A phenol-free, yellowing, fluffy, cotton-feeling softener and its preparation method

Abstract

The present invention belongs to the field of textile dyeing and finishing technology, and specifically relates to a softener with a fluffy, cotton-like feel without phenol yellowing and a preparation method thereof. The softener comprises the following components, measured by percentage: 8-12% tetramethyldisiloxane, 10-15% cyclohexylmethyldimethoxysilane, 3-6% polyetheramine, 8-12% allyl glycidyl ether, 10-15% isopropyl alcohol, 10-15% diethylene glycol butyl ether, 2-4% alkylbenzenesulfonate amine, 2-4% surfactant, 0.2-0.4% pH regulator, and 0.1-0.2% antibacterial agent. The softener prepared by the present invention can impart an excellent soft, fluffy, and smooth feel to fabrics, has substantially no effect on phenol yellowing of the fabrics, has excellent hydrophilic effect and wash resistance of the fabrics after treatment, does not affect the color shade and fastness of the dyed fabrics, and has excellent compatibility with general textile auxiliaries, excellent stability, and is fully usable.

Description

Technical Field

[0001] The invention belongs to the technical field of textile dyeing and finishing, and particularly relates to a phenol-free, yellowing, fluffy, cotton-feeling softener and a preparation method thereof. Background Art

[0002] Textiles such as yarns, fabrics, ribbons, and clothing require packaging using materials such as polyethylene film during storage and distribution. During the polyethylene production process, the hindered phenolic antioxidant BHT (2,6-di-tert-butyl-p-cresol) is added. At room temperature, BHT reacts chemically with nitrogen oxides (NOx) absorbed or stored in air and packaging materials (such as cardboard) to produce yellow DTNP (2,6-di-tert-butyl-p-nitrophenol). When the polyethylene packaging film comes into direct contact with the textile, the DTNP sublimates and transfers to the fabric surface, causing yellowing. This yellowing of fabrics caused by phenols in the packaging material is known in the textile industry as "phenolic yellowing." Generally speaking, phenolic yellowing is particularly severe in fabrics such as nylon and spandex, which contain amino groups in their fiber molecular structure. Although polyester and cotton fabrics are not prone to yellowing during storage, they have an unpleasant feel, and softeners are often added during printing and dyeing to improve their feel. Silicone oils and soft film softeners with a good hand feel also have an amino structure, especially amino silicone oils and cationic soft films with strong cationic properties, which are prone to phenol yellowing. Therefore, cotton and polyester fabrics that have been softened are also prone to phenol yellowing.

[0003] Guangdong Demei Fine Chemicals uses heat-resistant yellowing agent DM-2915 and anti-phenol yellowing agent DM-2903, and performs pre-setting and post-setting treatments to obtain yellowing-resistant fabrics; Zhongfang Chemical uses foam-free anti-phenol yellowing agent FK-162LF and antioxidant FK-161D that does not contain adipic acid diamide (ADH), and solves the yellowing problem of nylon-spandex fabrics during high-temperature molding and storage through exhaustion anti-phenol process and post-setting heat-resistant process. However, in the above processes, the anti-phenol and heat-resistant processes are carried out separately, which increases the costs in many aspects such as energy, time and labor. Chinese invention patent CN115928428A discloses an auxiliary agent for resisting high-temperature yellowing and phenolic yellowing of textiles, a preparation method and its application. The auxiliary agent is composed of an anti-high-temperature yellowing agent and an anti-phenolic yellowing agent. The amount of the anti-high-temperature yellowing agent is 40-100g / L, the amount of the anti-phenolic yellowing agent is 40-100g / L, and the application pH value is 4-6; the anti-high-temperature yellowing agent includes 10% to 30% antioxidant, 5% to 20% cosolvent, 0% to 10% emulsifier and water; the anti-phenolic yellowing agent includes 10% to 30% anti-phenolic yellowing agent, 5% to 15% pH adjuster and water. However, this invention only involves the application of specific products to solve the yellowing problem of nylon and its blended fabrics, and its scope of application is relatively limited.

[0004] There are many popular softeners on the market, each with its own unique feel. However, while ensuring excellent feel, most products have the following two problems: (1) the fabric will be severely phenolic yellowed after treatment, which greatly reduces the service life and sales price of the final garment; (2) the product stability is poor, which increases the risk of process production and is prone to problems such as sticking to rollers, sticking to cylinders, oil drifting, and demulsification. It is necessary to provide a new, highly safe, phenolic yellowing-free, fluffy, and cotton-feeling softener that can give fabrics a soft, fluffy, and strong cotton-feel feel and has little effect on phenolic yellowing of the fabric. Summary of the Invention

[0005] In view of the problems existing in the prior art, the present invention provides a phenol-free, yellowing, fluffy, cotton-feeling softener and a preparation method thereof.

