Cooling antistatic comfortable fabric and preparation method thereof

Abstract

The present application relates to the technical field of fabric, and discloses a cool and comfortable fabric with antistatic property and a preparation method thereof, wherein pentanedioic acid (glycine), 1,3-bis(3-glycidyl ether oxypropyl) tetramethyl disiloxane and epichlorohydrin are reacted to obtain an epoxy quaternary ammonium finishing agent, and cotton fabric is finished to obtain the cool and comfortable fabric with antistatic property. The epoxy quaternary ammonium finishing agent contains a flexible siloxane structure, which can improve the softness and wrinkle resistance of the cotton fabric. Meanwhile, the epoxy quaternary ammonium finishing agent contains quaternary ammonium salt and carboxyl hydrophilic groups, so that the cotton fabric has good hydrophilicity and cool feeling. The epoxy quaternary ammonium finishing agent contains quaternary ammonium salt cations, which can increase the conductivity of the surface of the cotton fabric and reduce the surface resistivity, thereby improving the antistatic property. Moreover, after multiple washes, the cotton fabric still has good softness, wrinkle resistance and antistatic property.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of fabric, in particular to a cool and anti-static comfortable fabric and a preparation method thereof. BACKGROUND

[0002] Cotton fabric has good hydrophilic and moisture absorption, air permeability, warmth and heat resistance, and is widely used in fabric and clothing. The traditional cotton fabric has poor wrinkle resistance and poor anti-static performance, which hinders the development and application of cotton fabric in high-grade clothing fabric. The cotton fabric can be finished with finishing agent to give it anti-static, soft and wrinkle resistance and wearing comfort.

[0003] The commonly used soft finishing agent is silicone finishing agent, but the hydrophobicity of the silicone finishing agent is large, which will affect the hydrophilic and moisture absorption performance of the cotton fabric. Modification of the silicone finishing agent is a research hotspot, such as amino-modified silicone finishing agent, polyether-modified silicone finishing agent, etc., which can make the cotton fabric maintain good softness and wrinkle resistance and hydrophilic and moisture absorption, but these silicone finishing agents are difficult to improve the anti-static performance of the cotton fabric. The patent with publication number CN106835715B discloses a cotton moisture absorption and heat dissipation finishing agent and a preparation method thereof, which uses amino-modified polysiloxane, block polysiloxane and alkyl glycoside surfactant as raw materials. The prepared finishing agent can improve the moisture absorption, heat dissipation and anti-static performance of the cotton fabric, but the polysiloxane finishing agent of the patent does not have anti-static performance, and additional surfactant is needed to improve the anti-static performance of the cotton fabric. SUMMARY

[0004] (I) Technical problems solved:

[0005] In view of the shortcomings of the prior art, the present application provides a cool and anti-static comfortable fabric, which improves the anti-static performance and soft hand feeling of the cotton fabric, and maintains good hydrophilicity.

[0006] (II) Technical scheme: a preparation method of a cool and anti-static comfortable fabric:

[0007] (1) adding glycine and potassium hydroxide into ethanol, stirring, then adding glutaraldehyde, stirring at 40-55 DEG C for 2-3h Schiff base condensation reaction, cooling to room temperature, adding sodium borohydride, controlling the molar ratio of glycine, potassium hydroxide, glutaraldehyde and sodium borohydride to be (2-2.2):(2-2.2):1:(2.6-3); reducing reaction for 3-4h, adding hydrochloric acid solution to adjust pH to 3-4, precipitate, filter, dissolve the product in ethanol aqueous solution, heat and evaporate, cool and crystallize to obtain glutaraldehyde (glycine). The reaction formula is:

[0008]

[0009] (2) adding pentanedio(glycine), 1,3-bis(3-glycidyl ether oxypropyl) tetramethyl disiloxane in a molar ratio of (1.2-1.5):1 to a solvent, distilling under reduced pressure after reaction, washing with acetone, drying to obtain finishing agent precursor.

[0010] (3) adding finishing agent precursor, epichlorohydrin in a mass ratio of 100:(5-60) to a solvent, distilling under reduced pressure after reaction, washing with acetone, drying to obtain epoxy quaternary ammonium finishing agent. The reaction formula is:

[0011]

[0012] (4) adding epoxy quaternary ammonium finishing agent to water, stirring, then adding cotton fabric, controlling bath ratio to be 1:(40-50); soaking at 60-70 DEG C for 30-60 min, then carrying out two-dip-two-pad finishing, picking up rate being 80-90%; taking out the cotton fabric, pre-washing at 80-100 DEG C for 4-7 min, then baking at 140-150 DEG C for 3-4 min, washing and drying to obtain cool anti-static comfortable fabric.

