A non-yellowing, soft and high-stability softener for cotton and preparation method thereof

Abstract

The invention discloses a non-yellowing, soft, and highly stable softener for cotton and a preparation method thereof, and relates to the technical field of textile printing and dyeing auxiliaries. The invention adopts methylcyclotetrasiloxane, 3-aminopropylmethyldimethoxysilane, cyclohexylmethyldimethoxysilane, and hexamethyldisiloxane to polymerize and prepare aminosilicone oil, utilizes the epoxy group in the diepoxy-terminated polyether to carry out an ammonia decomposition ring-opening reaction with the aminosilicone oil, introduces a polyether segment containing an epoxy group on the amino group of the aminosilicone oil, and then utilizes the introduced epoxy group to carry out an amino reaction with dodecyldimethyl tertiary amine to obtain a quaternary ammonium salt, prepares the final modified silicone oil, and the modified silicone oil is compounded with a surfactant to prepare a non-yellowing, soft, and highly stable softener for cotton, which has excellent softening effect, fluffy hand feeling, washability, extremely high stability, and can be self-emulsified, easy to use, and will not affect the whiteness, color light, and fastness of dyed fabrics.

Description

Technical Field

[0001] The invention belongs to the technical field of textile printing and dyeing auxiliaries, and particularly relates to a non-yellowing, soft and high-stability softener for cotton and a preparation method thereof. Background Art

[0002] Softening agents have been used on textiles for half a century. They are used to change the feel of textile materials and make the fabrics more comfortable. With the improvement of living standards, people pay more and more attention to the feel of textiles, requiring fabrics to be hygroscopic, breathable, comfortable to wear, and have a high-end soft, fluffy, and elegant feel. Among the softeners currently on the market, amino silicone oil softeners have the best feel, but most of the amino silicone oil softeners are N-(β-aminoethyl)-y-aminopropyl modified polysiloxanes. Because they contain active hydrogen on the side chain, they are easily oxidized to produce chromophores (azo and oxidized azo groups), causing yellowing. And due to the special structure of the amino group, there are also problems such as difficulty in emulsification, easy demulsification during storage and use, and easy oil floating.

[0003] At present, the softener that reduces the yellowing of amino silicone oil mainly adopts a heterocyclic coupling agent with a small amount of active hydrogen, and then introduces a polyether group into the amino silicone oil. By adjusting the ratio of the polyether group to the silicone chain segment, a microemulsion is prepared. While retaining the high hand feel characteristics of the original amino silicone oil, the yellowing phenomenon is effectively inhibited, and the shortcomings of amino silicone oil such as insolubility in organic matter and water and difficulty in emulsification can be solved. The demulsification and oil floating phenomena of amino silicone oil during storage and use are also improved, fundamentally solving the problems of traditional amino silicone oil's inability to withstand high shear force and centrifugal force. The compatibility of amino silicone oil with other textile dyeing and finishing auxiliaries is also improved, breaking the restrictions on the production and use of amino silicone oil, and synthesizing a softener with low yellowing, high hand feel and high stability.

[0004] The journal literature (Research and Development of Hydrophilic Silicone Softener, Fan Yanping et al., "Printing and Dyeing Auxiliary Agents") starts from the structure and properties of silicone, and according to the HLB value of the emulsifier emulsion polymer, the anionic surfactant and non-ionic surfactant are compounded and modified to develop a softener with good hydrophilicity and softness.

[0005] Master's thesis (Aminosilicone softener containing cyclic hydrocarbon groups in the molecule and its mechanism of action on fiber fabrics, Li Mingtao) Under the action of alkaline catalyst, a series of polysiloxanes ASO-702 and Ph-ASO with cyclic hydrocarbon groups in the molecule were synthesized by polymerization reaction of octamethylcyclotetrasiloxane (D4) and different silanes such as N-cyclohexyl-γ-aminopropylmethyldimethoxysilane (KH-702) or diphenyldimethoxysilane (KH-303). The application on cotton fiber fabrics shows that the newly developed aminosilicone can significantly reduce the bending stiffness of the fabric, increase the wrinkle recovery angle of the fabric, (improve the fracture and tear strength) and give the fabric a more comfortable feel.