[0006] To achieve the above object, the technical solution adopted by the present invention is as follows:

[0007] A softener comprises the following components: tetramethyldisiloxane, cyclohexylmethyldimethoxysilane, polyetheramine, allyl glycidyl ether, isopropyl alcohol, diethylene glycol butyl ether, alkylbenzenesulfonic acid amine, a surfactant, a pH regulator and an antibacterial agent.

[0008] A softener comprises the following components, calculated by percentage: 8-12% of tetramethyldisiloxane, 10-15% of cyclohexylmethyldimethoxysilane, 3-6% of polyetheramine, 8-12% of allyl glycidyl ether, 10-15% of isopropyl alcohol, 10-15% of diethylene glycol butyl ether, 2-4% of alkylbenzenesulfonate amine, 2-4% of surfactant, 0.2-0.4% of pH regulator and 0.1-0.2% of antibacterial agent.

[0009] Preferably, the molecular weight of the polyetheramine is 200-400, the alkylbenzenesulfonate amine is triethanolamine dodecylbenzenesulfonate, the surfactant includes an anionic surfactant and a nonionic surfactant, the pH regulator is glacial acetic acid, and the antibacterial agent is selected from one or more of inorganic antibacterial agents, organic antibacterial agents and natural antibacterial agents.

[0010] Preferably, the anionic surfactant is selected from sodium lauryl sulfate (SDS) or sodium of higher fatty acids, the nonionic surfactant is a polyoxyethylene ether surfactant, and the antibacterial agent is an organic antibacterial agent.

[0011] Preferably, the polyoxyethylene ether surfactant is fatty alcohol polyoxyethylene ether.

[0012] Preferably, the softener further comprises water.

[0013] The present invention also provides a method for preparing the above-mentioned softener, comprising the following steps:

[0014] (1) reacting tetramethyldisiloxane and cyclohexylmethyldimethoxysilane to obtain aminosilicone oil;

[0015] (2) reacting amino silicone oil with isopropyl alcohol, allyl glycidyl ether, diethylene glycol butyl ether and polyetheramine, and then adding alkylbenzene sulfonate amine to react to obtain modified amino silicone oil;

[0016] (3) reacting the modified amino silicone oil with a surfactant, adding a pH regulator, an antibacterial agent and water, and stirring to obtain the product.

[0017] Preferably, in step (1), the temperature needs to be raised before the reaction, and a catalyst, solvent and end-capping agent need to be added. After the reaction, the temperature needs to be lowered and distilled under reduced pressure.

[0018] Preferably, the heating temperature is 90-120° C., and the heating time is 5-9 hours.

[0019] Preferably, the catalyst is tetramethylammonium hydroxide, the solvent is dimethyl sulfoxide or isopropyl alcohol, and the capping agent is hexamethyldisiloxane.

[0020] Preferably, the mass ratio of tetramethyldisiloxane, cyclohexylmethyldimethoxysilane, solvent and end-capping agent is 3:3-4:2-3, and the amount of the catalyst is 0.5-2% of the total amount of tetramethyldisiloxane, cyclohexylmethyldimethoxysilane and end-capping agent.

[0021] Preferably, the reaction in step (1) is carried out in a sealed device comprising a condenser, a separatory funnel, a thermometer and a nitrogen protection device, the reaction temperature is 70-100° C., and the reaction time is 1-2 h.

[0022] Preferably, the heating temperature is 135-145°C.

[0023] Preferably, in step (2), the mass ratio of amino silicone oil, isopropyl alcohol, allyl glycidyl ether, diethylene glycol butyl ether, polyetheramine and alkylbenzenesulfonic acid amine is 10-30:4-5:2-3:2-3:1-3:1, the reaction temperature is 45-80° C., and the reaction time is 3-6 h.

[0024] Preferably, in step (3), the mass ratio of the modified amino silicone oil to the surfactant is 10-30:1, the stirring speed is 2500-3000 rpm, and the stirring time is 20-30 min.

[0025] The present invention also provides application of the softening agent in softening and finishing fabrics.

[0026] Compared with the prior art, the present invention has the following beneficial effects:

[0027] (1) The softener prepared by the present invention can give the fabric an excellent soft, fluffy and smooth feel, among which the soft, fluffy and thick feel is particularly prominent; it has basically no effect on the phenol yellow of the fabric, and is particularly suitable for use on white and light-colored fabrics; the treated fabric has an excellent hydrophilic effect; it has excellent wash resistance and can still maintain a good feel after multiple washings.

