, and undergoes a series of reactions to obtain an intermediate 2. The amino group contained in chitosan is subjected to an amidation reaction with 4-chlorobutyric acid under the catalysis of EDC to obtain chlorinated chitosan. The chitosan and the intermediate 2 are subjected to a quaternization reaction, and modified chitosan is obtained under the acidification of hydrochloric acid, thereby obtaining modified chitosan fiber. Finally, the chitosan and cotton fiber are blended into yarn to obtain an antibacterial and compliant fabric. The invention has the advantages that the chitosan structure, the quaternary ammonium salt structure and the guanidine hydrochloride structure are all antibacterial structures, so that the prepared fabric has better antibacterial performance. Meanwhile, the modified chitosan can form a lipid film on the surface of the chitosan, so that the fabric has better compliant performance, and the comfort level of the fabric is further improved.

Description

Technical Field

[0001] The invention relates to the technical field of fabrics, and in particular to a method for preparing an antibacterial and compliant fabric. Background Art

[0002] In recent years, as people use more and more fabric clothing products, they have put forward higher requirements for the comfort, health and softness of fabric products. Cotton fiber generally refers to cotton. Fabrics made from cotton fiber are becoming more and more popular, but traditional cotton fiber products can no longer meet people's needs. Therefore, it is necessary to improve the softness and antibacterial properties of cotton fiber products.

[0003] Chitosan is a biopolysaccharide, a product obtained by deacetylation of chitin, with excellent antibacterial and biodegradable properties, and is widely used in clothing, medical treatment, industry, etc. Biguanide compounds can change the normal material and energy metabolism of organisms through the action of guanidine on certain specific groups or elements in organisms, thereby showing higher antibacterial and bactericidal properties, and biguanide compounds are also widely used as broad-spectrum bactericides.

[0004] For example, the patent with application publication number CN 104757724 A discloses a moisture-absorbing and quick-drying chitosan cotton knitted fabric. The invention uses cotton fiber and chitosan through a series of steps to prepare the fabric. The prepared fabric has good antibacterial, moisture-absorbing and breathable properties. Summary of the invention

[0005] 1. Technical issues to be solved

[0006] In view of the deficiencies in the prior art, the present invention provides a method for preparing an antibacterial and compliant fabric, and the prepared fabric has good antibacterial and compliant properties.

[0007] (II) Technical solution

[0008] A method for preparing an antibacterial and compliant fabric, the preparation method is as follows:

[0009] Step (1), adding p-aminostyrene to deionized water, stirring and dispersing, adding dicyandiamide thereto, stirring and mixing evenly, heating to 75-90° C., reacting for 5-10 hours, concentrating after the reaction, precipitating with acetone, filtering, recrystallizing, and drying to obtain intermediate 1, the reaction equation of which is:

[0010]

[0011] Step (2), adding intermediate 1 and didodecylamine to deionized water, stirring and dispersing, heating to 80-100° C., reacting for 30-60 min, and after the reaction is completed, distilling under reduced pressure, washing, and drying to obtain intermediate 2, the reaction equation of which is:

[0012] Step (3), adding chitosan powder to acetonitrile solvent, stirring and dispersing, then adding 1-ethyl-3-(3-dimethylaminopropyl) carbodiimide (EDC) and 4-chlorobutyric acid thereto, reacting at room temperature for 5-12 hours, after the reaction is completed, washing with deionized water, and drying to obtain chlorinated chitosan, the reaction equation of which is:

[0013] Step (4), adding chlorinated chitosan and intermediate 2 to acetonitrile solvent, stirring and dispersing, heating to 60-70° C., stirring and reacting for 3-6 hours, after the reaction is completed, rotary evaporation, washing with deionized water, drying, and then adding 30-40% hydrochloric acid aqueous solution thereto, stirring and dispersing for 40-120 minutes, and drying to obtain modified chitosan, the reaction equation of which is:

[0014] Step (5), adding modified chitosan to a 2% acetic acid aqueous solution to prepare a solution, stirring and dispersing, standing and degassing at 40-50° C., injecting the spinning solution into a 10 mL syringe, spinning at a flow rate of 0.5 mL / h, a spinning voltage of 15 kV, using a rotating drum as a receiving device, and a receiving distance of 15 cm to obtain modified chitosan fiber; then blending the modified chitosan fiber and cotton fiber in a mass ratio of 1-2:1 into yarn to obtain an antibacterial and soft fabric.

