A method for preparing a cotton fabric softener with high loft and smooth touch.

Abstract

This invention relates to the technical field of fabric softeners and discloses a method for preparing a fabric softener for cotton fabrics with high fluffiness and a smooth feel. The method includes the following steps: mixing silicone oil a, silicone oil b, and additives to obtain the softener; the raw materials for silicone oil a include terminal epoxy polyether silicone oil, polyether amine, solvent, and fatty acid; the raw materials for silicone oil b include terminal epoxy silicone oil, polyether amine, solvent, and fatty acid; the mass ratio of silicone oil a to silicone oil b is 60-90%:10-40%, and the total mass percentage is 100%. This invention obtains a softener by compounding two silicone oils, which has good self-emulsifying properties, stability, and hydrophilicity. It not only helps to penetrate deep into cotton fibers, providing a soft hand feel to the fabric, but also better adheres to the surface of cotton fabrics, providing a fluffi and smooth hand feel.

Description

Technical Field

[0001] This invention relates to the technical field of fabric softeners, and in particular to a method for preparing a fabric softener for cotton fabrics that has a high degree of fluffiness and a smooth feel. Background Technology

[0002] The softness of cotton fabrics is one of the most valued qualities by consumers. Improving the softness of cotton textile products not only enhances product competitiveness but also increases their added value and profitability. Softening finishing is an important post-processing step in dyeing and printing, and currently, softeners are widely used. As an indispensable auxiliary agent in the textile industry, softeners play an irreplaceable role in improving the softness and hand feel of fabrics.

[0003] Softeners primarily act on the fiber surface, forming a lubricating film to reduce inter-fiber friction. Additionally, some softeners with relatively small molecular weights can penetrate the fiber interior, lowering its glass transition temperature and thus acting as a plasticizer. Cationic and silicone softeners offer the best finishing effects; however, cationic softeners suffer from poor resistance to yellowing and biotoxicity, while silicone softeners require the introduction of hydrophilic groups to improve their hydrophilicity. Anionic softeners have good hydrophilicity, but this also results in poor wash resistance.

[0004] In silicone softeners, compared to amino silicone oils, ternary block copolymer silicone oils not only exhibit superior anti-yellowing and stability, but also demonstrate significant advantages in improving smoothness, softness, and hydrophilicity, and have a noticeable effect on enhancing the durability and quality of textiles. However, in terms of production technology, ternary block copolymer silicone oils are much more complex than amino silicone oils. Furthermore, different raw material ratios, solvents, reaction temperatures, and reaction times all have a substantial impact on the performance of ternary block copolymer silicone oils. For example, Chinese invention patent CN 113652873 A discloses a method for preparing an organosilicon softener. It uses octamethylcyclotetrasiloxane as a monomer and methyldisiloxane as a capping agent to synthesize a hydrogen-terminated silicone oil. Next, it uses the hydrogen-terminated silicone oil and allyl glycidyl ether to undergo hydrosilylation under a platinum catalyst to synthesize an epoxy-terminated silicone oil. Finally, it utilizes the ring-opening addition reaction between the -NH2 group on the polyetheramine and the epoxy group on the epoxy silicone oil to synthesize a ternary block organosilicon softener. However, this method uses a high molecular weight hydrogen-terminated silicone oil to prepare a high molecular weight ternary copolymer block silicone oil. Therefore, the self-emulsifying, hydrophilic, and stable properties of this softener are insufficient to meet the requirements for giving fabrics a rich hand feel. Summary of the Invention

[0005] To address the aforementioned technical problems, this invention provides a method for preparing a cotton fabric softener with high fluffiness and a smooth touch. By compounding two silicone oils, the softener exhibits improved hydrophilicity, self-emulsification, and acid and alkali resistance. When applied to cotton fabrics, it enhances the hand feel, providing an ultra-soft, smooth, and fluffy texture, while also exhibiting good wash resistance.

[0006] The objective of this invention is achieved through the following technical solution: a method for preparing a cotton fabric softener with high fluffiness and a smooth touch, comprising the following steps: mixing silicone oil a, silicone oil b, and additives to obtain the softener; the raw materials of silicone oil a include terminal epoxy polyether silicone oil, polyether amine, solvent, and fatty acid; the raw materials of silicone oil b include terminal epoxy silicone oil, polyether amine, solvent, and fatty acid; the mass ratio of silicone oil a to silicone oil b is 60-90%:10-40%, and the total mass percentage is 100%.