[0006] Master's thesis (Synthesis of block polyether modified polysiloxane and its application in moisture absorption and perspiration finishing of fabrics, Xiao Bo) Using Si-H bond terminated polydimethylsiloxane (PHMS) and allyl epoxy terminated polyoxyethylene polyoxypropylene ether (APEE) as raw materials, the intermediate epoxy terminated polyether block polysiloxane (PESO) was synthesized through hydrosilylation addition reaction, and then the block polyether modified polysiloxane (BPEMS) was synthesized by aminolysis ring-opening reaction of PESO and tetramethylpiperidinamine (TEMP). Fatty alcohol polyoxyethylene ether (AEO) was selected as an emulsifier to emulsify BPEMS to obtain a microemulsion with transparent appearance and stable performance. The performance of the fabric finished with it was greatly improved, and when the molecular weight of the terminal hydrogen silicone oil (PHMS) was 0.67×1 0 4 When the content of Si-H is 0.03%, the molecular weight of active polyether (APEE) is 500g / mol, and the amount of emulsion is 8g / L, the finished fabric has good softness and resilience, the static water absorption time can reach 4.5s, and the whiteness is basically close to that of blank cotton fabric.

[0007] Although the above prior art has proposed some improvement methods, the degree of improvement in comprehensive performance is still limited. In view of the problems existing in conventional softeners on the market: (1) poor softening and fluffy effects, the treated fabric is hard and rough; (2) poor washability, the hand feel is seriously reduced after washing; (3) poor stability, and problems such as demulsification and roller sticking are easily generated during use; (4) it will affect the color and fastness of the fabric, seriously affecting the quality of the final fabric. It is necessary to provide a softener with excellent softening effect, fluffy hand feel, washability, extremely high stability, self-emulsification, easy to use, and will not affect the whiteness, color, and fastness of dyed fabrics. Summary of the invention

[0008] The present invention aims at the problems existing in the prior art and provides a non-yellowing, soft and high-stability softener for cotton and a preparation method thereof. The present invention adopts methylcyclotetrasiloxane, 3-aminopropylmethyldimethoxysilane, cyclohexylmethyldimethoxysilane and hexamethyldisiloxane to polymerize to prepare aminosilicone oil, utilizes the epoxy group in the diepoxy-terminated polyether to carry out an ammonia decomposition ring-opening reaction with the aminosilicone oil, introduces a polyether segment containing an epoxy group to the amino group of the aminosilicone oil, and then utilizes the introduced epoxy group to carry out an amino reaction with dodecyldimethyl tertiary amine to obtain a quaternary ammonium salt, thereby preparing the final modified silicone oil. Due to the introduction of the cyclohexyl high steric hindrance group, the amino group on the silicone oil needs higher energy to be oxidized, thereby reducing the yellowing of the amino silicone oil; after the primary amino group on the amino silicone oil is modified, the active hydrogen is reduced, effectively improving the yellowing of the amino silicone oil; due to the introduction of the polyether segment, the hydrophilicity of the silicone oil can be improved, making it easy to emulsify; due to the introduction of the ammonia reaction, the epoxy group ring is opened and the highly active hydroxyl group is introduced, which can be cross-linked or copolymerized with various fibers and other polymers, improving the hydrophilicity of the fabric, without the need to add additional emulsifiers, and can be directly dissolved in water under weak acidic conditions, which can give the silicone oil self-emulsification properties. The prepared modified silicone oil is compounded with a surfactant to prepare a non-yellowing soft and high-stability softener for cotton, which has excellent softening effect, fluffy feel, washability, extremely high stability, and can be self-emulsified, easy to use, and will not affect the whiteness, color, and fastness of the dyed fabric.

