Long-acting hydrophilic, soft, fluffy and washable silicone oil composition as well as preparation method and application thereof

Abstract

The invention belongs to the technical field of textile dyeing and finishing, and particularly relates to a long-acting hydrophilic, soft, fluffy and washable silicone oil composition as well as a preparation method and application thereof. The silicone oil composition is prepared from the following raw materials in parts by mass: 20 parts of modified silicone oil, 0.5 to 2.5 parts of anionic surfactant, 0.5 to 2 parts of nonionic surfactant, 0.1 to 1 part of polyhexamethylene biguanide hydrochloride, 0.2 to 0.5 part of glacial acetic acid and 76 to 79 parts of water, the modified silicone oil is prepared from the following raw materials: octamethylcyclotetrasiloxane, tetramethylethylenediamine, secondary aminated polyether amine, allyl epoxy polyether, polyether amine, allyl glycidyl ether, isopropanol, diethylene glycol butyl ether, an end-capping reagent and a catalyst. The silicone oil composition provided by the invention can endow a fabric with a long-acting hydrophilic effect, excellent hand feeling, low yellowing and washability; and the dye has excellent stability, is safe and stable to use, and does not influence the colored light of the dyed fabric.

Description

Technical Field

[0001] The invention belongs to the technical field of textile dyeing and finishing, and specifically relates to a long-lasting hydrophilic, soft, fluffy and washable silicone oil composition, and a preparation method and application thereof. Background Art

[0002] With the improvement of living standards, people have increasingly stringent requirements on the feel and wearing comfort of clothing, especially for close-fitting fabrics. In addition to requiring the fabrics to be soft, fluffy, dry, and have a strong cotton feel, they are also required to have excellent hydrophilic and hygroscopic properties, and their hydrophilic and hygroscopic properties need to be long-lasting and durable.

[0003] Softener is a product that can give fabrics the above properties, among which silicone oil softener is the leading product on the market. However, the fabrics treated with hydrophilic silicone oil on the market are soft to the touch, have poor fluffiness, poor hydrophilicity, and lack long-lasting hydrophilicity. Over time, the hydrophilicity and moisture absorption properties of the fabric will continue to deteriorate, and may even become water-repellent fabrics in the end, seriously affecting the quality of the fabric.

[0004] The applicant's previous research results: (1) The Chinese patent with publication number CN117646333A discloses a highly hydrophilic and highly stable ice-feeling softener, a preparation method and an application. The ice-feeling softener of the technical solution includes three components, wherein component 1 includes double-terminal hydrogen silicone oil, allyl polyoxyethylene polyoxypropylene epoxy polyether A, secondary amino polyether, catalyst A and solvent A, component 2 includes hydrogen-containing silicone oil, allyl polyoxyethylene polyoxypropylene epoxy polyether B, catalyst B and solvent B, and component 3 includes fatty alcohol polyoxyethylene ether, polyether polyol and water-soluble polyurethane. The ice-feeling softener prepared by the technical solution can give the fabric an excellent cool, smooth, delicate and soft hand feel. The ice-feeling softener has excellent hydrophilicity, washability and stability, and has no obvious effect on the whiteness, color and fastness of the dyed fabric.

[0005] (2) A Chinese patent with publication number CN117626670A discloses a fluffy cotton-feeling softener without phenol yellowing and its preparation method. The softener comprises the following components by percentage: 8-12% tetramethyl disiloxane, 10-15% cyclohexylmethyldimethoxysilane, 3-6% polyetheramine, 8-12% allyl glycidyl ether, 10-15% isopropyl alcohol, 10-15% diethylene glycol butyl ether, 2-4% alkylbenzenesulfonic acid amine, 2-4% surfactant, 0.2-0.4% pH regulator and 0.1-0.2% antibacterial agent. The softener prepared by the technical solution can give the fabric an excellent soft, fluffy and smooth feel, has little effect on the phenol yellowing of the fabric, has excellent hydrophilic effect and washing resistance of the fabric after treatment, and will not affect the color and fastness of the dyed fabric. The softener prepared by the technical solution has excellent compatibility with general textile auxiliaries, excellent stability and is completely usable. However, the applicant has found that the softener obtained by the above technical solution has poor hydrophilicity. Summary of the invention

[0006] In view of the above problems, the present invention provides a long-lasting hydrophilic, soft, fluffy and water-washable silicone oil composition and a preparation method and application thereof.