[0015] Furthermore, in the step (1), the usage ratio of p-aminostyrene to dicyandiamide is 1 mol:(2-2.5) mol.

[0016] Furthermore, in the step (2), the usage ratio of the intermediate 1 and didodecylamine is 1 mol:(0.8-1.2) mol.

[0017] Furthermore, in the step (3), the usage ratio of chitosan, EDC and 4-chlorobutyric acid is 1 g: (0.005-0.01) mol: (0.006-0.008) mol.

[0018] Furthermore, in the step (4), the usage ratio of chlorinated chitosan and intermediate 2 is 1 g: (0.008-0.015) mol.

[0019] Furthermore, in step (5), the mass fraction of the prepared solution is 2-5%.

[0020] (III) Beneficial technical effects

[0021] The present invention uses p-aminostyrene, dicyandiamide, didodecylamine and the like as raw materials, and obtains intermediate 2 through a series of reactions. The amino group contained in chitosan is subjected to an amidation reaction with 4-chlorobutyric acid under the catalysis of EDC to obtain chlorinated chitosan. The chitosan is then subjected to a quaternization reaction with intermediate 2, and modified chitosan is obtained under the acidification of hydrochloric acid, thereby obtaining modified chitosan fiber. Finally, the chitosan fiber is blended with cotton fiber into yarn to obtain antibacterial and soft fabric.

[0022] The modified chitosan prepared by the invention has a novel structure and contains a chitosan structure, a quaternary ammonium salt structure and a guanidinium hydrochloride structure, all of which are antibacterial structures. The quaternary ammonium salt structure is combined with the guanidinium hydrochloride structure and then grafted into chitosan to prepare a fabric. The prepared fabric has good antibacterial performance.

[0023] The modified chitosan prepared by the present invention contains more long carbon chains, which can form a lipid film on the surface of the chitosan, improve the surface structure of the fiber, reduce the friction coefficient between the fibers, so that the fabric has better softness and further improves the comfort of the fabric. The fabric prepared by the present invention has better softness and antibacterial properties. DETAILED DESCRIPTION

[0024] The present invention will be further described below in conjunction with specific embodiments:

[0025] Example 1

[0026] (1) Add 0.2 mol of p-aminostyrene to deionized water, stir and disperse, add 0.4 mol of dicyandiamide, stir and mix evenly, heat to 80° C., react for 6 h, and after the reaction is completed, concentrate, precipitate with acetone, filter, recrystallize, and dry to obtain intermediate 1.

[0027] (2) 1 mol of intermediate 1 and 1.1 mol of didodecylamine were added to deionized water, stirred and dispersed, heated to 85° C., and reacted for 50 min. After the reaction was completed, the mixture was distilled under reduced pressure, washed, and dried to obtain intermediate 2.

[0028] (3) 10 g of chitosan powder was added to acetonitrile solvent, stirred and dispersed, and then 0.08 mol of EDC and 0.08 mol of 4-chlorobutyric acid were added thereto. The mixture was reacted at room temperature for 12 h. After the reaction was completed, the mixture was washed with deionized water and dried to obtain chlorinated chitosan.

[0029] (4) 20 g of chlorinated chitosan and 0.16 mol of intermediate 2 were added to acetonitrile solvent, stirred and dispersed, heated to 70° C., and stirred for reaction for 5 h. After the reaction was completed, rotary evaporation was performed, the mixture was washed with deionized water, and dried. A 30% hydrochloric acid aqueous solution was then added, stirred and dispersed for 40 min, and dried to obtain modified chitosan.