[0009] To achieve the above purpose, the technical solution adopted by the present invention is as follows:

[0010] In a first aspect, the present invention provides a non-yellowing, soft and high-stability softener for cotton, which comprises the following raw materials in parts by weight:

[0011]

[0012] Wherein, the anionic surfactant is selected from SDS and / or sodium of higher fatty acid.

[0013] Among them, the nonionic surfactant is a polyoxyethylene ether surfactant, preferably a fatty alcohol polyoxyethylene ether.

[0014] The antibacterial agent is selected from one or more of inorganic antibacterial agents, organic antibacterial agents or natural antibacterial agents, preferably organic antibacterial agents.

[0015] The pH adjuster may be any common pH adjuster in the art, preferably glacial acetic acid.

[0016] The preparation method of the modified silicone oil comprises the following steps:

[0017] Step S1: Prepare amino silicone oil. Add methylcyclotetrasiloxane, 3-aminopropylmethyldimethoxysilane, and cyclohexylmethyldimethoxysilane in a four-necked flask equipped with a condenser, a separatory funnel, a thermometer, and a nitrogen protection device. Seal the device, pass nitrogen, and heat to 70-100°C. After keeping warm for 1-2 hours, add the catalyst tetramethylammonium hydroxide and the solvent. Stir and heat to 90-120°C for 5-9 hours, then add the end-capping agent hexamethyldisiloxane and continue to react for 1-2 hours. Heat to 135-155°C to decompose the catalyst tetramethylammonium hydroxide at high temperature. After cooling, remove small molecular weight low-boiling substances by vacuum distillation to obtain amino silicone oil;

[0018] Step S2: preparing modified amino silicone oil containing epoxy groups, mixing isopropyl alcohol and diepoxy-terminated polyether and then dropping the mixture into a three-necked flask containing amino silicone oil, using nitrogen protection, stirring and heating to react;

[0019] Step S3: Add dodecyldimethyl tertiary amine to the three-necked flask containing the modified amino silicone oil containing epoxy groups in step S2, continue stirring the reaction for 4-8 hours, and after cooling, remove small molecular weight low-boiling substances by reduced pressure distillation to obtain amino silicone oil.

[0020] Wherein, in step S1, the mass ratio of methylcyclotetrasiloxane, 3-aminopropylmethyldimethoxysilane and cyclohexylmethyldimethoxysilane is 1:1.3:1.1.

[0021] Wherein, the molecular weight of the diepoxy terminated polyether is 2000-4000.

[0022] The solvent in step S1 can be any common solvent in the art, preferably DMSO and / or isopropanol.

[0023] Wherein, the amount of the catalyst used in step S1 is 0.5%-2% of the total amount of methylcyclotetrasiloxane, 3-aminopropylmethyldimethoxysilane, cyclohexylmethyldimethoxysilane and the end-capping agent hexamethyldisiloxane.

[0024] Wherein, in step S2, the mass ratio of the diepoxy-terminated polyether to the amino silicone oil is 1:(10-30).

[0025] Wherein, the reaction temperature of step S2 is 40-80°C and the reaction time is 3-7h.

[0026] Wherein, in step S3, the mass ratio of dodecyldimethyl tertiary amine to modified amino silicone oil containing epoxy group is 1:(10-30).

[0027] Wherein, the reaction temperature of step S3 is 40-80°C and the reaction time is 4-8h.

[0028] In a second aspect, the present application provides a method for preparing the above-mentioned non-yellowing, soft and high-stability softener for cotton, comprising the following steps:

[0029] Weigh the raw materials according to the formula, mix and stir the nonionic surfactant and anionic surfactant evenly, add modified silicone oil, stir at a speed of 100-200r / min for 5-10min, then increase the speed to 800-1500r / min, slowly add a mixture of water and pH regulator in multiple times within 20-40min, when all the water has been dripped, add the antibacterial agent, increase the speed to 2500-3000r / min and continue stirring for 20-30min, so as to obtain a non-yellowing, soft and high-stability softener for cotton.