[0007] To achieve the above purpose, the technical solution adopted by the present invention is as follows:

[0008] The first aspect of the present invention provides a long-lasting hydrophilic, soft, fluffy, and washable silicone oil composition, which comprises, by weight, 20 parts of modified silicone oil, 0.5-2.5 parts of anionic surfactant, 0.5-2 parts of nonionic surfactant, 0.1-1 parts of polyhexamethylene biguanide hydrochloride, 0.2-0.5 parts of glacial acetic acid, and 76-79 parts of water;

[0009] The modified silicone oil comprises raw materials including: octamethylcyclotetrasiloxane, tetramethylethylenediamine, secondary aminated polyetheramine, allyl epoxy polyether, polyetheramine, allyl glycidyl ether, isopropanol, diethylene glycol butyl ether, a capping agent and a catalyst.

[0010] In some preferred embodiments, the modified silicone oil, calculated by mass, includes the following raw materials: 15-25 parts of octamethylcyclotetrasiloxane, 10-15 parts of tetramethylethylenediamine, 5-16 parts of secondary aminated polyetheramine, 5-15 parts of allyl epoxy polyether, 10-16 parts of polyetheramine, 8-16 parts of allyl glycidyl ether, 13-17 parts of isopropanol, 8-12 parts of diethylene glycol butyl ether, 0.4-0.6 parts of end-capping agent, and 0.4-0.6 parts of catalyst.

[0011] Preferably, the mass ratio of the secondary aminated polyetheramine, allyl epoxy polyether, polyetheramine and allyl glycidyl ether is 0.6-2:0.6-2:1-2:1.

[0012] In some preferred embodiments, the number average molecular weight of the secondary aminated polyetheramine is 300-500, preferably 400.

[0013] In some preferred embodiments, the number average molecular weight of the allyl epoxy polyether is 1000-2000, preferably 1500.

[0014] In some preferred embodiments, the polyetheramine has a number average molecular weight of 3000-5000, preferably 4000.

[0015] Preferably, the end-capping agent is selected from at least one of hexamethyldisiloxane and octamethyltrisiloxane.

[0016] Preferably, the catalyst is chloroplatinic acid.

[0017] In some preferred embodiments, the method for preparing the modified silicone oil comprises the following steps:

[0018] S1. Under a nitrogen atmosphere, octamethylcyclotetrasiloxane and tetramethylethylenediamine are mixed, reacted, a catalyst and isopropanol are added, the reaction is continued, a capping agent is added, the reaction is continued, and after the reaction is completed, the catalyst and isopropanol are removed to obtain amino silicone oil;

[0019] S2. Adding secondary aminated polyetheramine, allyl epoxy polyether, polyetheramine, allyl glycidyl ether and diethylene glycol butyl ether to the amino silicone oil for reaction, removing the diethylene glycol butyl ether after the reaction is completed, and obtaining modified amino silicone oil.

[0020] Preferably, step S1 is specifically as follows: under a nitrogen protective atmosphere, octamethylcyclotetrasiloxane and tetramethylethylenediamine are mixed, reacted at 75-85° C. for 1-3 hours, a catalyst and isopropanol are added, stirred and heated to 90-95° C. and the reaction is continued for 7-9 hours, a capping agent is added, and the reaction is continued for 0.5-1.5 hours. After the reaction is completed, the catalyst and isopropanol are removed to obtain amino silicone oil.

[0021] Further preferably, step S1 is specifically as follows: under a nitrogen protective atmosphere, octamethylcyclotetrasiloxane and tetramethylethylenediamine are mixed, reacted at 80° C. for 2 hours, a catalyst and isopropanol are added, the temperature is raised to 90° C. with stirring and the reaction is continued for 8 hours, a capping agent is added, the reaction is continued for 1 hour, and after the reaction is completed, the catalyst and isopropanol are removed to obtain amino silicone oil.

[0022] Preferably, step S2 is specifically: adding secondary aminated polyetheramine, allyl epoxy polyether, polyetheramine, allyl glycidyl ether and diethylene glycol butyl ether to amino silicone oil to react at 75-85° C. for 4-6 hours, and removing diethylene glycol butyl ether after the reaction to obtain modified amino silicone oil.

[0023] Further preferably, step S2 is specifically: adding secondary aminated polyetheramine, allyl epoxy polyether, polyetheramine, allyl glycidyl ether and diethylene glycol butyl ether to amino silicone oil to react at 80°C for 5 hours, and removing diethylene glycol butyl ether after the reaction to obtain modified amino silicone oil.