[0028] (2) The softener prepared by the present invention has excellent compatibility with general textile auxiliaries, such as cationic softeners, and will not affect the color and fastness of dyed fabrics. It also has excellent stability and can be used completely. DETAILED DESCRIPTION

[0029] The remaining raw materials used in the present invention are all common commercially available products.

[0030] Example 1

[0031] A softener is composed of the following components, calculated by percentage: 12% tetramethyldisiloxane, 15% cyclohexylmethyldimethoxysilane, 8% allyl glycidyl ether, 3% polyetheramine, 15% isopropyl alcohol, 10% diethylene glycol butyl ether, 4% triethanolamine dodecylbenzenesulfonate, 2% sodium lauryl sulfate (SDS), 2% fatty alcohol polyoxyethylene ether, 0.2% glacial acetic acid, 0.1% organic antibacterial agent, and the balance being water.

[0032] The preparation method is as follows:

[0033] (1) Tetramethyldisiloxane and cyclohexylmethyldimethoxysilane were sequentially added to a four-necked flask equipped with a condenser, a separating funnel, a thermometer, and a nitrogen protection device. The device was sealed, nitrogen was introduced, and the temperature was raised to 70°C. After keeping the temperature for 2 hours, the catalyst tetramethylammonium hydroxide and the solvent dimethyl sulfoxide (DMSO) were added. After stirring and heating to 90°C for 8 hours, the end-capping agent hexamethyldisiloxane was added and the reaction was continued for 1 hour. The mass ratio of tetramethyldisiloxane, cyclohexylmethyldimethoxysilane, solvent, and end-capping agent was 3:3:2, and the amount of catalyst was 0.5% of the total amount of tetramethyldisiloxane, end-capping agent, and cyclohexylmethyldimethoxysilane. The catalyst tetramethylammonium hydroxide was heated to 135°C to decompose under high temperature. After cooling, the low-boiling-point substances were removed by vacuum distillation to obtain amino silicone oil.

[0034] (2) Isopropyl alcohol, allyl glycidyl ether, diethylene glycol butyl ether, and polyetheramine were mixed and then dropped into a three-necked flask containing amino silicone oil, wherein the mass ratio of amino silicone oil to polyetheramine was 20:3. Nitrogen was used for protection, and the temperature was raised to 80°C with stirring. The reaction time was 3 hours. Triethanolamine dodecylbenzenesulfonate was added, and the reaction was continued with stirring for 5 hours. The reaction temperature was 50°C. After cooling, the low-boiling-point substances were removed by reduced pressure distillation to obtain modified amino silicone oil.

[0035] (3) SDS and fatty alcohol polyoxyethylene ether are mixed and stirred evenly, and modified amino silicone oil is added, wherein the mass ratio of fatty alcohol polyoxyethylene ether to modified amino silicone oil is 1:10, and stirred at a speed of 100 r / min for 10 minutes, and then the speed is increased to 1000 r / min, and a mixture of water and glacial acetic acid is slowly added dropwise in multiple times within 30 minutes. When all the water has been dripped, an organic antibacterial agent is added, and the speed is increased to 2500 r / min and stirring is continued for 30 minutes to obtain a softener.

[0036] Example 2

[0037] A softener is composed of the following components, calculated by percentage: 8% tetramethyldisiloxane, 10% cyclohexylmethyldimethoxysilane, 12% allyl glycidyl ether, 6% polyetheramine, 10% isopropyl alcohol, 15% diethylene glycol butyl ether, 2% triethanolamine dodecylbenzenesulfonate, 3% sodium of higher fatty acids, 3% fatty alcohol polyoxyethylene ether, 0.4% glacial acetic acid, 0.2% organic antibacterial agent, and the balance being water.

[0038] The preparation method is as follows:

[0039] (1) Tetramethyldisiloxane and cyclohexylmethyldimethoxysilane were sequentially added to a four-necked flask equipped with a condenser, a separatory funnel, a thermometer, and a nitrogen protection device. The device was sealed, nitrogen was introduced, and the temperature was raised to 100°C. After keeping the temperature for 1 hour, the catalyst tetramethylammonium hydroxide and the solvent isopropyl alcohol were added. After stirring and heating to 110°C for 5 hours, the end-capping agent hexamethyldisiloxane was added and the reaction was continued for 1.5 hours. The mass ratio of tetramethyldisiloxane, cyclohexylmethyldimethoxysilane, solvent, and end-capping agent was 3:4:3, and the amount of catalyst was 2% of the total amount of tetramethyldisiloxane, cyclohexylmethyldimethoxysilane, and end-capping agent. The catalyst tetramethylammonium hydroxide was heated to 145°C to decompose under high temperature. After cooling, the low-boiling-point substances were removed by vacuum distillation to obtain amino silicone oil.