[0030] Compared with the prior art, the present invention has the following beneficial effects:

[0031] 1. The present invention adopts methylcyclotetrasiloxane, 3-aminopropylmethyldimethoxysilane, cyclohexylmethyldimethoxysilane and hexamethyldisiloxane to polymerize and prepare aminosilicone oil, utilizes the epoxy group in the diepoxy-terminated polyether to carry out an ammonia ring-opening reaction with the aminosilicone oil, introduces a polyether segment containing an epoxy group into the amino group of the aminosilicone oil, and then utilizes the introduced epoxy group to carry out an amino reaction with dodecyldimethyl tertiary amine to obtain a quaternary ammonium salt, thereby preparing the final modified silicone oil. Due to the introduction of the cyclohexyl high steric hindrance group, the amino group on the silicone oil needs higher energy to be oxidized, thereby reducing the yellowing of the amino silicone oil; after the primary amino group on the amino silicone oil is modified, the active hydrogen is reduced, effectively improving the yellowing of the amino silicone oil; due to the introduction of the polyether segment, the hydrophilicity of the silicone oil can be improved, making it easy to emulsify; due to the introduction of the ammonia reaction, the epoxy group ring is opened and the highly active hydroxyl group is introduced, which can be cross-linked or copolymerized with various fibers and other polymers, improving the hydrophilicity of the fabric, without the need to add additional emulsifiers, and can be directly dissolved in water under weak acidic conditions, which can give the silicone oil self-emulsification properties. The prepared modified silicone oil is compounded with a surfactant to prepare a non-yellowing soft and high-stability softener for cotton, which has excellent softening effect, fluffy feel, washability, extremely high stability, and can be self-emulsified, easy to use, and will not affect the whiteness, color, and fastness of the dyed fabric.

[0032] 2. The non-yellowing, soft, and highly stable softener for cotton of the present invention has the following advantages: it imparts excellent soft, fluffy, and smooth feel to the fabric, among which the soft and fluffy feel is particularly prominent; it has low yellowing or even no yellowing characteristics, and can also be used on white / light-colored fabrics; it has excellent hydrophilic properties, and the hydrophilic effect of the treated fabric is excellent; it has excellent wash resistance, and can still maintain a good feel after multiple washings; it has excellent compatibility with general textile auxiliaries, such as cationic softeners, etc.; it will not affect the color and fastness of dyed fabrics; it has excellent stability and can be fully used. DETAILED DESCRIPTION

[0033] It is worth noting that the raw materials used in the present invention are all common commercially available products, and their sources are not specifically limited.

[0034] The following sources of raw materials are provided for illustrative purposes:

[0035] Methylcyclotetrasiloxane, 3-aminopropylmethyldimethoxysilane, cyclohexylmethyldimethoxysilane, tetramethylammonium hydroxide, DMSO, isopropanol, hexamethyldisiloxane, dodecyldimethyl tertiary amine: commercially available;

[0036] Diepoxy-terminated polyether: molecular weight 2000-4000, commercially available;

[0037] Nonionic surfactant: AEO-9, commercially available;

[0038] Anionic surfactant: SDS, commercially available;

[0039] Antimicrobial agent: polyhexamethylene biguanide hydrochloride, commercially available;

[0040] pH adjuster: glacial acetic acid, commercially available.

[0041] Example 1

[0042] Weigh 40g of modified silicone oil, 10g of anionic surfactant, 10g of nonionic surfactant, 0.4g of antibacterial agent, 5g of pH regulator and 150g of water, mix the nonionic surfactant and anionic surfactant and stir evenly, add modified silicone oil, stir at 100r / min for 10min, then increase the speed to 1000r / min, slowly add the mixture of water and pH regulator in several times within 30min, when all the water has been dripped, add antibacterial agent, increase the speed to 2500r / min and continue stirring for 20min to obtain a non-yellowing, soft and high-stability softener for cotton.