[0007] This invention provides a fabric softener by compounding silicone oil a and silicone oil b. Silicone oil a and silicone oil b have different molecular structures, resulting in different molecular weights, hydrophilic effects, and emulsifying effects. However, they are both combinations of organosilicon and polyetheramine segments, leading to excellent compatibility and superior stability when compounded. Silicone oil a has low viscosity, facilitating penetration into cotton fibers and providing a soft hand feel, while silicone oil b has high viscosity, aiding adhesion to the cotton fabric surface and providing a smooth hand feel. Furthermore, the lower molecular weight of silicone oil a contributes to good hydrophilicity and self-emulsification, and its compounding with silicone oil b further promotes the emulsification of silicone oil b. This invention, through the adjustment of structure and molecular weight, provides a fabric softener with a rich hand feel, exhibiting both high fluffiness and a smooth touch.

[0008] Specifically, silicone oil a reacts with hydrogen-terminated silicone oil and allyl epoxy polyether. Allyl epoxy polyether is more suitable for reacting with hydrogen-terminated silicone oil with a smaller molecular weight, while hydrogen-terminated silicone oil with a larger molecular weight is difficult to react due to excessive steric hindrance. Furthermore, silicone oil a, obtained by controlling the molecular weights of both, exhibits an additional characteristic of a fluffy and delicate feel. Silicone oil b reacts with hydrogen-terminated silicone oil and allyl glycidyl ether. Allyl glycidyl ether has a smaller molecular weight, which is more conducive to reacting with hydrogen-terminated silicone oil with a larger molecular weight, resulting in a better fluffy feel. Secondly, silicone oil a uses a polyetheramine with a smaller molecular weight, while silicone oil b uses a polyetheramine with a larger molecular weight. The polyetheramine segments are used to modify the hydrophilicity of the organosilicon segments and are also beneficial for the adsorption between the softener and cotton fibers. This invention, by matching organosilicon segments with different molecular weights of polyetheramines, helps to maintain better hydrophilicity. Finally, fatty acids are added to adjust the pH, which simultaneously binds to amino groups, further improving the hydrophilic and emulsifying effects.

[0009] Preferably, the method for preparing the silicone oil a includes the following steps:

[0010] Step 1: Mix hydrogen-terminated silicone oil, allyl epoxy polyether and catalyst, add solvent, and react at 80-85℃ for 6-10 hours to obtain hydrogen-terminated epoxy polyether silicone oil.

[0011] Step 2: Stir and reflux the epoxy polyether silicone oil and polyether amine at 80-85°C for 6-10 hours, then add fatty acids and react for 1-2 hours to obtain silicone oil a.

[0012] Preferably, in step 1, the average molecular weight of the hydrogen-terminated silicone oil is 3000-8000 g / mol; the molar ratio of the hydrogen-terminated silicone oil to the allyl epoxy polyether is 1:(2.0-2.2); and the average molecular weight of the allyl epoxy polyether is 400-1000 g / mol.

[0013] Preferably, the allyl epoxy polyether is a mixture of ethylene oxide and propylene oxide polyether or pure ethylene oxide polyether, more preferably pure ethylene oxide polyether.

[0014] Preferably, in step 1, the solvent is one or more combinations of isopropanol, propylene glycol, ethylene glycol butyl ether, diethylene glycol butyl ether, dipropylene glycol methyl ether, and dipropylene glycol butyl ether; the amount of solvent used is 10-40% of the total mass of the hydrogen-terminated silicone oil, allyl glycidyl ether, and solvent.

[0015] Preferably, the catalyst is chloroplatinic acid, and its dosage is such that the platinum content is 1 to 10 ppm of the total mass of the hydrogen-terminated silicone oil and allyl epoxy polyether.

[0016] Preferably, in step 2, the polyetheramine is a linear double-terminated amino polyether with an average molecular weight of 200-900 g / mol, and the terminal amino group is a primary, secondary, or tertiary amine; the molar ratio of the terminal hydrogen-containing silicone oil to the polyetheramine is 1:(2.0-2.2); the fatty acid is decanoic acid, lauric acid, myristic acid, or malic acid; and the amount of the fatty acid used is 0.5-5% of the total mass of the terminal epoxy polyether silicone oil and the polyetheramine.

[0017] Preferably, the method for preparing the silicone oil b includes the following steps:

[0018] Step 3: After mixing the hydrogen-terminated silicone oil, allyl glycidyl ether and catalyst, react at 80-85℃ for 6-10 hours to obtain the terminal epoxy silicone oil.

[0019] Step 4: Stir and reflux the terminal epoxy silicone oil, polyetheramine and solvent at 80-85℃ for 8-10 hours, then add fatty acid and react for 1-2 hours to obtain silicone oil b.