[0040] (2) Isopropyl alcohol, allyl glycidyl ether, diethylene glycol butyl ether, and polyetheramine were mixed and then added dropwise to a three-necked flask containing amino silicone oil, wherein the mass ratio of amino silicone oil to polyetheramine was 10:3. Under nitrogen protection, the temperature was raised to 45°C with stirring, and the reaction time was 6 hours. Dodecylbenzenesulfonic acid triethanolamine was added, and the reaction was continued with stirring for 4 hours at 60°C. After cooling, the low-boiling-point substances were removed by vacuum distillation to obtain modified amino silicone oil.

[0041] (3) Sodium fatty acid and fatty alcohol polyoxyethylene ether are mixed and stirred evenly, and modified amino silicone oil is added, wherein the mass ratio of fatty alcohol polyoxyethylene ether to modified amino silicone oil is 1:30, and stirred at a speed of 200 r / min for 5 minutes, and then the speed is increased to 1500 r / min, and a mixture of water and glacial acetic acid is slowly added dropwise in multiple times within 20 minutes. When all the water has been dripped, an organic antibacterial agent is added, and the speed is increased to 3000 r / min and stirring is continued for 20 minutes to obtain a softener.

[0042] Example 3

[0043] A softener is composed of the following components, calculated by percentage: 10% tetramethyldisiloxane, 12% cyclohexylmethyldimethoxysilane, 10% allyl glycidyl ether, 5% polyetheramine, 13% isopropyl alcohol, 12% diethylene glycol butyl ether, 3% triethanolamine dodecylbenzenesulfonate, 2% SDS, 4% fatty alcohol polyoxyethylene ether, 0.3% glacial acetic acid, 0.2% natural antibacterial agent, and the balance is water.

[0044] The preparation method is as follows:

[0045] (1) Tetramethyldisiloxane and cyclohexylmethyldimethoxysilane were sequentially added to a four-necked flask equipped with a condenser, a separatory funnel, a thermometer, and a nitrogen protection device. The device was sealed, nitrogen was introduced, and the temperature was raised to 80°C. After keeping the temperature for 1.5 hours, the catalyst tetramethylammonium hydroxide and the solvent DMSO were added. After stirring and heating to 120°C for 5 hours, the end-capping agent hexamethyldisiloxane was added and the reaction was continued for 1.5 hours. The mass ratio of tetramethyldisiloxane, cyclohexylmethyldimethoxysilane, solvent, and end-capping agent was 3:3:2, and the amount of catalyst was 1% of the total amount of tetramethyldisiloxane, cyclohexylmethyldimethoxysilane, and end-capping agent. The catalyst tetramethylammonium hydroxide was heated to 140°C to decompose under high temperature. After cooling, the low-boiling-point substances were removed by vacuum distillation to obtain amino silicone oil.

[0046] (2) Isopropyl alcohol, allyl glycidyl ether, diethylene glycol butyl ether, and polyetheramine were mixed and then dripped into a three-necked flask containing amino silicone oil, wherein the mass ratio of amino silicone oil to polyetheramine was 30:1. Nitrogen was used for protection, and the temperature was raised to 50°C with stirring. The reaction time was 6 hours. Triethanolamine dodecylbenzenesulfonate was added, and the reaction was continued with stirring for 3 hours. The reaction temperature was 70°C. After cooling, the low-boiling-point substances were removed by reduced pressure distillation to obtain modified amino silicone oil.

[0047] (3) SDS and fatty alcohol polyoxyethylene ether are mixed and stirred evenly, and modified amino silicone oil is added, wherein the mass ratio of fatty alcohol polyoxyethylene ether to modified amino silicone oil is 1:20, and stirred at a speed of 150 r / min for 8 minutes, and then the speed is increased to 800 r / min, and a mixture of water and glacial acetic acid is slowly added dropwise in multiple times within 40 minutes. When all the water has been dripped, a natural antibacterial agent is added, and the speed is increased to 2500 r / min and stirring is continued for 25 minutes to obtain a softener.