[0013] Further, the solvent in (2) is isopropyl alcohol or N,N-dimethylformamide.

[0014] Further, the reaction in (2) is stirred at 65-85 DEG C for 10-15 h.

[0015] Further, the solvent in (3) is isopropyl alcohol, N,N-dimethylformamide, 1,4-dioxane or tetrahydrofuran.

[0016] Further, the reaction in (3) is carried out at 60-80 DEG C for 6-10 h.

[0017] Further, the ratio of water to epoxy quaternary ammonium finishing agent in (4) is 1L:(10-40)g.

[0018] (Three) beneficial technical effects: the imino group of pentanedio(glycine) and the epoxy group of 1,3-bis(3-glycidyl ether oxypropyl) tetramethyl disiloxane are subjected to addition polymerization reaction, then quaternary ammonium reaction with epichlorohydrin to obtain epoxy quaternary ammonium finishing agent, then finishing cotton fabric, the epoxy quaternary ammonium finishing agent contains flexible siloxane structure, which can improve the softness, wrinkle resistance and wearing comfort of cotton fabric, and contains quaternary ammonium salt and carboxyl hydrophilic group, so that the cotton fabric maintains good hydrophilicity and cool feeling.

[0019] The epoxy quaternary ammonium finishing agent of the application contains quaternary ammonium salt cation, which can increase the conductivity of the surface of cotton fabric and reduce the surface resistivity, thereby improving the anti-static performance.

[0020] The epoxy quaternary ammonium finishing agent contains an epoxy group, which can react with the hydroxyl group of cellulose in the cotton fabric, thereby grafting the finishing agent to the surface of the cotton fabric through a chemical bond, and the carboxyl group contained in the finishing agent can form a hydrogen bond interaction with the surface of the cotton fabric, thereby firmly attaching a large amount of finishing agent to the surface of the cotton fabric, which is not easy to wash off, has good washing resistance, and after multiple washing, the cotton fabric still has a high crease recovery angle and a low surface resistivity, maintaining good softness, wrinkle resistance and antistatic performance. DETAILED DESCRIPTION

[0021] The detailed description set forth below should not be interpreted as a limitation on the scope or the application of the present application but merely as a description of certain aspects, features and embodiments of the present application. It should be understood that the terms used herein are for the purpose of describing particular embodiments and are not intended to be limiting of the present application.

[0022] Example 1

[0023] (1) 100 mmol of glycine, 100 mmol of potassium hydroxide were added to 500 mL of ethanol, after stirring, 50 mmol of glutaraldehyde was added, and Schiff base condensation reaction was carried out at 55°C for 2h, and then cooled to room temperature, 150 mmol of sodium borohydride was added, and reduction reaction was carried out for 3h, and then hydrochloric acid solution was added dropwise to adjust the pH to 4, and then the precipitate was separated, filtered, and the product was dissolved in 300 mL of 40% ethanol aqueous solution, heated and evaporated, and then cooled and crystallized to obtain pentanedio(glycine).

[0024] (2) 260 mmol of pentanedio(glycine), 200 mmol of 1,3-bis(3-glycidyl ether oxypropyl) tetramethyl disiloxane were added to 700 mL of isopropyl alcohol, and then stirred and refluxed at 85°C for 10h, and then distilled under reduced pressure, washed with acetone and dried to obtain the finishing agent precursor.

[0025] (3) 200 g of the finishing agent precursor, 10 g of epoxy chloropropane were added to 2.5 L of 1,4-dioxane, and then stirred and reacted at 75°C for 6h, and then distilled under reduced pressure, washed with acetone and dried to obtain the epoxy quaternary ammonium finishing agent.

[0026] (4) 100 g of the epoxy quaternary ammonium finishing agent was added to 10 L of water, and then cotton fabric was added after stirring, and the bath ratio was controlled to be 1:40; and then soaked at 70°C for 30 min, and then finished by double dipping and double padding, and the padding rate was 85%; and then the cotton fabric was taken out, pre-washed at 100°C for 4 min, and then baked at 140°C for 3 min, and then washed and dried to obtain the cool and antistatic comfortable fabric.