[0020] Preferably, in step 3, the average molecular weight of the hydrogen-terminated silicone oil is 10,000 to 15,000 g / mol; and the molar ratio of the hydrogen-terminated silicone oil to allyl glycidyl ether is 1:(2.0 to 2.2).

[0021] When the molecular weight of the hydrogen-containing silicone oil is too small, the viscosity of silicone oil b is too low, which cannot provide a sufficient feel. When the viscosity is too high, the reaction becomes more difficult and the hydrophilicity deteriorates, making emulsification difficult.

[0022] Preferably, the catalyst is chloroplatinic acid, and its dosage is such that the platinum content is 1 to 10 ppm of the total mass of the hydrogen-terminated silicone oil and allyl glycidyl ether.

[0023] Preferably, in step 4, the polyetheramine is a linear double-terminated amino polyether with an average molecular weight of 900-2003 g / mol, and the terminal amino group is a primary amine, secondary amine, or tertiary amine, more preferably a tertiary amine; the molar ratio of the terminal hydrogen-containing silicone oil to the polyetheramine is 1:(2.0-2.2).

[0024] Because silicone oil b has a relatively large molecular weight, the combination of tertiary amine polyether amines with organosilicon segments is more conducive to improving hydrophilicity. After combining with subsequent fatty acids, the tertiary amine polyether forms a quaternary ammonium salt structure, which spontaneously forms micelles in water, with the hydrophilic groups facing the aqueous phase and the hydrophobic groups facing inward.

[0025] Preferably, in step 4, the amount of solvent used is 10-40% of the total mass of the terminal epoxy silicone oil, polyetheramine, and solvent; the solvent is one or a combination of isopropanol, propylene glycol, ethylene glycol butyl ether, diethylene glycol butyl ether, dipropylene glycol methyl ether, and dipropylene glycol butyl ether; the fatty acid is decanoic acid, lauric acid, myristic acid, or malic acid; and the amount of fatty acid used is 0.5-5% of the total mass of the terminal epoxy silicone oil and polyetheramine.

[0026] Since high molecular weight organosilicon segments and polyether segments have poor compatibility, the addition of solvents can improve the compatibility of the two segments and the controllability of the reaction.

[0027] Preferably, the additive is at least one of a dispersant, a mildew inhibitor, a defoamer, and a fragrance.

[0028] Compared with the prior art, the present invention has the following beneficial effects:

[0029] (1) In this invention, two different silicone oils are added to the compound silicone oil softener. Silicone oil a has a smaller molecular weight, which helps to penetrate deep into the cotton fibers and provide a soft hand feel to the fabric. Silicone oil b has a larger molecular weight, which adheres to the surface of the cotton fabric and provides a smooth hand feel to the fabric. The combination of the two makes the silicone oil softener have good self-emulsification, stability and hydrophilicity at the same time.

[0030] (2) Adding polyetheramine segments to modify the hydrophilicity of organosilicon segments also helps the adsorption between the softener and cotton fibers; adding fatty acids further improves the hydrophilicity and emulsification effects. Detailed Implementation

[0031] The technical solution of the present invention is illustrated below with specific embodiments, but the scope of protection of the present invention is not limited thereto:

[0032] Example 1

[0033] (1) Silicone oil a:

[0034] Step 1: Take 1 mol of hydrogen-terminated silicone oil with a molecular weight of 6000 g / mol, and mix it with 2 mol of allyl epoxy polyether with a molecular weight of 500 g / mol and chloroplatinic acid catalyst (platinum content is 5 ppm of the total mass of hydrogen-terminated silicone oil and allyl epoxy polyether) under nitrogen protection. Then add isopropanol (20% of the total mass of hydrogen-terminated silicone oil, allyl epoxy polyether and isopropanol) and react at 80℃ for 8 h to obtain end-epoxy polyether silicone oil.

[0035] Step 2: React the terminal epoxy polyether silicone oil with 2 mol of polyether amine EA600 (tertiary amine structure) under stirring and reflux at 80°C for 8 hours. Add lauric acid (2% of the total mass of terminal epoxy polyether silicone oil and polyether amine EA600) and react for 1 hour to obtain silicone oil a.

[0036] (2) Silicone oil b:

[0037] Step 3: Take 1 mol of hydrogen-terminated silicone oil with a molecular weight of 13000 g / mol, mix it with 2 mol of allyl glycidyl ether and chloroplatinic acid catalyst (platinum content is 7 ppm of the total mass of hydrogen-terminated silicone oil and allyl glycidyl ether) under nitrogen protection, and react at 80℃ for 6 h to obtain epoxy silicone oil.