[0048] Comparative Example 1

[0049] A softener is composed of the following components, calculated by percentage: 12% tetramethyldisiloxane, 15% cyclohexylmethyldimethoxysilane, 8% allyl glycidyl ether, 3% polyetheramine, 15% isopropyl alcohol, 10% diethylene glycol butyl ether, 4% dodecyldimethyl tertiary amine, 2% SDS, 2% fatty alcohol polyoxyethylene ether, 0.2% glacial acetic acid, 0.1% organic antibacterial agent, and the balance being water.

[0050] The preparation method is as follows:

[0051] (1) Tetramethyldisiloxane and cyclohexylmethyldimethoxysilane were sequentially added to a four-necked flask equipped with a condenser, a separating funnel, a thermometer, and a nitrogen protection device. The device was sealed, nitrogen was introduced, and the temperature was raised to 70°C. After keeping the temperature for 2 hours, the catalyst tetramethylammonium hydroxide and the solvent DMSO were added. After stirring and heating to 90°C for 8 hours, the end-capping agent hexamethyldisiloxane was added and the reaction was continued for 1 hour. The mass ratio of tetramethyldisiloxane, cyclohexylmethyldimethoxysilane, solvent, and end-capping agent was 3:3:2, and the amount of catalyst was 0.5% of the total amount of tetramethyldisiloxane, end-capping agent, and cyclohexylmethyldimethoxysilane. The catalyst tetramethylammonium hydroxide was heated to 135°C to decompose under high temperature. After cooling, the low-boiling-point substances were removed by vacuum distillation to obtain amino silicone oil.

[0052] (2) Isopropyl alcohol, allyl glycidyl ether, diethylene glycol butyl ether, and polyetheramine were mixed and then dropped into a three-necked flask containing amino silicone oil, wherein the mass ratio of amino silicone oil to polyetheramine was 20:3. Nitrogen was used for protection, and the temperature was raised to 80°C with stirring. The reaction time was 3 hours. Dodecyldimethyl tertiary amine was added and the reaction was continued with stirring for 5 hours. The reaction temperature was 50°C. After cooling, the low-boiling-point substances were removed by vacuum distillation to obtain modified amino silicone oil.

[0053] (3) SDS and fatty alcohol polyoxyethylene ether are mixed and stirred evenly, and modified amino silicone oil is added, wherein the mass ratio of fatty alcohol polyoxyethylene ether to modified amino silicone oil is 1:10, and stirred at a speed of 100 r / min for 10 minutes, and then the speed is increased to 1000 r / min, and a mixture of water and glacial acetic acid is slowly added dropwise in multiple times within 30 minutes. When all the water has been dripped, an organic antibacterial agent is added, and the speed is increased to 2500 r / min and stirring is continued for 30 minutes to obtain a softener.

[0054] Comparative Example 2

[0055] A softener is composed of the following components, calculated by percentage: 12% methylcyclotetrasiloxane, 15% cyclohexylmethyldimethoxysilane, 8% allyl glycidyl ether, 3% polyetheramine, 15% isopropyl alcohol, 10% diethylene glycol butyl ether, 4% sodium lauryl sulfate, 2% SDS, 2% fatty alcohol polyoxyethylene ether, 0.2% glacial acetic acid, 0.1% organic antibacterial agent, and the balance is water.

[0056] The preparation method is as follows:

[0057] (1) Methylcyclotetrasiloxane and cyclohexylmethyldimethoxysilane were sequentially added to a four-necked flask equipped with a condenser, a separating funnel, a thermometer, and a nitrogen protection device. The device was sealed, nitrogen was introduced, and the temperature was raised to 70°C. After keeping the temperature for 2 hours, the catalyst tetramethylammonium hydroxide and the solvent DMSO were added. After stirring and heating to 90°C for 8 hours, the end-capping agent hexamethyldisiloxane was added and the reaction was continued for 1 hour. The mass ratio of tetramethyldisiloxane, cyclohexylmethyldimethoxysilane, solvent, and end-capping agent was 3:3:2, and the amount of catalyst was 0.5% of the total amount of tetramethyldisiloxane, end-capping agent, and cyclohexylmethyldimethoxysilane. The catalyst tetramethylammonium hydroxide was heated to 135°C to decompose under high temperature. After cooling, the low-boiling-point substances were removed by vacuum distillation to obtain amino silicone oil.

[0058] (2) Isopropyl alcohol, allyl glycidyl ether, diethylene glycol butyl ether, and polyetheramine were mixed and then dropped into a three-necked flask containing amino silicone oil, wherein the mass ratio of amino silicone oil to polyetheramine was 20:3. Nitrogen was used for protection, and the temperature was raised to 80°C with stirring. The reaction time was 3 hours. Triethanolamine dodecylbenzenesulfonate was added, and the reaction was continued with stirring for 5 hours. The reaction temperature was 50°C. After cooling, the low-boiling-point substances were removed by reduced pressure distillation to obtain modified amino silicone oil.