[0027] Example 2

[0028] (1) To 600 mL of ethanol, 110 mmol of glycine and 110 mmol of potassium hydroxide were added, and after stirring, 50 mmol of glutaraldehyde was added, and the Schiff base condensation reaction was carried out at 40°C for 3 h, cooled to room temperature, 130 mmol of sodium borohydride was added, and the reduction reaction was carried out for 4 h, and the pH was adjusted to 3 by adding a hydrochloric acid solution, and the precipitate was separated, and the product was dissolved in 300 mL of 40% ethanol aqueous solution, and heated to evaporate, and cooled to crystallize, to obtain glutaroyl (glycine).

[0029] (2) To 700 mL of N,N-dimethylformamide, 300 mmol of glutaroyl (glycine) and 200 mmol of 1,3-bis(3-glycidyl ether oxypropyl) tetramethyl disiloxane were added, and the reaction was carried out at 80°C for 12 h with stirring, and distilled under reduced pressure, washed with acetone, and dried to obtain a finishing agent precursor.

[0030] (3) To 2.5 L of N,N-dimethylformamide, 200 g of the finishing agent precursor and 45 g of epichlorohydrin were added, and the reaction was carried out at 80°C for 6 h with stirring, and distilled under reduced pressure, washed with acetone, and dried to obtain an epoxy quaternary ammonium finishing agent.

[0031] (4) To 10 L of water, 200 g of the epoxy quaternary ammonium finishing agent was added, and after stirring, cotton fabric was added, and the bath ratio was controlled to be 1:40; soaked at 60°C for 60 min, and then two-dip-two-pad finishing was carried out, and the pick-up rate was 80%; the cotton fabric was taken out, pre-washed at 80°C for 7 min, and then baked at 140°C for 4 min, and after washing and drying, a cool and anti-static comfortable fabric was obtained.

[0032] Example 3:

[0033] (1) To 800 mL of N,N-dimethylformamide, 280 mmol of glutaroyl (glycine) (prepared according to the method of Example 1) and 200 mmol of 1,3-bis(3-glycidyl ether oxypropyl) tetramethyl disiloxane were added, and the reaction was carried out at 85°C for 10 h with stirring, and distilled under reduced pressure, washed with acetone, and dried to obtain a finishing agent precursor.

[0034] (2) To 3.5 L of tetrahydrofuran, 200 g of the finishing agent precursor and 80 g of epichlorohydrin were added, and the reaction was carried out at 60°C for 10 h with stirring, and distilled under reduced pressure, washed with acetone, and dried to obtain an epoxy quaternary ammonium finishing agent.

[0035] (3) To 10 L of water, 30 g of the epoxy quaternary ammonium finishing agent was added, and after stirring, cotton fabric was added, and the bath ratio was controlled to be 1:50; soaked at 70°C for 40 min, and then two-dip-two-pad finishing was carried out, and the pick-up rate was 90%; the cotton fabric was taken out, pre-washed at 90°C for 6 min, and then baked at 150°C for 3 min, and after washing and drying, a cool and anti-static comfortable fabric was obtained.

[0036] Example 4:

[0037] (1) To 800 mL of isopropyl alcohol, 240 mmol of pentane di(glycine) (prepared according to the method of Example 1), 200 mmol of 1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane were added, and the reaction was stirred at 65 °C for 15 h, distilled under reduced pressure, washed with acetone, and dried to obtain the finishing agent precursor.

[0038] (2) To 3.5 L of isopropyl alcohol, 200 g of the finishing agent precursor, 120 g of epichlorohydrin were added, and the reaction was stirred at 80 °C for 8 h, distilled under reduced pressure, washed with acetone, and dried to obtain the epoxy quaternary ammonium finishing agent.

[0039] (3) To 10 L of water, 400 g of the epoxy quaternary ammonium finishing agent was added, and after stirring, cotton fabric was added, and the bath ratio was controlled to be 1:40; the cotton fabric was soaked at 70 °C for 40 min, and then two-dip-two-pad finishing was carried out, with a pick-up rate of 85%; the cotton fabric was taken out, pre-washed at 90 °C for 6 min, and then baked at 150 °C for 3 min, and after washing and drying, a cool- feeling antistatic comfortable fabric was obtained.

[0040] Comparative Example 1:

[0041] (1) To 10 L of water, 100 g of the finishing agent precursor (prepared according to the method of Example 1) was added, and after stirring, cotton fabric was added, and the bath ratio was controlled to be 1:40; the cotton fabric was soaked at 70 °C for 30 min, and then two-dip-two-pad finishing was carried out, with a pick-up rate of 85%; the cotton fabric was taken out, pre-washed at 100 °C for 4 min, and then baked at 140 °C for 3 min, and after washing and drying, a fabric was obtained.