[0038] Step 4: The terminal epoxy silicone oil is reacted with 2 mol of polyetheramine ED900 (primary amine structure) and isopropanol (40% of the total mass of terminal epoxy silicone oil, polyetheramine ED900 and isopropanol) under stirring and reflux at 80°C for 8 hours. Lauric acid (3% of the total mass of terminal epoxy silicone oil and polyetheramine EA900) is added and reacted for 1 hour to obtain silicone oil b.

[0039] (3) Take silicone oil a and silicone oil b in a mass ratio of 8:2, then add 0.05% of the total mass of defoamer (water-based organosilicon defoamer) and mix evenly to obtain a compound silicone oil softener.

[0040] Example 2

[0041] The only difference from Example 1 is that the mixing ratio of silicone oil a to silicone oil b is 6:4.

[0042] Mix silicone oil a and silicone oil b in a mass ratio of 6:4, then add 0.05% of the total mass of defoamer (water-based silicone defoamer) and mix evenly to obtain a compounded silicone oil softener.

[0043] Example 3

[0044] The only difference from Example 1 is that the hydrogen-terminated silicone oil used in silicone oil a has an average molecular weight of 8000 g / mol.

[0045] (1) Silicone oil a:

[0046] Step 1: Take 1 mol of hydrogen-terminated silicone oil with a molecular weight of 8000 g / mol, and mix it with 2 mol of allyl epoxy polyether with a molecular weight of 500 g / mol and chloroplatinic acid catalyst (platinum content is 5 ppm of the total mass of hydrogen-terminated silicone oil and allyl epoxy polyether) under nitrogen protection. Then add isopropanol (20% of the total mass of hydrogen-terminated silicone oil, allyl epoxy polyether and isopropanol) and react at 80℃ for 8 h to obtain end-epoxy polyether silicone oil.

[0047] Step 2: React the terminal epoxy polyether silicone oil with 2 mol of polyether amine EA600 (tertiary amine structure) under stirring and reflux at 80°C for 8 hours. Add lauric acid (2% of the total mass of terminal epoxy polyether silicone oil and polyether amine EA600) and react for 1 hour to obtain silicone oil a.

[0048] (2) Silicone oil b:

[0049] Step 3: Take 1 mol of hydrogen-terminated silicone oil with a molecular weight of 13000 g / mol, mix it with 2 mol of allyl glycidyl ether and chloroplatinic acid catalyst (platinum content is 7 ppm of the total mass of hydrogen-terminated silicone oil and allyl glycidyl ether) under nitrogen protection, and react at 80℃ for 6 h to obtain epoxy silicone oil.

[0050] Step 4: The terminal epoxy silicone oil is reacted with 2 mol of polyetheramine ED900 (primary amine structure) and isopropanol (40% of the total mass of terminal epoxy silicone oil, polyetheramine ED900 and isopropanol) under stirring and reflux at 80°C for 8 hours. Lauric acid (3% of the total mass of terminal epoxy silicone oil and polyetheramine EA900) is added and reacted for 1 hour to obtain silicone oil b.

[0051] (3) Take silicone oil a and silicone oil b in a mass ratio of 8:2, then add 0.05% of the total mass of defoamer (water-based organosilicon defoamer) and mix evenly to obtain a compound silicone oil softener.

[0052] Example 4

[0053] The only difference from Example 1 is that the hydrogen-terminated silicone oil used in silicone oil b has an average molecular weight of 10,000 g / mol.

[0054] (1) Silicone oil a:

[0055] Step 1: Take 1 mol of hydrogen-terminated silicone oil with a molecular weight of 6000 g / mol, and mix it with 2 mol of allyl epoxy polyether with a molecular weight of 500 g / mol and chloroplatinic acid catalyst (platinum content is 5 ppm of the total mass of hydrogen-terminated silicone oil and allyl epoxy polyether) under nitrogen protection. Then add isopropanol (20% of the total mass of hydrogen-terminated silicone oil, allyl epoxy polyether and isopropanol) and react at 80℃ for 8 h to obtain end-epoxy polyether silicone oil.

[0056] Step 2: React the terminal epoxy polyether silicone oil with 2 mol of polyether amine EA600 (tertiary amine structure) under stirring and reflux at 80°C for 8 hours. Add lauric acid (2% of the total mass of terminal epoxy polyether silicone oil and polyether amine EA600) and react for 1 hour to obtain silicone oil a.