[0030] (5) Add the modified chitosan to a 2% acetic acid aqueous solution to prepare a 2% solution, stir and disperse, stand at 40°C for degassing, inject the spinning solution into a 10mL syringe, and spin at a flow rate of 0.5mL / h. The spinning voltage is 15kV, and a rotating drum is used as a receiving device with a receiving distance of 15cm to obtain modified chitosan fiber; then, the modified chitosan fiber and cotton fiber with a mass ratio of 1:1 are blended into yarn to obtain an antibacterial and soft fabric.

[0031] Example 2

[0032] (1) Add 0.2 mol of p-aminostyrene to deionized water, stir and disperse, add 0.5 mol of dicyandiamide, stir and mix evenly, heat to 75° C., react for 10 h, and after the reaction is completed, concentrate, precipitate with acetone, filter, recrystallize, and dry to obtain intermediate 1.

[0033] (2) 1 mol of intermediate 1 and 0.8 mol of didodecylamine were added to deionized water, stirred and dispersed, heated to 100° C., and reacted for 40 min. After the reaction was completed, the mixture was distilled under reduced pressure, washed, and dried to obtain intermediate 2.

[0034] (3) 10 g of chitosan powder was added to acetonitrile solvent, stirred and dispersed, and then 0.1 mol of EDC and 0.08 mol of 4-chlorobutyric acid were added thereto. The mixture was reacted at room temperature for 10 h. After the reaction was completed, the mixture was washed with deionized water and dried to obtain chlorinated chitosan.

[0035] (4) 20 g of chlorinated chitosan and 0.1 mol of intermediate 2 were added to acetonitrile solvent, stirred and dispersed, heated to 60° C., stirred and reacted for 6 h. After the reaction was completed, rotary evaporation was performed, the mixture was washed with deionized water, and dried. A 40% hydrochloric acid aqueous solution was then added, stirred and dispersed for 120 min, and dried to obtain modified chitosan.

[0036] (5) Add the modified chitosan to a 2% acetic acid aqueous solution to prepare a 3% solution, stir and disperse, stand at 50°C for degassing, inject the spinning solution into a 10mL syringe, and spin at a flow rate of 0.5mL / h. The spinning voltage is 15kV, and a rotating drum is used as a receiving device with a receiving distance of 15cm to obtain modified chitosan fiber; then the modified chitosan fiber and cotton fiber with a mass ratio of 1.2:1 are blended into yarn to obtain an antibacterial and soft fabric.

[0037] Example 3

[0038] (1) Add 0.2 mol of p-aminostyrene to deionized water, stir and disperse, add 0.45 mol of dicyandiamide, stir and mix evenly, heat to 90° C., react for 5 h, and after the reaction is completed, concentrate, precipitate with acetone, filter, recrystallize, and dry to obtain intermediate 1.

[0039] (2) 1 mol of intermediate 1 and 1 mol of didodecylamine were added to deionized water, stirred and dispersed, heated to 90° C., and reacted for 60 min. After the reaction was completed, the mixture was distilled under reduced pressure, washed, and dried to obtain intermediate 2.

[0040] (3) 10 g of chitosan powder was added to acetonitrile solvent, stirred and dispersed, and then 0.1 mol of EDC and 0.06 mol of 4-chlorobutyric acid were added thereto. The mixture was reacted at room temperature for 5 h. After the reaction was completed, the mixture was washed with deionized water and dried to obtain chlorinated chitosan.

[0041] (4) 20 g of chlorinated chitosan and 0.2 mol of intermediate 2 were added to acetonitrile solvent, stirred and dispersed, heated to 70° C., and stirred for reaction for 3 h. After the reaction was completed, rotary evaporation was performed, the mixture was washed with deionized water, and dried. A 35% hydrochloric acid aqueous solution was then added, stirred and dispersed for 60 min, and dried to obtain modified chitosan.

[0042] (5) Add the modified chitosan to a 2% acetic acid aqueous solution to prepare a 4% solution, stir and disperse, stand at 45°C for degassing, inject the spinning solution into a 10mL syringe, and spin at a flow rate of 0.5mL / h. The spinning voltage is 15kV, and a rotating drum is used as a receiving device with a receiving distance of 15cm to obtain modified chitosan fiber; then the modified chitosan fiber and cotton fiber with a mass ratio of 1.5:1 are blended into yarn to obtain an antibacterial and soft fabric.