[0024] In some preferred embodiments, the anionic surfactant is selected from at least one of fatty alcohol polyoxyethylene ether alkylbenzene sulfonate, ethoxylated fatty alcohol ether carboxylate, and anionic polyacrylamide, preferably anionic polyacrylamide.

[0025] In some preferred embodiments, the nonionic surfactant is selected from at least one of alkylphenol polyoxyethylene ether and fatty alcohol polyoxyethylene ether.

[0026] In some preferred embodiments, the antibacterial agent is selected from at least one of dioctadecyldimethylammonium chloride, hexadecyltrimethylammonium chloride and polyhexamethylene biguanide hydrochloride, preferably polyhexamethylene biguanide hydrochloride.

[0027] In some preferred embodiments, the pH adjuster is an inorganic acid.

[0028] Preferably, the inorganic acid is selected from at least one of formic acid, acetic acid, propionic acid, hydrochloric acid and sulfuric acid.

[0029] The second aspect of the present invention provides a method for preparing the above-mentioned silicone oil composition, comprising the following steps: slowly adding a mixture of water and a pH adjuster to the modified amino silicone oil in multiple times, adding anionic surfactants, nonionic surfactants and antibacterial agents after the addition is completed, and stirring to obtain the silicone oil composition.

[0030] Preferably, the stirring speed is 2000-3000 r / min, and the stirring time is 20-40 min.

[0031] More preferably, the stirring speed is 2500 r / min and the stirring time is 30 min.

[0032] The third aspect of the present invention provides use of the silicone oil composition in fabric treatment.

[0033] Compared with the prior art, the present invention has the following beneficial effects:

[0034] 1. The silicone oil composition prepared by the preferred formula of the present invention can give fabrics: (1) excellent hydrophilic effect; (2) excellent long-lasting hydrophilicity, and the hydrophilicity does not decrease after long-term storage; (3) soft, fluffy, and cotton-like feel; (4) low yellowing or even no yellowing properties, and can also be used on white / light-colored fabrics; (5) excellent wash resistance, and can still maintain a good feel after multiple washings;

[0035] 2. The silicone oil composition prepared by the preferred formula of the present invention has excellent stability, is safe and stable to use, and will not affect the color of dyed fabrics. DETAILED DESCRIPTION

[0036] Various exemplary embodiments of the present invention will now be described in detail. This detailed description should not be considered as limiting the present invention, but should be understood as a more detailed description of certain aspects, features, and embodiments of the present invention.

[0037] It should be understood that the terms described in the present invention are only for describing special embodiments and are not intended to limit the present invention. In addition, for the numerical range in the present invention, it should be understood that each intermediate value between the upper and lower limits of the scope is also specifically disclosed. Each smaller range between the intermediate value in any stated value or stated range and any other stated value or intermediate value in the described range is also included in the present invention. The upper and lower limits of these smaller ranges can be independently included or excluded in the scope.

[0038] Unless otherwise indicated, all technical and scientific terms used herein have the same meanings as those generally understood by those skilled in the art. Although the present invention describes only preferred methods and materials, any methods and materials similar or equivalent to those described herein may also be used in the implementation or testing of the present invention. All documents mentioned in this specification are incorporated by reference to disclose and describe the methods and / or materials associated with the documents. In the event of a conflict with any incorporated document, the content of this specification shall prevail.

[0039] It will be apparent to those skilled in the art that various modifications and variations may be made to the specific embodiments of the present invention description without departing from the scope or spirit of the present invention. Other embodiments derived from the present invention description will be apparent to those skilled in the art. The present invention description and examples are exemplary only.

[0040] The words “include,” “including,” “have,” “contain,” etc. used in this document are open-ended terms, meaning including but not limited to.

[0041] In the following examples and comparative examples, unless otherwise specified, all raw materials used were commercially available or prepared by conventional methods in the art.

[0042] The raw materials involved in the examples and comparative examples of the present invention are as follows:

[0043] The anionic polyacrylamide is Kemira surfactant A120.

[0044] The alkylphenol polyoxyethylene ether is Emulsogen LCN 287 from Clariant.

[0045] Example 1

[0046] A long-lasting hydrophilic, soft, fluffy and washable silicone oil composition, which comprises, by weight, 20 parts of modified silicone oil, 0.5 parts of anionic polyacrylamide, 0.5 parts of alkylphenol polyoxyethylene ether, 0.1 parts of polyhexamethylene biguanide hydrochloride, 0.2 parts of glacial acetic acid and 78.7 parts of water.