[0043] Wherein, the preparation method of modified silicone oil comprises the following steps:

[0044] Step S1: Prepare amino silicone oil. Add 50 grams of methylcyclotetrasiloxane, 65 grams of 3-aminopropylmethyldimethoxysilane, and 55 grams of cyclohexylmethyldimethoxysilane into a four-necked flask equipped with a condenser, a separatory funnel, a thermometer, and a nitrogen protection device. Seal the device, pass nitrogen, and heat to 70°C. After keeping warm for 2 hours, add 20 grams of catalyst tetramethylammonium hydroxide and 40 grams of DMSO. Stir and heat to 90°C for 8 hours, then add 20 grams of end-capping agent hexamethyldisiloxane and continue to react for 1 hour. Heat to 135°C to decompose the catalyst tetramethylammonium hydroxide at high temperature. After cooling, remove small molecular low-boiling substances by vacuum distillation to obtain amino silicone oil;

[0045] Step S2: Prepare modified amino silicone oil containing epoxy groups, mix 40g of isopropanol and 10g of diepoxy-terminated polyether and drop them into a three-necked flask filled with amino silicone oil, use nitrogen protection, stir and heat to 80°C, and the reaction time is 3h;

[0046] Step S3: Add 10 g of dodecyl dimethyl tertiary amine into the three-necked flask containing the modified amino silicone oil containing epoxy groups in step S2, continue stirring and reacting for 5 hours at a reaction temperature of 50°C. After cooling, remove small molecular weight low-boiling substances by reduced pressure distillation to obtain amino silicone oil.

[0047] Example 2

[0048] Weigh 20g of modified silicone oil, 20g of anionic surfactant, 20g of nonionic surfactant, 0.4g of antibacterial agent, 4g of pH regulator and 100g of water, mix the nonionic surfactant and anionic surfactant and stir evenly, add modified silicone oil, stir at 200r / min for 5min, then increase the speed to 1500r / min, slowly add the mixture of water and pH regulator in several times within 20min, when all the water has been dripped, add antibacterial agent, increase the speed to 3000r / min and continue stirring for 20min to obtain a non-yellowing, soft and high-stability softener for cotton.

[0049] Wherein, the preparation method of modified silicone oil comprises the following steps:

[0050] Step S1: Prepare amino silicone oil. Add 60 grams of methylcyclotetrasiloxane, 78 grams of 3-aminopropylmethyldimethoxysilane, and 66 grams of cyclohexylmethyldimethoxysilane into a four-necked flask equipped with a condenser, a separatory funnel, a thermometer, and a nitrogen protection device. Seal the device, pass nitrogen, and heat to 100°C. After keeping warm for 1 hour, add 20 grams of catalyst tetramethylammonium hydroxide and 45 grams of DMSO. Stir and heat to 110°C for 5 hours, then add 20 grams of end-capping agent hexamethyldisiloxane and continue to react for 1.5 hours. Heat to 145°C to decompose the catalyst tetramethylammonium hydroxide at high temperature. After cooling, remove small molecular low-boiling substances by vacuum distillation to obtain amino silicone oil;

[0051] Step S2: Prepare modified amino silicone oil containing epoxy groups, mix 40g of isopropanol and 10g of diepoxy-terminated polyether and drop them into a three-necked flask containing amino silicone oil, use nitrogen protection, stir and heat to 45°C, and the reaction time is 6h;

[0052] Step S3: Add 10 g of dodecyl dimethyl tertiary amine into the three-necked flask containing the modified amino silicone oil containing epoxy groups in step S2, continue stirring and reacting for 4 hours at a reaction temperature of 60°C. After cooling, remove small molecular weight low-boiling substances by reduced pressure distillation to obtain amino silicone oil.