[0042] Comparative Example 2:

[0043] (1) To 700 mL of isopropyl alcohol, 260 mmol of pentane di(glycine) (prepared according to the method of Example 1), 200 mmol of ethylene glycol diglycidyl were added, and the reaction was stirred and refluxed at 85 °C for 10 h, distilled under reduced pressure, washed with acetone, and dried to obtain the finishing agent precursor.

[0044] (2) To 2.5 L of 1,4-dioxane, 200 g of the finishing agent precursor, 10 g of epichlorohydrin were added, and the reaction was stirred at 75 °C for 6 h, distilled under reduced pressure, washed with acetone, and dried to obtain the epoxy quaternary ammonium finishing agent.

[0045] (3) To 10 L of water, 100 g of the epoxy quaternary ammonium finishing agent was added, and after stirring, cotton fabric was added, and the bath ratio was controlled to be 1:40; the cotton fabric was soaked at 70 °C for 30 min, and then two-dip-two-pad finishing was carried out, with a pick-up rate of 85%; the cotton fabric was taken out, pre-washed at 100 °C for 4 min, and then baked at 140 °C for 3 min, and after washing and drying, a fabric was obtained.

[0046] Comparative Example 3

[0047] (1) 260 mmol N,N'-dimethylethylenediamine (structure formula ), 200 mmol 1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane, stirring and condensing reflux reaction at 85°C for 10h, distillation under reduced pressure, acetone washing, drying, to get finishing agent precursor.

[0048] (2) 200g finishing agent precursor, 10g epichlorohydrin were added to 2.5L 1,4-dioxane, stirring reaction at 75°C for 6h, distillation under reduced pressure, acetone washing, drying, to get epoxy quaternary ammonium finishing agent.

[0049] (3) 100g epoxy quaternary ammonium finishing agent was added to 10L water, after stirring, cotton fabric was added, and the bath ratio was controlled to be 1:40; soaked at 70°C for 30min, then two-dip-two-pad finishing was carried out, and the pick-up rate was 85%; the cotton fabric was taken out, pre-washed at 100°C for 4min, and then baked at 140°C for 3min, washed and dried to get the fabric.

[0050] The ordinary cotton fabric was used as a blank sample.

[0051] The water drop spreading time and hydrophilicity of the fabric were tested according to AATCC-79 standard.

[0052] The surface resistivity and antistatic property of the fabric were tested according to GB / T 12703.4-2010 standard. The surface resistivity was tested again after the fabric was subjected to washing and drying process for 30 times according to GB / T 8629-2017 standard.

[0053] The warp+weft crease recovery angle of the fabric was tested according to GB / T 3819-1997 standard. The crease recovery angle was tested again after the fabric was subjected to washing and drying process for 30 times according to GB / T 8629-2017 standard.

[0054] Table 1 Fabric performance test

[0055]

[0056] After testing, compared with the cotton fabric blank sample, the crease recovery angle of the cotton fabric of Examples 1-4 after being finished with the epoxy quaternary ammonium finishing agent is obviously increased, and the surface resistivity is reduced, and the cotton fabric has good softness, wrinkle resistance, and antistatic performance, and the water drop spreading time is low, and the cotton fabric still has good hydrophilicity. This is mainly because the epoxy quaternary ammonium finishing agent contains a flexible siloxane structure, which can improve the softness, wrinkle resistance, and wearing comfort of the cotton fabric, and at the same time contains a quaternary ammonium salt and a carboxyl hydrophilic group, so that the cotton fabric maintains good hydrophilicity, and the quaternary ammonium salt cation can increase the conductivity of the surface of the cotton fabric and reduce the surface resistivity, thereby improving the antistatic performance. After multiple washes, the cotton fabric still has a high crease recovery angle and a low surface resistivity, mainly because the finishing agent contains an epoxy group that can react with the hydroxyl groups of cellulose in the cotton fabric, thereby grafting the finishing agent to the surface of the cotton fabric through a chemical bond, and the carboxyl group of the finishing agent can form a hydrogen bond interaction with the surface of the cotton fabric, thereby allowing a large amount of finishing agent to be firmly attached to the surface of the cotton fabric and not easily washed off.

[0057] Compared with Example 1, the finishing agent precursor of Comparative Example 1 does not contain a quaternary ammonium salt, resulting in a larger water drop spreading time and surface resistivity of the cotton fabric, and poor hydrophilicity and antistatic performance. At the same time, the finishing agent precursor does not contain an epoxy group and cannot react with the cotton fabric, resulting in the finishing agent precursor not being firmly attached to the surface of the cotton fabric, and being washed off in solution. After washing, the crease recovery angle of the cotton fabric decreases by a large margin, and the softness and wrinkle resistance of the cotton fabric deteriorate.