[0043] Example 4

[0044] (1) Add 0.2 mol of p-aminostyrene to deionized water, stir and disperse, add 0.45 mol of dicyandiamide, stir and mix evenly, heat to 85° C., react for 6 h, and after the reaction is completed, concentrate, precipitate with acetone, filter, recrystallize, and dry to obtain intermediate 1.

[0045] (2) 1 mol of intermediate 1 and 1.2 mol of didodecylamine were added to deionized water, stirred and dispersed, heated to 80° C., and reacted for 50 min. After the reaction was completed, the mixture was distilled under reduced pressure, washed, and dried to obtain intermediate 2.

[0046] (3) 10 g of chitosan powder was added to acetonitrile solvent, stirred and dispersed, and then 0.06 mol of EDC and 0.07 mol of 4-chlorobutyric acid were added thereto. The mixture was reacted at room temperature for 12 h. After the reaction was completed, the mixture was washed with deionized water and dried to obtain chlorinated chitosan.

[0047] (4) 20 g of chlorinated chitosan and 0.25 mol of intermediate 2 were added to acetonitrile solvent, stirred and dispersed, heated to 65° C., stirred and reacted for 6 h. After the reaction was completed, rotary evaporation was performed, the mixture was washed with deionized water, and dried. A 35% hydrochloric acid aqueous solution was then added, stirred and dispersed for 120 min, and dried to obtain modified chitosan.

[0048] (5) Add the modified chitosan to a 2% acetic acid aqueous solution to prepare a 4.5% solution, stir and disperse, stand at 50°C for degassing, inject the spinning solution into a 10mL syringe, and spin at a flow rate of 0.5mL / h. The spinning voltage is 15kV, and a rotating drum is used as a receiving device with a receiving distance of 15cm to obtain modified chitosan fiber; then the modified chitosan fiber and cotton fiber with a mass ratio of 1.8:1 are blended into yarn to obtain an antibacterial and soft fabric.

[0049] Example 5

[0050] (1) Add 0.2 mol of p-aminostyrene to deionized water, stir and disperse, add 0.4 mol of dicyandiamide, stir and mix evenly, heat to 90° C., react for 6 h, and after the reaction is completed, concentrate, precipitate with acetone, filter, recrystallize, and dry to obtain intermediate 1.

[0051] (2) 1 mol of intermediate 1 and 0.8 mol of didodecylamine were added to deionized water, stirred and dispersed, heated to 100° C., and reacted for 30 min. After the reaction was completed, the mixture was distilled under reduced pressure, washed, and dried to obtain intermediate 2.

[0052] (3) 10 g of chitosan powder was added to acetonitrile solvent, stirred and dispersed, and then 0.05 mol of EDC and 0.08 mol of 4-chlorobutyric acid were added thereto. The mixture was reacted at room temperature for 10 h. After the reaction was completed, the mixture was washed with deionized water and dried to obtain chlorinated chitosan.

[0053] (4) 20 g of chlorinated chitosan and 0.2 mol of intermediate 2 were added to acetonitrile solvent, stirred and dispersed, heated to 65° C., stirred and reacted for 6 h. After the reaction was completed, rotary evaporation was performed, the mixture was washed with deionized water, and dried. A 40% hydrochloric acid aqueous solution was then added, stirred and dispersed for 120 min, and dried to obtain modified chitosan.

[0054] (5) Add the modified chitosan to a 2% acetic acid aqueous solution to prepare a 5% solution, stir and disperse, stand at 40°C for degassing, inject the spinning solution into a 10mL syringe, and spin at a flow rate of 0.5mL / h. The spinning voltage is 15kV, and a rotating drum is used as a receiving device with a receiving distance of 15cm to obtain modified chitosan fiber; then the modified chitosan fiber and cotton fiber with a mass ratio of 2:1 are blended into yarn to obtain an antibacterial and soft fabric.