[0053] Example 3

[0054] Weigh 30g of modified silicone oil, 15g of anionic surfactant, 15g of nonionic surfactant, 0.4g of antibacterial agent, 3g of pH regulator and 150g of water, mix the nonionic surfactant and anionic surfactant and stir evenly, add modified silicone oil, stir at 150r / min for 8min, then increase the speed to 800r / min, slowly add dropwise the mixture of water and pH regulator in several times within 40min, when all the water has been dripped off, add antibacterial agent, increase the speed to 2500r / min and continue stirring for 25min to obtain a non-yellowing, soft and high-stability softener for cotton.

[0055] Wherein, the preparation method of modified silicone oil comprises the following steps:

[0056] Step S1: Prepare amino silicone oil. Add 65 grams of methylcyclotetrasiloxane, 84.5 grams of 3-aminopropylmethyldimethoxysilane, and 71.5 grams of cyclohexylmethyldimethoxysilane into a four-necked flask equipped with a condenser, a separatory funnel, a thermometer, and a nitrogen protection device. Seal the device, pass nitrogen, and heat to 80°C. After keeping warm for 1.5 hours, add 20 grams of catalyst tetramethylammonium hydroxide and 60 grams of DMSO. Stir and heat to 120°C for 5 hours, then add 20 grams of end-capping agent hexamethyldisiloxane and continue to react for 1.5 hours. Heat to 140°C to decompose the catalyst tetramethylammonium hydroxide at high temperature. After cooling, remove small molecular weight low-boiling substances by vacuum distillation to obtain amino silicone oil;

[0057] Step S2: Prepare modified amino silicone oil containing epoxy groups, mix 45g of isopropanol and 10g of diepoxy-terminated polyether, and then drop them into a three-necked flask filled with amino silicone oil, use nitrogen protection, stir and heat to 50°C, and the reaction time is 6h;

[0058] Step S3: Add 10 g of dodecyl dimethyl tertiary amine into the three-necked flask containing the modified amino silicone oil containing epoxy groups in step S2, continue stirring and reacting for 3 hours at a reaction temperature of 70°C. After cooling, remove small molecular weight low-boiling substances by reduced pressure distillation to obtain amino silicone oil.

[0059] Comparative Example 1

[0060] Except that dodecyl dimethyl tertiary amine was not added when preparing the modified silicone oil, the rest was the same as in Example 1.

[0061] Comparative Example 2

[0062] Except that cyclohexylmethyldimethoxysilane was not added when preparing the modified silicone oil, the rest was the same as in Example 1.

[0063] Comparative Example 3

[0064] The modified silicone oil was prepared in the same manner as in Example 1 except that the total amount of methylcyclotetrasiloxane, 3-aminopropylmethyldimethoxysilane and cyclohexylmethyldimethoxysilane was the same as in Example 1, but the mass ratio of the three was 1.5:1.1:0.8. The rest was the same as in Example 1.

[0065] Comparative Example 4

[0066] The same procedures as in Example 1 were followed except that the molar ratio of dodecyldimethyl tertiary amine to the epoxy-containing modified amino silicone oil was 0.8:1.2 during the preparation of the modified silicone oil.

[0067] Comparative Example 5

[0068] Except for using 3-dimethylaminopropylamine instead of dodecyldimethyl tertiary amine, the rest is the same as Example 1.

[0069] Test example

[0070] Experiment 1: Fabric feel test after different softeners were applied to fabrics

[0071] Formula: softener Xg / l (see the table for details), working solution PH value: 4-6; fabric: 20×16 / 128×60 blue cotton woven fabric;

[0072] Process: two dips and two rolls (liquid carrying rate: 75%) → shaping (160℃×90s) → hand feel evaluation Table 1: Fabric hand feel evaluation table for fabrics treated with different softeners

[0073]

[0074]

[0075] Note: The score is based on a 100-point system and is given by professionals who evaluate lubrication in the bath. The higher the score, the better the feel, and the lower the score, the worse the feel.