[0047] The modified silicone oil is composed of 20 parts of octamethylcyclotetrasiloxane, 15 parts of tetramethylethylenediamine, 5 parts of secondary aminated polyetheramine, 15 parts of allyl epoxy polyether, 11 parts of polyetheramine, 8 parts of allyl glycidyl ether, 15 parts of isopropanol, 10 parts of diethylene glycol butyl ether, 0.5 parts of end-capping agent and 0.5 parts of catalyst, calculated by mass.

[0048] The number average molecular weight of the secondary aminated polyetheramine is 400.

[0049] The number average molecular weight of the allyl epoxy polyether is 1500.

[0050] The number average molecular weight of the polyetheramine is 4000.

[0051] The end-capping agent is hexamethyldisiloxane.

[0052] The catalyst is chloroplatinic acid.

[0053] The preparation method of the above modified silicone oil is:

[0054] S1. Octamethylcyclotetrasiloxane and tetramethylethylenediamine were sequentially added into a four-necked flask equipped with a condenser, a separating funnel, a thermometer, and a nitrogen protection device. The device was sealed and nitrogen was passed through and the temperature was raised to 80°C. After keeping the temperature for 2 hours, the catalyst and isopropanol were added. After stirring and heating to 90°C for reaction for 8 hours, the end-capping agent was added and the reaction was continued for 1 hour. Finally, the catalyst was heated to 150°C to decompose the catalyst at high temperature. After cooling, the isopropanol was removed by reduced pressure distillation to obtain amino silicone oil.

[0055] S2. Add secondary aminated polyetheramine, allyl epoxy polyether, polyetheramine, allyl glycidyl ether and diethylene glycol butyl ether into a three-necked flask, protect with nitrogen, stir and heat to 80°C, keep warm for 5 hours, cool down, remove diethylene glycol butyl ether by vacuum distillation, and obtain modified amino silicone oil.

[0056] The preparation method of the above-mentioned silicone oil composition is: add modified amino silicone oil into a reaction kettle, slowly add a mixture of water and glacial acetic acid in multiple times within 40 minutes, stirring while adding, and when all the mixed liquid is dropped, add anionic polyacrylamide, alkylphenol polyoxyethylene ether and polyhexamethylene biguanide hydrochloride, and continue stirring at 2500r / min for 30 minutes to obtain the silicone oil composition.

[0057] Example 2

[0058] The only difference from Example 1 is that the long-lasting hydrophilic, soft, fluffy, and washable silicone oil composition is composed of 20 parts of modified silicone oil, 2.5 parts of anionic polyacrylamide, 0.5 parts of alkylphenol polyoxyethylene ether, 0.5 parts of polyhexamethylene biguanide hydrochloride, 0.5 parts of glacial acetic acid, and 76 parts of water, calculated by mass.

[0059] Example 3

[0060] The only difference from Example 1 is that the long-lasting hydrophilic, soft, fluffy, and washable silicone oil composition is composed of 20 parts of modified silicone oil, 0.5 parts of anionic polyacrylamide, 2 parts of alkylphenol polyoxyethylene ether, 1 part of polyhexamethylene biguanide hydrochloride, 0.5 parts of glacial acetic acid, and 76 parts of water, calculated by mass.

[0061] Example 4

[0062] The only difference from Example 1 is that the modified silicone oil, calculated by mass, consists of 15 parts of octamethylcyclotetrasiloxane, 15 parts of tetramethylethylenediamine, 16 parts of secondary aminated polyetheramine, 10 parts of allyl epoxy polyether, 10 parts of polyetheramine, 8 parts of allyl glycidyl ether, 15 parts of isopropanol, 10 parts of diethylene glycol butyl ether, 0.5 parts of end-capping agent, and 0.5 parts of catalyst; the rest are the same.

[0063] Example 5

[0064] The only difference from Example 1 is that the modified silicone oil, calculated by mass, consists of 25 parts of octamethylcyclotetrasiloxane, 10 parts of tetramethylethylenediamine, 10 parts of secondary aminated polyetheramine, 5 parts of allyl epoxy polyether, 16 parts of polyetheramine, 8 parts of allyl glycidyl ether, 15 parts of isopropanol, 10 parts of diethylene glycol butyl ether, 0.5 parts of end-capping agent, and 0.5 parts of catalyst; the rest are the same.