[0055] Referring to GB / T20944.3-2008 and FZ / T73023-2006, the test size was 10cm×10cm, and Escherichia coli and Staphylococcus aureus were used as test bacteria for antibacterial performance testing.

[0056] Table 1:

[0057]

[0058] It can be seen from the table that the antibacterial rates of the fabrics prepared by the present invention can reach up to 98.23% and 99.84% at the highest. Therefore, the fabrics prepared by the present invention have good antibacterial properties.

[0059] Refer to ZBW04002-86 and use a fabric softness tester to test the softness.

[0060] Table 2:

[0061] Softness Example 1 Level 2 Example 2 Level 3 Example 3 Level 3 Example 4 Level 4 Example 5 Level 4

[0062] It can be seen from the table that the fabric prepared by the present invention has good softness.

[0063] The above description of the disclosed embodiments enables those skilled in the art to implement or use the present invention. Various modifications to these embodiments will be 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 will not be limited to the embodiments shown herein, but rather to the widest scope consistent with the principles and novel features disclosed herein.

Claims

1. A method for preparing an antibacterial and compliant fabric, characterized in that: The preparation method is as follows: Step (1), adding p-aminostyrene to deionized water, stirring and dispersing, adding dicyandiamide thereto, stirring and mixing evenly, heating to 75-90° C., reacting for 5-10 hours, concentrating after the reaction, precipitating with acetone, filtering, recrystallizing, and drying to obtain intermediate 1; Step (2), adding intermediate 1 and didodecylamine to deionized water, stirring and dispersing, heating to 80-100° C., reacting for 30-60 min, and after the reaction is completed, distilling under reduced pressure, washing, and drying to obtain intermediate 2; Step (3), adding chitosan powder to acetonitrile solvent, stirring and dispersing, then adding EDC and 4-chlorobutyric acid thereto, reacting at room temperature for 5-12 hours, and after the reaction is completed, washing with deionized water and drying to obtain chlorinated chitosan; Step (4), adding chlorinated chitosan and intermediate 2 to acetonitrile solvent, stirring and dispersing, heating to 60-70° C., stirring and reacting for 3-6 hours, after the reaction is completed, rotary evaporation, washing with deionized water, drying, and then adding 30-40% hydrochloric acid aqueous solution thereto, stirring and dispersing for 40-120 minutes, and drying to obtain modified chitosan; Step (5), adding the modified chitosan to a 2% acetic acid aqueous solution to prepare a solution, stirring and dispersing, standing at 40-50° C. for degassing, injecting the spinning solution into a 10 mL syringe, spinning at a flow rate of 0.5 mL / h, a spinning voltage of 15 kV, using a rotating drum as a receiving device, and a receiving distance of 15 cm to obtain modified chitosan fiber; then blending the modified chitosan fiber and cotton fiber into yarn to obtain an antibacterial and soft fabric.

2. The method for preparing the antibacterial and compliant fabric according to claim 1, characterized in that: In the step (1), the usage ratio of p-aminostyrene to dicyandiamide is 1 mol:(2-2.5) mol.

3. The method for preparing the antibacterial and compliant fabric according to claim 1, characterized in that: In the step (2), the usage ratio of the intermediate 1 and didodecylamine is 1 mol:(0.8-1.2) mol.

4. The method for preparing the antibacterial and compliant fabric according to claim 1, characterized in that: In the step (3), the usage ratio of chitosan, EDC and 4-chlorobutyric acid is 1 g: (0.005-0.01) mol: (0.006-0.008) mol.

5. The method for preparing the antibacterial and compliant fabric according to claim 1, characterized in that: In the step (4), the usage ratio of chlorinated chitosan and intermediate 2 is 1 g: (0.008-0.015) mol.

6. The method for preparing the antibacterial and compliant fabric according to claim 1, characterized in that: In the step (5), the mass fraction of the prepared solution is 2-5%.

7. The method for preparing the antibacterial and compliant fabric according to claim 1, characterized in that: In the step (5), the mass ratio of the modified chitosan fiber to the cotton fiber is 1-2:1.

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