[0076] It can be seen from the above table that the non-yellowing, soft and high-stability softeners for cotton of Examples 1-3 have an excellent soft and fluffy feel effect, which is significantly better than the representative softeners on the market.

[0077] Experiment 2. Fabric yellowing test after being treated with different softeners

[0078] Formula: softener Xg / l (see table for details), working solution PH value: 4-6; fabric: 40×40 / 133×76 whitening cotton woven fabric;

[0079] Process: two dips and two rolls (liquid rate: 65%) → shaping (160℃×90s) → whiteness test

[0080] Table 2: Fabric yellowing test table of fabrics treated with different softeners

[0081]

[0082] It can be seen from the above table that the fabrics treated with the non-yellowing, soft and high-stability softeners for cotton of Examples 1-3 of the present invention have substantially no yellowing.

[0083] Experiment 3. Fabric color change test after being treated with different softeners

[0084] Formula: softener 30g / l (see table for details), working solution PH value: 4-6; fabric: 20×16 / 128×60 blue cotton woven fabric;

[0085] Process: two dips and two rolls (liquid rate: 75%) → shaping (160℃×90s) → color change test

[0086] Table 3: Fabric color change test table of fabrics treated with different softeners

[0087]

[0088] It can be seen from the above table that after the fabric is treated with the non-yellowing, soft and high-stability softener for cotton of Examples 1-3 of the present invention, the color of the fabric is basically not affected;

[0089] Experiment 4: Fabrics treated with different softeners, fabric hydrophilicity test

[0090] Formula: softener Xg / l (see table for details), working solution PH value: 4-6; fabric: 40×40 / 133×76 whitening cotton woven fabric;

[0091] Process: two dips and two rolls (liquid carrying rate: 65%) → shaping (160℃×90s) → hydrophilic test

[0092] Table 4: Fabric hydrophilicity test table of fabrics treated with different softeners

[0093]

[0094]

[0095] It can be seen from the above table that the hydrophilicity of the fabric treated with the non-yellowing, soft and high-stability softener for cotton of Examples 1-3 of the present invention is significantly improved, which is better than the representative softener on the market;

[0096] Experiment 5. Fabric fastness test after different softeners were applied to the fabric

[0097] Formula: softener Xg / l (see the table for details), working solution PH value: 4-6; fabric: 20×16 / 128×60 blue cotton woven fabric;

[0098] Process: two dips and two rolls (liquid rate: 75%) → shaping (160℃×90s) → fastness test

[0099] Table 5: Fabric fastness test table of fabrics treated with different softeners

[0100]

[0101]

[0102] It can be seen from the above table that the fastness of the fabrics treated with the non-yellowing, soft and high-stability softeners for cotton of Examples 1-3 of the present invention decreases very slightly.

[0103] Experiment 6. Stability test of different softeners

[0104] Formula: Softener 100g / l (see table for details), other conditions see table for details;

[0105] Table 6: Stability test table of different softeners

[0106]

[0107] Remark:

[0108] High safety judgment standard: at PH=11, temperature 70℃, speed 2000rpm / min, keep warm for 30min and stand for 7d;

[0109] Medium safety judgment standard: at pH = 10.5, temperature 70°C, speed 2000rpm / min, keep warm for 20 minutes and stand for 7 days;

[0110] Basic safety judgment standard: at PH=9, temperature of 50℃, rotation speed of 2000rpm / min, keep stable for 10min, and stand stable for 7d.

[0111] It can be seen from the above table that the non-yellowing, soft and high-stability softeners for cotton of Examples 1-3 of the present invention have excellent stability.