[0065] Comparative Example 1

[0066] The only difference from Example 1 is that the mass ratio of the secondary aminated polyetheramine, allyl epoxy polyether, polyetheramine and allyl glycidyl ether is not in the range of 0.6-2:0.6-2:1-2:1, that is, the modified silicone oil, by mass, consists of 18 parts of octamethylcyclotetrasiloxane, 15 parts of tetramethylethylenediamine, 10 parts of secondary aminated polyetheramine, 5 parts of allyl epoxy polyether, 10 parts of polyetheramine, 16 parts of allyl glycidyl ether, 15 parts of isopropanol, 10 parts of diethylene glycol butyl ether, 0.5 parts of a capping agent and 0.5 parts of a catalyst; the rest are the same.

[0067] Comparative Example 2

[0068] The only difference from Example 1 is that the mass ratio of the secondary aminated polyetheramine, allyl epoxy polyether, polyetheramine and allyl glycidyl ether is not in the range of 0.6-2:0.6-2:1-2:1, that is, the modified silicone oil, by mass, consists of 20 parts of octamethylcyclotetrasiloxane, 15 parts of tetramethylethylenediamine, 10 parts of secondary aminated polyetheramine, 10 parts of allyl epoxy polyether, 5 parts of polyetheramine, 8 parts of allyl glycidyl ether, 10 parts of isopropanol, 10 parts of diethylene glycol butyl ether, 0.5 parts of a capping agent and 0.5 parts of a catalyst; the rest are the same.

[0069] Comparative Example 3

[0070] The only difference from Example 1 is that the preparation method of the modified amino silicone oil is different. The preparation method of the modified amino silicone oil is:

[0071] S1. Octamethylcyclotetrasiloxane and tetramethylethylenediamine were added to a four-necked flask equipped with a condenser, a separating funnel, a thermometer, and a nitrogen protection device in sequence. The device was sealed and nitrogen was passed through and the temperature was raised to 60°C. After keeping the temperature for 10 hours, the catalyst and isopropanol were added. After stirring and heating to 90°C for reaction for 8 hours, the end-capping agent was added and the reaction was continued for 1 hour. Finally, the catalyst was heated to 150°C to decompose the catalyst at high temperature. After cooling, the isopropanol was removed by vacuum distillation to obtain amino silicone oil.

[0072] S2, amino silicone oil, secondary aminated polyetheramine, allyl epoxy polyether, polyetheramine, allyl glycidyl ether and diethylene glycol butyl ether were added to a three-necked flask, protected by nitrogen, heated to 70°C with stirring, and kept warm for 3 hours. After cooling, diethylene glycol butyl ether was removed by reduced pressure distillation to obtain modified amino silicone oil.

[0073] Comparative Example 4

[0074] The only difference from Example 1 is that the preparation method of the modified amino silicone oil is different. The preparation method of the modified amino silicone oil is:

[0075] S1. Octamethylcyclotetrasiloxane and tetramethylethylenediamine were added to a four-necked flask equipped with a condenser, a separating funnel, a thermometer, and a nitrogen protection device in sequence. The device was sealed and nitrogen was passed through and the temperature was raised to 70°C. After keeping the temperature for 6 hours, the catalyst and isopropanol were added. The temperature was stirred and raised to 90°C for reaction for 8 hours, and then the end-capping agent was added. The reaction was continued for 1 hour, and finally heated to 150°C to decompose the catalyst at high temperature. After cooling, the isopropanol was removed by vacuum distillation to obtain amino silicone oil.

[0076] S2. Add amino silicone oil, secondary aminated polyetheramine, allyl epoxy polyether, polyetheramine, allyl glycidyl ether and diethylene glycol butyl ether into a three-necked flask, protect with nitrogen, stir and heat to 80°C, keep warm for 5 hours, cool down, remove diethylene glycol butyl ether by vacuum distillation, and obtain modified amino silicone oil.

[0077] Comparative Example 5

[0078] The only difference from Example 1 is that the preparation method of the modified silicone oil is different. The preparation method of the modified amino silicone oil is:

[0079] S1. Octamethylcyclotetrasiloxane and tetramethylethylenediamine were added to a four-necked flask equipped with a condenser, a separating funnel, a thermometer, and a nitrogen protection device in sequence. The device was sealed and nitrogen was passed through and the temperature was raised to 80°C. After keeping the temperature for 2 hours, the catalyst and isopropanol were added. After stirring and heating to 90°C for reaction for 8 hours, the end-capping agent was added and the reaction was continued for 1 hour. Finally, the catalyst was heated to 140°C to decompose the catalyst at high temperature. After cooling, the isopropanol was removed by reduced pressure distillation to obtain amino silicone oil.