[0059] (3) SDS and fatty alcohol polyoxyethylene ether are mixed and stirred evenly, and modified amino silicone oil is added, wherein the mass ratio of fatty alcohol polyoxyethylene ether to modified amino silicone oil is 1:10, and stirred at a speed of 100 r / min for 10 minutes, and then the speed is increased to 1000 r / min, and a mixture of water and glacial acetic acid is slowly added dropwise in multiple times within 30 minutes. When all the water has been dripped, an organic antibacterial agent is added, and the speed is increased to 2500 r / min and stirring is continued for 30 minutes to obtain a softener.

[0060] Comparative Example 3

[0061] A softener is composed of the following components, calculated by percentage: 12% tetramethyldisiloxane, 36% cyclohexylmethyldimethoxysilane, 8% allyl glycidyl ether, 3% polyetheramine, 15% isopropyl alcohol, 10% diethylene glycol butyl ether, 4% triethanolamine dodecylbenzenesulfonate, 2% SDS, 2% fatty alcohol polyoxyethylene ether, 0.2% glacial acetic acid, 0.1% organic antibacterial agent, and the balance being water.

[0062] The preparation method is as follows:

[0063] (1) Tetramethyldisiloxane and cyclohexylmethyldimethoxysilane were sequentially added to a four-necked flask equipped with a condenser, a separating funnel, a thermometer, and a nitrogen protection device. The device was sealed, nitrogen was introduced, and the temperature was raised to 70°C. After keeping the temperature for 2 hours, the catalyst tetramethylammonium hydroxide and the solvent DMSO were added. After stirring and heating to 90°C for 8 hours, the end-capping agent hexamethyldisiloxane was added and the reaction was continued for 1 hour. The mass ratio of tetramethyldisiloxane, cyclohexylmethyldimethoxysilane, solvent, and end-capping agent was 3:3:2, and the amount of catalyst was 0.5% of the total amount of tetramethyldisiloxane, end-capping agent, and cyclohexylmethyldimethoxysilane. The catalyst tetramethylammonium hydroxide was heated to 135°C to decompose under high temperature. After cooling, the low-boiling-point substances were removed by vacuum distillation to obtain amino silicone oil.

[0064] (2) Isopropyl alcohol, allyl glycidyl ether, diethylene glycol butyl ether, and polyetheramine were mixed and then dropped into a three-necked flask containing amino silicone oil, wherein the mass ratio of amino silicone oil to polyetheramine was 20:3. Nitrogen was used for protection, and the temperature was raised to 80°C with stirring. The reaction time was 3 hours. Triethanolamine dodecylbenzenesulfonate was added, and the reaction was continued with stirring for 5 hours. The reaction temperature was 50°C. After cooling, the low-boiling-point substances were removed by reduced pressure distillation to obtain modified amino silicone oil.

[0065] (3) SDS and fatty alcohol polyoxyethylene ether are mixed and stirred evenly, and modified amino silicone oil is added, wherein the mass ratio of fatty alcohol polyoxyethylene ether to modified amino silicone oil is 1:10, and stirred at a speed of 100 r / min for 10 minutes, and then the speed is increased to 1000 r / min, and a mixture of water and glacial acetic acid is slowly added dropwise in multiple times within 30 minutes. When all the water has been dripped, an organic antibacterial agent is added, and the speed is increased to 2500 r / min and stirring is continued for 30 minutes to obtain a softener.

[0066] Effect test 1: fabric feel test

[0067] Formula: softener, (g / L) (see Table 1 for details), working solution pH value: 4-6, fabric: 20×16 / 128×60 blue cotton woven fabric.

[0068] Process: The fabric sample to be treated is subjected to two-dipping and two-rolling softening treatment on a vertical rolling mill (rolling pressure: 2kg; liquid carrying rate: 75%) → set in a tenter drying and setting machine (160℃×90s) → evaluate the feel.

[0069] Feel evaluation rules: The scoring is based on a 100-point system and is given by feel evaluation professionals. The higher the score, the better the feel, and the lower the score, the worse the feel.

[0070] The fabric feel evaluation table of fabrics treated with different softeners is shown in Table 1. As can be seen from Table 1, the new non-yellowing, soft, and highly stable cotton softener has an excellent soft and fluffy feel, which is significantly better than the representative softeners on the market.