[0057] (2) Silicone oil b:

[0058] Step 3: Take 1 mol of hydrogen-terminated silicone oil with a molecular weight of 10000 g / mol, mix it with 2 mol of allyl glycidyl ether and chloroplatinic acid catalyst (platinum content is 7 ppm of the total mass of hydrogen-terminated silicone oil and allyl glycidyl ether) under nitrogen protection, and react at 80℃ for 6 h to obtain epoxy silicone oil.

[0059] Step 4: The terminal epoxy silicone oil is reacted with 2 mol of polyetheramine ED900 (primary amine structure) and isopropanol (40% of the total mass of terminal epoxy silicone oil, polyetheramine ED900 and isopropanol) under stirring and reflux at 80°C for 8 hours. Lauric acid (3% of the total mass of terminal epoxy silicone oil and polyetheramine EA900) is added and reacted for 1 hour to obtain silicone oil b.

[0060] (3) Take silicone oil a and silicone oil b in a mass ratio of 8:2, then add 0.05% of the total mass of defoamer (water-based organosilicon defoamer) and mix evenly to obtain a compound silicone oil softener.

[0061] Example 5

[0062] The only difference from Example 1 is that the polyetheramine used in silicone oil a is ED600 (primary amine structure).

[0063] (1) Silicone oil a:

[0064] Step 1: Take 1 mol of hydrogen-terminated silicone oil with a molecular weight of 6000 g / mol, and mix it with 2 mol of allyl epoxy polyether with a molecular weight of 500 g / mol and chloroplatinic acid catalyst (platinum content is 5 ppm of the total mass of hydrogen-terminated silicone oil and allyl epoxy polyether) under nitrogen protection. Then add isopropanol (20% of the total mass of hydrogen-terminated silicone oil, allyl epoxy polyether and isopropanol) and react at 80℃ for 8 h to obtain end-epoxy polyether silicone oil.

[0065] Step 2: React the terminal epoxy polyether silicone oil with 2 mol of polyether amine ED600 (primary amine structure) under stirring and reflux at 80°C for 8 hours. Add lauric acid (2% of the total mass of terminal epoxy polyether silicone oil and polyether amine EA600) and react for 1 hour to obtain silicone oil a.

[0066] (2) Silicone oil b:

[0067] Step 3: Take 1 mol of hydrogen-terminated silicone oil with a molecular weight of 13000 g / mol, mix it with 2 mol of allyl glycidyl ether and chloroplatinic acid catalyst (platinum content is 7 ppm of the total mass of hydrogen-terminated silicone oil and allyl glycidyl ether) under nitrogen protection, and react at 80℃ for 6 h to obtain epoxy silicone oil.

[0068] Step 4: The terminal epoxy silicone oil is reacted with 2 mol of polyetheramine ED900 (primary amine structure) and isopropanol (40% of the total mass of terminal epoxy silicone oil, polyetheramine ED900 and isopropanol) under stirring and reflux at 80°C for 8 hours. Lauric acid (3% of the total mass of terminal epoxy silicone oil and polyetheramine EA900) is added and reacted for 1 hour to obtain silicone oil b.

[0069] (3) Take silicone oil a and silicone oil b in a mass ratio of 8:2, then add 0.05% of the total mass of defoamer (water-based organosilicon defoamer) and mix evenly to obtain a compound silicone oil softener.

[0070] Example 6

[0071] The only difference from Example 1 is that the amount of isopropanol used in silicone oils a and b is 30% of the total mass.

[0072] (1) Silicone oil a:

[0073] Step 1: Take 1 mol of hydrogen-terminated silicone oil with a molecular weight of 6000 g / mol, and mix it with 2 mol of allyl epoxy polyether with a molecular weight of 500 g / mol and chloroplatinic acid catalyst (platinum content is 5 ppm of the total mass of hydrogen-terminated silicone oil and allyl epoxy polyether) under nitrogen protection. Then add isopropanol (30% of the total mass of hydrogen-terminated silicone oil, allyl epoxy polyether and isopropanol) and react at 80℃ for 8 h to obtain end-epoxy polyether silicone oil.

[0074] Step 2: React the terminal epoxy polyether silicone oil with 2 mol of polyether amine EA600 (tertiary amine structure) under stirring and reflux at 80°C for 8 hours. Add lauric acid (2% of the total mass of terminal epoxy polyether silicone oil and polyether amine EA600) and react for 1 hour to obtain silicone oil a.