[0080] S2. Add amino silicone oil, secondary aminated polyetheramine, allyl epoxy polyether, polyetheramine, allyl glycidyl ether and diethylene glycol butyl ether into a three-necked flask, protect with nitrogen, stir and heat to 90°C, keep warm for 7 hours, cool down, remove diethylene glycol butyl ether by vacuum distillation to obtain modified amino silicone oil.

[0081] Comparative Example 6

[0082] The difference from Example 1 is that the allyl epoxy polyether is replaced by a secondary aminated polyether amine of the same mass, and the rest are the same.

[0083] Comparative Example 7

[0084] The difference from Example 1 is that the number average molecular weight of the allyl epoxy polyether is 2,500.

[0085] Comparative Example 8

[0086] The difference from Example 1 is that octamethylcyclotetrasiloxane is replaced by α,ω-dihydroxypolydimethylsiloxane of the same mass.

[0087] Comparative Example 9

[0088] The scheme of the best embodiment (embodiment 1) recorded in the Chinese patent of publication number CN117626670A, that is: a softener, by content percentage, is composed of the following components: 12 parts of tetramethyl disiloxane, 15 parts of cyclohexylmethyldimethoxysilane, 8 parts of allyl glycidyl ether, 3 parts of polyetheramine, 15 parts of isopropyl alcohol, 10 parts of diethylene glycol butyl ether, 4 parts of triethanolamine dodecylbenzenesulfonate, 2 parts of sodium lauryl sulfate (SDS), 2 parts of fatty alcohol polyoxyethylene ether, 0.2 parts of glacial acetic acid, 0.1 parts of polyhexamethylene biguanide hydrochloride, and the balance is water.

[0089] The preparation method is as follows:

[0090] (1) Tetramethyldisiloxane and cyclohexylmethyldimethoxysilane are sequentially added to a four-necked flask equipped with a condenser, a separating funnel, a thermometer, and a nitrogen protection device. After sealing the device, nitrogen is passed through and the temperature is raised to 70°C. After keeping the temperature for 2 hours, the catalyst tetramethylammonium hydroxide and the solvent dimethyl sulfoxide (DMSO) are added. After stirring and heating to 90°C for reaction for 8 hours, the end-capping agent hexamethyldisiloxane is added and the reaction is continued for 1 hour. The mass ratio of tetramethyldisiloxane, cyclohexylmethyldimethoxysilane, solvent and end-capping agent is 3:3:2, and the amount of catalyst is 0.5 parts of the total amount of tetramethyldisiloxane, end-capping agent and cyclohexylmethyldimethoxysilane. The catalyst tetramethylammonium hydroxide is heated to 135°C to decompose at high temperature. After cooling, the low-boiling substances are removed by vacuum distillation to obtain amino silicone oil.

[0091] (2) Isopropanol, allyl glycidyl ether, diethylene glycol butyl ether and polyetheramine are mixed and then dripped into a three-necked flask containing amino silicone oil, wherein the mass ratio of amino silicone oil to polyetheramine is 20:3, and nitrogen protection is adopted. The temperature is raised to 80°C with stirring, and the reaction time is 3h. Dodecylbenzenesulfonic acid triethanolamine is added, and the reaction is continued with stirring for 5h. The reaction temperature is 50°C. After cooling, small molecular weight low-boiling substances are removed by reduced pressure distillation to obtain modified amino silicone oil.

[0092] (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 the mixture is stirred at a speed of 100 r / min for 10 min, 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 min. When all the water has been dripped off, polyhexamethylene biguanide hydrochloride is added, and the speed is increased to 2500 r / min and stirring is continued for 30 min to obtain a softener.

[0093] Comparative Example 10

[0094] The scheme of the best embodiment (embodiment 1) recorded in the Chinese patent publication number CN117626670A, namely:

[0095] An ice-feeling softener comprises component 1, component 2 and component 3. The weight ratio of component 1: component 2: component 3 is 30:5:10. The components in component 1 are calculated in the following weight parts: 100 parts of double-terminal hydrogen silicone oil with a molecular weight of 2000, 15 parts of allyl polyoxyethylene polyoxypropylene epoxy polyether, 30 parts of secondary amino polyether, 2 parts of chloroplatinic acid, and 100 parts of isopropanol; the components in component 2 are calculated in the following weight parts: 100 parts of low-hydrogen silicone oil, 100 parts of allyl polyoxyethylene polyoxypropylene epoxy polyether, 2 parts of chloroplatinic acid, and 100 parts of isopropanol; the components in component 3 are calculated in the following weight parts: 50 parts of fatty alcohol polyoxyethylene ether, 100 parts of polyether polyol, and 15 parts of water-soluble polyurethane.