[0112] 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 non-yellowing, soft and highly stable softener for cotton, characterized in that: By weight, it includes the following raw materials: Modified silicone oil 20-60 parts; 10-30 parts of anionic surfactant; 10-30 parts of nonionic surfactant; Antibacterial agent 0.2-1 part; 3-5 parts of pH regulator; 60-200 parts of water; The preparation method of the modified silicone oil comprises the following steps: Step S1: preparing amino silicone oil, methylcyclotetrasiloxane, 3-aminopropylmethyldimethoxysilane, and cyclohexylmethyldimethoxysilane are sequentially added into a four-necked flask equipped with a condenser, a separatory funnel, a thermometer, and a nitrogen protection device, the device is sealed, nitrogen is passed through, and the temperature is raised to 70-100° C., and after keeping the temperature for 1-2 hours, a catalyst tetramethylammonium hydroxide and a solvent are added, and the temperature is stirred and raised to 90-120° C. for reaction for 5-9 hours, and then a capping agent hexamethyldisiloxane is added, and the reaction is continued for 1-2 hours, and the temperature is raised to 135-155° C. to decompose the catalyst tetramethylammonium hydroxide at high temperature, and after cooling, small molecular weight low-boiling products are removed by reduced pressure distillation to obtain amino silicone oil; wherein the mass ratio of methylcyclotetrasiloxane, 3-aminopropylmethyldimethoxysilane, and cyclohexylmethyldimethoxysilane is 1:1.3:1.1; Step S2: preparing modified amino silicone oil containing epoxy groups, mixing isopropyl alcohol and diepoxy-terminated polyether and then dropping the mixture into a three-necked flask containing amino silicone oil, using nitrogen protection, stirring and heating to react; Step S3: adding dodecyl dimethyl tertiary amine to the three-necked flask containing the modified amino silicone oil containing epoxy groups in step S2, continuing to stir the reaction for 4-8 hours, and after cooling, removing small molecular weight low-boiling products by reduced pressure distillation to obtain modified silicone oil; wherein the mass ratio of dodecyl dimethyl tertiary amine to the modified amino silicone oil containing epoxy groups is 1: (10-30).

2. The non-yellowing, soft and highly stable softener for cotton according to claim 1, characterized in that: The anionic surfactant is selected from SDS and / or sodium of higher fatty acids; the nonionic surfactant is a polyoxyethylene ether surfactant; the antibacterial agent is selected from one or more of inorganic antibacterial agents, organic antibacterial agents or natural antibacterial agents; and the pH regulator is glacial acetic acid.

3. The non-yellowing, soft and highly stable softener for cotton according to claim 2, characterized in that: The nonionic surfactant is fatty alcohol polyoxyethylene ether; the antibacterial agent is an organic antibacterial agent.

4. The non-yellowing, soft and highly stable softener for cotton according to claim 1, characterized in that: The molecular weight of the diepoxy terminated polyether is 2000-4000.

5. The non-yellowing, soft and highly stable softener for cotton according to claim 1, characterized in that: In step S1, the solvent is selected from DMSO and / or isopropanol; in step S2, the mass ratio of the diepoxy-terminated polyether to the amino silicone oil is 1:(10-30).

6. The non-yellowing, soft and highly stable softener for cotton according to claim 1, characterized in that: The reaction temperature of step S2 is 40-80°C, and the reaction time is 3-7h; the reaction temperature of step S3 is 40-80°C, and the reaction time is 4-8h.

7. A method for preparing the non-yellowing, soft and high-stability softener for cotton according to any one of claims 1 to 6, characterized in that: The steps include: Weigh the raw materials according to the formula, mix and stir the nonionic surfactant and anionic surfactant evenly, add modified silicone oil, stir at a speed of 100-200r / min for 5-10min, then increase the speed to 800-1500r / min, slowly add a mixture of water and pH regulator in multiple times within 20-40min, when all the water has been dripped, add the antibacterial agent, increase the speed to 2500-3000r / min and continue stirring for 20-30min, so as to obtain a non-yellowing, soft and high-stability softener for cotton.

8. Use of the non-yellowing, soft and high-stability softener for cotton according to any one of claims 1 to 6 in fabric treatment, characterized in that: The usage of the non-yellowing, soft and high-stability softener for cotton is 5-100 g / L.

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