[0075] (2) Silicone oil b:

[0076] Step 3: Take 1 mol of hydrogen-terminated silicone oil with a molecular weight of 13000 g / mol, mix it with 2 mol of allyl glycidyl ether and chloroplatinic acid catalyst (platinum content is 7 ppm of the total mass of hydrogen-terminated silicone oil and allyl glycidyl ether) under nitrogen protection, and react at 80℃ for 6 h to obtain epoxy silicone oil.

[0077] Step 4: The terminal epoxy silicone oil is reacted with 2 mol of polyetheramine ED900 (primary amine structure) and isopropanol (30% of the total mass of terminal epoxy silicone oil, polyetheramine ED900 and isopropanol) under stirring and reflux at 80°C for 8 hours. Lauric acid (3% of the total mass of terminal epoxy silicone oil and polyetheramine EA900) is added and reacted for 1 hour to obtain silicone oil b.

[0078] (3) Take silicone oil a and silicone oil b in a mass ratio of 8:2, then add 0.05% of the total mass of defoamer (water-based organosilicon defoamer) and mix evenly to obtain a compound silicone oil softener.

[0079] Example 7

[0080] The only difference from Example 1 is that the solvent used in silicone oils a and b is diethylene glycol butyl ether.

[0081] (1) Silicone oil a:

[0082] Step 1: Take 1 mol of hydrogen-terminated silicone oil with a molecular weight of 6000 g / mol, and mix it with 2 mol of allyl epoxy polyether with a molecular weight of 500 g / mol and chloroplatinic acid catalyst (platinum content is 5 ppm of the total mass of hydrogen-terminated silicone oil and allyl epoxy polyether) under nitrogen protection. Then add diethylene glycol butyl ether (20% of the total mass of hydrogen-terminated silicone oil, allyl epoxy polyether and diethylene glycol butyl ether) and react at 80℃ for 8 h to obtain end-epoxy polyether silicone oil.

[0083] Step 2: React the terminal epoxy polyether silicone oil with 2 mol of polyether amine EA600 (tertiary amine structure) under stirring and reflux at 80°C for 8 hours. Add lauric acid (2% of the total mass of terminal epoxy polyether silicone oil and polyether amine EA600) and react for 1 hour to obtain silicone oil a.

[0084] (2) Silicone oil b:

[0085] Step 3: Take 1 mol of hydrogen-terminated silicone oil with a molecular weight of 13000 g / mol, mix it with 2 mol of allyl glycidyl ether and chloroplatinic acid catalyst (platinum content is 7 ppm of the total mass of hydrogen-terminated silicone oil and allyl glycidyl ether) under nitrogen protection, and react at 80℃ for 6 h to obtain epoxy silicone oil.

[0086] Step 4: The terminal epoxy silicone oil is reacted with 2 mol of polyetheramine ED900 (primary amine structure) and diethylene glycol butyl ether (40% of the total mass of terminal epoxy silicone oil, polyetheramine ED900 and diethylene glycol butyl ether) under stirring and reflux at 80°C for 8 hours. Lauric acid (3% of the total mass of terminal epoxy silicone oil and polyetheramine EA900) is added and reacted for 1 hour to obtain silicone oil b.

[0087] (3) Take silicone oil a and silicone oil b in a mass ratio of 8:2, then add 0.05% of the total mass of defoamer (water-based organosilicon defoamer) and mix evenly to obtain a compound silicone oil softener.

[0088] Comparative Example 1

[0089] The only difference from Example 1 is that it does not contain silicone oil a.

[0090] (1) Silicone oil b:

[0091] Step 3: Take 1 mol of hydrogen-terminated silicone oil with a molecular weight of 13000 g / mol, mix it with 2 mol of allyl glycidyl ether and chloroplatinic acid catalyst (platinum content is 7 ppm of the total mass of hydrogen-terminated silicone oil and allyl glycidyl ether) under nitrogen protection, and react at 80℃ for 6 h to obtain epoxy silicone oil.

[0092] Step 4: The terminal epoxy silicone oil is reacted with 2 mol of polyetheramine ED900 (primary amine structure) and isopropanol (40% of the total mass of terminal epoxy silicone oil, polyetheramine ED900 and isopropanol) under stirring and reflux at 80°C for 8 hours. Lauric acid (3% of the total mass of terminal epoxy silicone oil and polyetheramine EA900) is added and reacted for 1 hour to obtain silicone oil b.

[0093] (2) Take silicone oil b, add 0.05% of defoamer (water-based silicone defoamer) by total mass and mix evenly to obtain compound silicone oil softener.

[0094] Comparative Example 2

[0095] The only difference from Example 1 is that it does not contain silicone oil b.