[0096] The specific preparation method is as follows: allyl polyoxyethylene polyoxypropylene epoxy polyether, chloroplatinic acid and isopropanol are mixed and heated to 60°C, double-end hydrogen silicone oil is added, the temperature is raised to 90°C, the reaction is carried out for 5 hours, the solvent and unreacted products are removed by vacuum, the mixture is cooled to room temperature, secondary amino polyether is added, the mixture is heated to 45°C, and the mixture is kept warm for 3 hours to obtain component 1; allyl polyethylene polyoxypropylene epoxy polyether, chloroplatinic acid and isopropanol are mixed and heated to 55°C, low hydrogen silicone oil is added, the mixture is heated to 90°C, and the reaction is carried out for 5 hours to obtain component 2; fatty alcohol polyoxyethylene ether, polyether polyol and water-soluble polyurethane are mixed and compounded to obtain component 3; component 1, component 2, component 3 and deionized water are placed in a mixer and mixed and stirred at a stirring speed of 300 r / min for 30 minutes to obtain an ice-feel softener.

[0097] Effect experiment 1: fabric feel

[0098] Working liquid pH value: 4-6; Fabric: white cotton knitted cloth;

[0099] Process: two dips and two rolls (liquid content: 75%) → shaping (160℃×90s) → hand feel evaluation

[0100] Hand feel evaluation criteria: The score is based on a 100-point system and is given by hand feel evaluation professionals. The higher the score, the better the feel, and the lower the score, the worse the feel.

[0101] The formula and results are shown in Table 1.

[0102] Table 1 Fabric feel results

[0103]

[0104]

[0105] It can be seen from Table 1 that the fabrics treated with the silicone oil compositions of Examples 1-5 of the present invention and the products of Comparative Examples 9-10 have comparable hand feel effects, and are significantly better than Comparative Examples 1-8 and representative hydrophilic silicone oils on the market.

[0106] Effect experiment 2: Long-term hydrophilicity of fabric

[0107] Working liquid pH value: 4-6; Fabric: 40×40 / 133×76 whitening cotton woven fabric;

[0108] Process: two dips and two rolls (liquid carrying rate: 65%) → shaping (160℃×90s) → testing long-term hydrophilicity

[0109] Long-term hydrophilic test standard: After the treated fabric is placed in a constant temperature and humidity environment for 3 months, the hydrophilicity of the fabric surface is tested. The hydrophilic test requires dripping water with a rubber-tipped dropper in 5 different areas of the fabric surface to test the time it takes for the water to completely penetrate the fabric surface;

[0110] The formula and results are shown in Table 2.

[0111] Table 2 Long-term hydrophilicity results of fabrics

[0112]

[0113]

[0114] As can be seen from Table 2, the hydrophilicity and long-term hydrophilicity of the fabrics treated with the silicone oil compositions of Examples 1-5 of the present invention are better than those of the silicone oil compositions of Comparative Examples 1-8 and the products of Comparative Examples 9-10, and better than the long-term hydrophilicity of representative hydrophilic silicone oils on the market.

[0115] Effect experiment 3: Fabric yellowing

[0116] Working liquid pH value: 4-6; Fabric: 40×40 / 133×76 whitening cotton woven fabric;

[0117] Process: two dips and two rolls (liquid rate: 65%) → shaping (160℃×90s) → whiteness test

[0118] Yellowing test standard: Use a fully automatic colorimeter to test the Wg value and compare it with a blank sample (original cloth). The smaller the difference, the lighter the yellowing effect.

[0119] The formula and results are shown in Table 3.

[0120] Table 3 Fabric yellowing results

[0121]

[0122]

[0123] It can be seen from Table 3 that the silicone oil compositions of Examples 1-5 of the present invention and the products of Comparative Examples 9-10 have comparable non-yellowing effects on fabrics treated therewith, and are better than Comparative Examples 1-8 and representative hydrophilic silicone oils on the market.