[0071] Table 1

[0072]

[0073] Effect test 2: Fabric phenol yellowing test

[0074] Formula: softener, (g / L) (see Table 2 for details), working solution pH value: 4-6, fabric: 40×40 / 133×76 whitening cotton woven fabric.

[0075] Process: The fabric samples to be treated are subjected to a two-dip and two-roll softening treatment using a vertical padder (rolling pressure: 2kg; liquid carryover rate: 65%) → tested in accordance with GB / T 29778-2013 “Textiles - Tests for Colour Fastness - Evaluation of Potential Phenolic Yellowing”.

[0076] The yellowing test table of fabrics treated with different softeners is shown in Table 2. As can be seen from Table 2, the fabrics treated with the new non-yellowing, soft and high-stability softener for cotton have basically no phenol yellowing.

[0077] Table 2

[0078]

[0079]

[0080] Effect test 3: fabric color change test

[0081] Formula: softener 30g / L (see Table 3 for details), working solution pH value: 4-6, fabric: 20×16 / 128×60 blue cotton woven fabric.

[0082] Process: The fabric sample to be treated is subjected to a two-immersion and two-rolling softening treatment using a vertical roller (rolling pressure: 2kg; liquid carryover rate: 65%) → tested in accordance with GB / T 30669-2014 “Textiles - Tests for colour fastness - Colour fastness to yellowing”.

[0083] The test table of fabric color change after the fabrics were treated with different softeners is shown in Table 3. As can be seen from Table 3, the fabric color is basically not affected after the fabric is treated with the new non-yellowing, soft and high-stability softener for cotton.

[0084] Table 3

[0085]

[0086] Effect test 4: Fabric hydrophilicity test

[0087] Formula: softener, (g / L) (see Table 4 for details), working solution pH value: 4-6, fabric: 40×40 / 133×76 whitening cotton woven fabric.

[0088] Process: The fabric sample to be treated is subjected to a two-immersion and two-rolling softening treatment using a vertical roller (rolling pressure: 2kg; liquid pick-up rate: 65%) → GB / T 21655.1 Textiles - Evaluation of Moisture Absorption and Quick-Drying Performance Series (II) - Droplet Diffusion Time is tested.

[0089] The hydrophilicity test table of fabrics treated with different softeners is shown in Table 4. As can be seen from Table 4, the hydrophilicity of fabrics treated with the new non-yellowing, soft and high-stability softener for cotton is significantly improved, which is better than the representative softeners on the market.

[0090] Table 4

[0091]

[0092]

[0093] Effect test 5: Fabric fastness test

[0094] Formula: softener, (g / L) (see Table 5 for details), working solution pH value: 4-6, fabric: 20×16 / 128×60 blue cotton woven fabric.

[0095] Process: The fabric sample to be treated is subjected to a two-immersion and two-rolling softening treatment using a vertical roller (rolling pressure: 2kg; liquid carryover rate: 65%) → tested in accordance with GB / T 3921-2008 “Textiles—Tests for Colour Fastness—Colour Fastness to Washing with Soap”.

[0096] The test table of fabric soap fastness after treatment with different softeners is shown in Table 5. As can be seen from Table 5, the soap fastness of fabric treated with the new non-yellowing, soft and high-stability softener for cotton decreases very slightly.

[0097] Table 5

[0098]

[0099]

[0100] Effect test 6: softener stability test

[0101] Formula: Softener, (g / L) (see Table 6 for details), other conditions are shown in the table.

[0102] The stability test table of different softeners is shown in Table 6. The relevant test methods are briefly described as follows:

[0103] The comprehensive stability test method is to test the stability of the working fluid of the sample to be tested under different pH values and high-speed shear force conditions.

[0104] The alkali resistance test method is to test the stability of the working solution of the sample to be tested under alkaline conditions.

[0105] The salt tolerance test method is to test the stability of the working solution of the sample to be tested under high salt conditions.

[0106] The high temperature resistance test method is to test the stability of the working fluid of the sample to be tested under high temperature conditions.

[0107] The test method for the stability of the fixing agent in a co-bath is to test the stability of the working solution of the sample to be tested and the fixing agent in a co-bath.

[0108] The test method for the co-bath stability of the brightener is to test the stability of the co-bath of the working solution of the sample to be tested and the brightener.

[0109] As can be seen from Table 6, the new non-yellowing, soft and high-stability softener for cotton has excellent stability.