[0096] (1) Silicone oil a:

[0097] Step 1: Take 1 mol of hydrogen-terminated silicone oil with a molecular weight of 6000 g / mol, and mix it with 2 mol of allyl epoxy polyether with a molecular weight of 500 g / mol and chloroplatinic acid catalyst (platinum content is 5 ppm of the total mass of hydrogen-terminated silicone oil and allyl epoxy polyether) under nitrogen protection. Then add isopropanol (20% of the total mass of hydrogen-terminated silicone oil, allyl epoxy polyether and isopropanol) and react at 80℃ for 8 h to obtain end-epoxy polyether silicone oil.

[0098] Step 2: React the terminal epoxy polyether silicone oil with 2 mol of polyether amine EA600 (tertiary amine structure) under stirring and reflux at 80°C for 8 hours. Add lauric acid (2% of the total mass of terminal epoxy polyether silicone oil and polyether amine EA600) and react for 1 hour to obtain silicone oil a.

[0099] (2) Take silicone oil a, and add 0.05% of the total mass of defoamer (water-based silicone defoamer) and mix evenly to obtain the compounded silicone oil softener.

[0100] Comparative Example 3

[0101] The only difference from Example 1 is that the mixing ratio of silicone oil a to silicone oil b is 2:8.

[0102] Mix silicone oil a and silicone oil b in a mass ratio of 2:8, then add 0.05% of the total mass of defoamer (water-based silicone defoamer) and mix evenly to obtain a compounded silicone oil softener.

[0103] The compound silicone oil softeners obtained in the examples and comparative examples were all emulsified with acetic acid (1% by weight of softener) and emulsifier AEO-3 (5% by weight of softener) to obtain emulsions containing 2 wt% compound silicone oil softener. The emulsions were then used to treat unprocessed cotton fabric samples. The blank samples were unprocessed cotton fabric samples. The following performance tests were then performed.

[0104] (1) Appearance of emulsion: used to characterize the state of emulsion. "Transparent" indicates that the emulsion has good uniformity and high transparency, while "with blue light" indicates that the emulsion has small particle size and good hydrophilicity.

[0105] (2) Hydrophilicity: Measured according to AATCC79 Absorption Test for Bleached Fabrics, expressed as water absorption and diffusion time.

[0106] (3) Hand feel: A team of 5 professionals will evaluate the hand feel of the fabric. The hand feel assessment is based on two aspects: softness and smoothness, and is divided into 5 levels. The higher the level, the better the hand feel.

[0107] (4) Softness: Measured using a computer-controlled softness meter. Fabric samples of the same size were treated with a softener and dried before being placed in the softness meter for testing. When the plate-shaped probe pressed the sample into the seam to a certain depth, the maximum vector sum of the sample's own bending resistance and the frictional force between the sample and the seam is called the softness, expressed in millinewtons. The smaller the softness value, the softer the sample. The samples were tested in both the transverse and longitudinal directions. The overall result was calculated by summing the percentage reduction compared to the measured value of the untreated fabric sample (blank sample). The larger the value, the better the softening effect.

[0108] Table 1

[0109] Sample Emulsion Appearance hydrophilicity / s feel / grade blank sample -- 0.6 1 Example 1 Transparent, with a blue glow 2.6 5 Example 2 Transparent, with a blue glow 2.9 5 Example 3 Transparent, with a blue glow 3.0 5 Example 4 Transparent, with a blue glow 2.8 5 Example 5 Slightly cloudy, with a bluish tint 3.4 4 Example 6 Transparent, with a blue glow 3.2 4 Example 7 Slightly cloudy, with a bluish tint 3.3 4 Comparative Example 1 Slightly white with a hint of blue light 3.7 3 Comparative Example 2 Slightly cloudy, with a little blue light 3.6 3 Comparative Example 3 Transparent, with a slight blue glow 3.2 3

[0110] Table 2

[0111]

[0112] As shown in Tables 1-2, the softener synthesized by the preparation method of the present invention exhibits excellent hand feel when applied to cotton fabric, significantly improves the hydrophilicity of the fabric sample, and at the same time makes the fabric sample exhibit a variety of rich hand feel such as softness, fluffiness, and smoothness.

[0113] A comparison of Examples 1 and 5 shows that the hydrophilic effect is better when the polyetheramine used is a tertiary amine. A comparison of Example 1 and Comparative Examples 1-2 shows that when only one type of silicone oil is used as the softener, the synergistic effect of molecules of different sizes is not fully utilized, resulting in a less uniform hand feel. A comparison of Examples 1-2 and Comparative Example 3 shows that reducing the proportion of silicone oil a significantly decreases the hydrophilic effect and reduces the softness of the fabric sample.