[0058] Comparative Example 2 uses ethylene glycol diglycidyl as a raw material to prepare a finishing agent that does not contain a flexible siloxane structure, resulting in a lower crease recovery angle of the cotton fabric and poor softness and wrinkle resistance.

[0059] Comparative Example 3 uses N,N'-dimethylethylenediamine to prepare a finishing agent that does not contain a hydrophilic carboxyl group, resulting in a larger water drop spreading time of the cotton fabric and poor hydrophilicity. In addition, the finishing agent does not contain a carboxyl group, and the hydrogen bond interaction force between the finishing agent and the surface of the cotton fabric is lower than that of Example 1, resulting in the finishing agent being easily washed off. After multiple washes, the crease recovery angle decreases by a large margin, the softness and wrinkle resistance of the cotton fabric are poor, the surface resistivity increases by a large margin, and the antistatic performance deteriorates.

[0060] The above-described examples only describe the preferred modes of the present application and do not limit the scope of the present application. Without departing from the design spirit of the present application, various modifications and improvements to the technical solutions of the present application made by those of ordinary skill in the art should fall within the protection scope determined by the claims of the present application.

Claims

1. A method for preparing a cool antistatic comfortable fabric, characterized in that: The preparation method is: (1) adding pentylene(glycine) and 1,3-bis(3-glycidyloxypropyl)tetramethyldisiloxane in a molar ratio of (1.2-1.5):1 to a solvent, and performing distillation under reduced pressure after the reaction, washing, and drying to obtain a finishing agent precursor; (2) adding a finishing agent precursor and epichlorohydrin in a mass ratio of 100:(5-60) to a solvent, distilling under reduced pressure after the reaction, washing, and drying to obtain an epoxy quaternary ammonium finishing agent; (3) adding an epoxy quaternary ammonium finishing agent to water, stirring, and then adding cotton fabric, soaking and then performing two-dip and two-padding finishing, taking out the cotton fabric, pre-baking, baking, washing and drying to obtain a cool antistatic and comfortable fabric; The preparation method of glutaraldehyde in (1) is as follows: glycine and potassium hydroxide are added to ethanol, glutaraldehyde is added after stirring, the mixture is stirred at 40-55°C for 2-3 hours, the mixture is cooled to room temperature, sodium borohydride is added, the reaction is continued for 3-4 hours, hydrochloric acid solution is added dropwise to adjust the pH to 3-4, a precipitate is precipitated, the precipitate is filtered, the product is dissolved in ethanol aqueous solution, heated for volatilization, and cooled for crystallization to obtain glutaraldehyde.

2. The method for preparing the cool antistatic comfortable fabric according to claim 1, characterized in that: The solvent in (1) is isopropyl alcohol or N,N-dimethylformamide.

3. The method for preparing the cool antistatic comfortable fabric according to claim 1, characterized in that: The reaction in (1) is stirred at 65-85°C for 10-15h.

4. The method for preparing the cool antistatic comfortable fabric according to claim 1, characterized in that: The solvent in (2) is isopropyl alcohol, N,N-dimethylformamide, 1,4-dioxane or tetrahydrofuran.

5. The method for preparing the cool antistatic comfortable fabric according to claim 1, characterized in that: The reaction in (2) is carried out at 60-80°C for 6-10 hours.

6. The method for preparing the cool antistatic comfortable fabric according to claim 1, characterized in that: The ratio of water to epoxy quaternary ammonium finishing agent in (3) is 1L:(10-40)g.

7. The method for preparing the cool antistatic comfortable fabric according to claim 1, characterized in that: Cotton fabric is added to the (3) and the bath ratio is controlled to be 1:(40-50); the rolling rate of the double-immersion and double-rolling finishing is 80-90%; the temperature during the soaking is 60-70°C and the time is 30-60 minutes; the temperature of the pre-baking is 80-100°C and the time is 4-7 minutes; the temperature of the baking is 140-150°C and the time is 3-4 minutes.

8. The method for preparing the cool antistatic comfortable fabric according to claim 1, characterized in that: In the preparation method of glutaric acid (glycine), the molar ratio of glycine, potassium hydroxide, glutaraldehyde and sodium borohydride is (2-2.2):(2-2.2):1:(2.6-3).

9. A cool, antistatic, and comfortable fabric obtained by the preparation method according to any one of claims 1 to 8.

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