[0110] Table 6

[0111]

[0112]

[0113] Note: High stability judgment standard: the working liquid pH is adjusted to 11, the shearing equipment speed is 2000rad / mintiao, and the test liquid is still stable after being placed for 24 hours;

[0114] Medium stability judgment standard: the working liquid pH is adjusted to 10.5, the shear equipment speed is 2000rad / mintiao, and the test liquid remains stable after being placed for 24 hours;

[0115] Basic stability judgment standard: the working liquid pH is adjusted to 9, the shearing equipment speed is 2000rad / mintiao, and the test liquid remains stable after being placed for 24 hours;

[0116] Stability judgment standard: the sample working solution remains stable after being placed for 24 hours after the test;

[0117] Instability judgment standard: If the test sample shows unstable phenomena such as floating fibers, floating oil, or stratification during testing or the working fluid is left for less than 24 hours, it is judged to be unstable.

[0118] Finally, it should be noted that the above content is only used to illustrate the technical solution of the present invention, rather than to limit the scope of protection of the present invention. Simple modifications or equivalent substitutions of the technical solution of the present invention by ordinary technicians in this field do not deviate from the essence and scope of the technical solution of the present invention.

Claims

1. A softener, characterized in that Calculated by percentage, it is composed of the following components: 8-12% of tetramethyldisiloxane, 10-15% of cyclohexylmethyldimethoxysilane, 3-6% of polyetheramine, 8-12% of allyl glycidyl ether, 10-15% of isopropyl alcohol, 10-15% of diethylene glycol butyl ether, 2-4% of alkylbenzenesulfonic acid amine, 2-4% of surfactant, 0.2-0.4% of pH regulator, 0.1-0.2% of antibacterial agent and water to make up to 100%. The alkylbenzenesulfonate amine is triethanolamine dodecylbenzenesulfonate, the surfactant includes an anionic surfactant and a nonionic surfactant, and the antibacterial agent is selected from one or more of an inorganic antibacterial agent, an organic antibacterial agent and a natural antibacterial agent.

2. The softener according to claim 1, characterized in that The molecular weight of the polyetheramine is 200-400, and the pH regulator is glacial acetic acid.

3. The softener according to claim 1, characterized in that The anionic surfactant is selected from sodium lauryl sulfate or sodium of higher fatty acid, the nonionic surfactant is a polyoxyethylene ether surfactant, the antibacterial agent is an organic antibacterial agent, and the polyoxyethylene ether surfactant is fatty alcohol polyoxyethylene ether.

4. A method for preparing a softener according to claim 1, characterized in that: The steps include: (1) reacting tetramethyldisiloxane and cyclohexylmethyldimethoxysilane to obtain aminosilicone oil; (2) reacting amino silicone oil with isopropyl alcohol, allyl glycidyl ether, diethylene glycol butyl ether and polyetheramine, and then adding alkylbenzene sulfonate amine to react to obtain modified amino silicone oil; (3) The modified amino silicone oil is reacted with a surfactant, and a pH regulator, an antibacterial agent and water are added and stirred to obtain a softener.

5. The preparation method according to claim 4, characterized in that In step (1), the temperature needs to be raised before the reaction, and a catalyst, a solvent and a capping agent need to be added. After the reaction, the temperature needs to be lowered and the mixture needs to be distilled under reduced pressure.

6. The preparation method according to claim 5, characterized in that The heating temperature is 90-120° C., the heating time is 5-9 hours, the catalyst is tetramethylammonium hydroxide, the solvent is dimethyl sulfoxide or isopropyl alcohol, the end-capping agent is hexamethyldisiloxane, the mass ratio of tetramethyldisiloxane, cyclohexylmethyldimethoxysilane, solvent and end-capping agent is 3:3-4:2-3, the amount of the catalyst is 0.5-2% of the total amount of tetramethyldisiloxane, cyclohexylmethyldimethoxysilane and end-capping agent, the heating temperature is 135-145° C., the reaction in step (1) is carried out in a sealed device, the sealed device includes a condenser, a separatory funnel, a thermometer and a nitrogen protection device, the reaction temperature in step (1) is 70-100° C., and the reaction time is 1-2 hours.

7. The preparation method according to claim 4, characterized in that The mass ratio of the amino silicone oil, isopropyl alcohol, allyl glycidyl ether, diethylene glycol butyl ether, polyetheramine and alkylbenzenesulfonic acid amine in step (2) is 10-30:4-5:2-3:2-3:1-3:1, the reaction temperature in step (2) is 45-80°C, the reaction time is 3-6h, the mass ratio of the modified amino silicone oil to the surfactant in step (3) is 10-30:1, the stirring speed is 2500-3000rpm, and the stirring time is 20-30min.

8. Use of the softener according to any one of claims 1 to 3 or the softener prepared by the preparation method according to any one of claims 4 to 7 in softening and finishing fabrics.

Images