[0114] The above are merely preferred embodiments of the present invention and do not limit the patent scope of the present invention. Any equivalent structural or procedural transformations made using the present invention specification, or direct or indirect applications in other related technical fields, are similarly included within the patent protection scope of the present invention.

Claims

1. A method for preparing a fabric softener for cotton fabrics with high fluffiness and a smooth touch, characterized in that, Includes the following steps: Step 1: Mix hydrogen-terminated silicone oil with an average molecular weight of 3000~8000 g / mol, allyl epoxy polyether with an average molecular weight of 400~1000 g / mol, and catalyst, add solvent, and react at 80~85℃ for 6~10h to obtain end-epoxy polyether silicone oil. Step 2: Stir and reflux the epoxy polyether silicone oil and polyether amine at 80~85℃ for 6~10h, then add fatty acids and react for 1~2h to obtain silicone oil a; Step 3: After mixing hydrogen-terminated silicone oil with an average molecular weight of 10,000~15,000 g / mol, allyl glycidyl ether and catalyst, react at 80~85℃ for 6~10h to obtain terminal epoxy silicone oil. Step 4: Stir and reflux the epoxy silicone oil, polyetheramine and solvent at 80~85℃ for 8~10h, then add fatty acid and react for 1~2h to obtain silicone oil b; The softener is obtained by mixing silicone oil a, silicone oil b and additives, with the mass ratio of silicone oil a to silicone oil b being 60~90%: 10~40% and the total mass percentage being 100%.

2. The method for preparing a cotton fabric softener with high fluffiness and a smooth feel as described in claim 1, characterized in that, In step 1, the average molecular weight of the allyl epoxy polyether is 500 g / mol.

3. The method for preparing a cotton fabric softener with high fluffiness and a smooth feel as described in claim 1, characterized in that, In step 1, the molar ratio of the hydrogen-terminated silicone oil and the allyl epoxy polyether is 1:(2.0~2.2).

4. The method for preparing a cotton fabric softener with high fluffiness and smooth touch as described in claim 1 or 3, characterized in that, In step 1, the solvent is one or a combination of isopropanol, propylene glycol, ethylene glycol butyl ether, diethylene glycol butyl ether, dipropylene glycol methyl ether, and dipropylene glycol butyl ether; the amount of solvent used is 10-40% of the total mass of hydrogen-terminated silicone oil, allyl glycidyl ether, and solvent.

5. The method for preparing a cotton fabric softener with high fluffiness and a smooth feel as described in claim 1, characterized in that, In step 2, the polyetheramine is a linear double-terminated amino polyether with an average molecular weight of 200-900 g / mol; the molar ratio of the terminal hydrogen-containing silicone oil to the polyetheramine is 1:(2.0-2.2); the fatty acid is decanoic acid, lauric acid, myristic acid, or malic acid; the amount of the fatty acid used is 0.5-5% of the total mass of the terminal epoxy polyether silicone oil and the polyetheramine.

6. The method for preparing a cotton fabric softener with high fluffiness and smooth touch as described in claim 1, characterized in that, In step 3, the molar ratio of the end-hydrogenated silicone oil and allyl glycidyl ether is 1:(2.0~2.2).

7. The method for preparing a cotton fabric softener with high fluffiness and a smooth feel as described in claim 1, characterized in that, In step 4, the polyetheramine is a linear double-terminated amino polyether with an average molecular weight of 900~2003 g / mol; the molar ratio of the end-hydrogen silicone oil to the polyetheramine is 1:(2.0~2.2).

8. The method for preparing a cotton fabric softener with high fluffiness and smooth touch as described in claim 1, 6, or 7, characterized in that, In step 4, the amount of solvent used is 10-40% of the total mass of the terminal epoxy silicone oil, polyetheramine, and solvent; the solvent is one or a combination of isopropanol, propylene glycol, ethylene glycol butyl ether, diethylene glycol butyl ether, dipropylene glycol methyl ether, and dipropylene glycol butyl ether; the fatty acid is decanoic acid, lauric acid, myristic acid, or malic acid; and the amount of fatty acid used is 0.5-5% of the total mass of the terminal epoxy silicone oil and polyetheramine.

9. The method for preparing a cotton fabric softener with high fluffiness and smooth touch as described in claim 1, characterized in that, The additive is at least one of dispersant, mildew inhibitor, defoamer and fragrance.

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