[0124] Effect experiment 4: fabric color change

[0125] Working liquid pH value: 4-6; Fabric: 20×16 / 128×60 blue cotton woven fabric;

[0126] Process: two dips and two rolls (liquid rate: 75%) → shaping (160℃×90s) → color change test

[0127] Color change test standard: visual inspection method, using naked eyes to compare the brightness of two pieces of fabric with and without silicone oil composition added, and the test personnel will grade the brightness of the examples before and after the processing, and the test results are grades;

[0128] The formula and results are shown in Table 4.

[0129] Table 4 Fabric color change results

[0130]

[0131]

[0132] It can be seen from Table 4 that the fabrics treated with the silicone oil compositions of Examples 1-5 of the present invention and the products of Comparative Examples 9-10 have comparable colorless light effects, and are better than Comparative Examples 1-8 and representative hydrophilic silicone oils on the market.

[0133] Effect experiment 5: Fabric fastness

[0134] Working liquid pH value: 4-6; Fabric: 20×16 / 128×60 blue cotton woven fabric;

[0135] Process: two dips and two rolls (liquid rate: 75%) → shaping (160℃×90s) → fastness test

[0136] Fastness test method: Refer to GB / T 3920-1997 dry friction method, use color fastness tester to test, the test result is grade;

[0137] The formula and results are shown in Table 5.

[0138] Table 5 Fabric fastness results

[0139]

[0140]

[0141] It can be seen from Table 5 that the fabrics treated with the silicone oil compositions of Examples 1-5 of the present invention and the products of Comparative Examples 9-10 have comparable fastness, and are better than Comparative Examples 1-8 and representative hydrophilic silicone oils on the market.

[0142] Effect experiment 6: Fabric feel and washability

[0143] Working liquid pH value: 4-6; Fabric: 20×16 / 128×60 blue cotton woven fabric;

[0144] Process: two dips and two rolls (liquid rate: 75%) → shaping (160℃×90s) → test hand feel and washability

[0145] Test method for hand feel washability: The fabric treated with the silicone oil composition is washed in a standard washing machine at 45°C with 20g of standard detergent ECE for 15 minutes each time for 30 times. The fabric after washing is then compared with the fabric treated with 10 / 20 / 30 / 40 / 50 / 60 / 70 / 80 / 90 / 100% of the dosage before washing to determine the final hand feel retention rate.

[0146] The formula and results are shown in Table 6.

[0147] Table 6 Fabric Hand Washability Results

[0148]

[0149]

[0150] It can be seen from Table 6 that the fabrics treated with the silicone oil compositions of Examples 1-5 of the present invention and the product of Comparative Example 10 have comparable wash resistance, and are better than Comparative Examples 1-9 and representative hydrophilic silicone oils on the market.

[0151] Effect Experiment 7: Stability

[0152] Stability test method: prepare the working solution, add other additives to the silicone oil composition, stir evenly and let it stand for 7 days to observe the stability;

[0153] The formula and results are shown in Table 7.

[0154] Table 7 Stability results

[0155]

[0156]

[0157] It can be seen from Table 7 that the silicone oil compositions of Examples 1-5 of the present invention have comparable stability effects to the products of Comparative Examples 9-10, and are better than Comparative Examples 1-5, Comparative Examples 7-8 and representative hydrophilic silicone oils on the market.

Claims

1. A long-lasting hydrophilic, soft, fluffy, and washable silicone oil composition, characterized in that: The raw materials include, by weight: 20 parts of modified silicone oil, 0.5-2.5 parts of anionic surfactant, 0.5-2 parts of nonionic surfactant, 0.1-1 parts of polyhexamethylene biguanide hydrochloride, 0.2-0.5 parts of glacial acetic acid, and 76-79 parts of water; The modified silicone oil comprises raw materials including: octamethylcyclotetrasiloxane, tetramethylethylenediamine, secondary aminated polyetheramine, allyl epoxy polyether, polyetheramine, allyl glycidyl ether, isopropanol, diethylene glycol butyl ether, a capping agent and a catalyst.

2. The silicone oil composition according to claim 1, characterized in that The number average molecular weight of the secondary aminated polyetheramine is 300-500.

3. The silicone oil composition according to claim 2, characterized in that The number average molecular weight of the allyl epoxy polyether is 1000-2000; the number average molecular weight of the polyether amine is 3000-5000.

4. The silicone oil composition according to claim 3, characterized in that The modified silicone oil comprises, by weight, 15-25 parts of octamethylcyclotetrasiloxane, 10-15 parts of tetramethylethylenediamine, 5-16 parts of secondary aminated polyetheramine, 5-15 parts of allyl epoxy polyether, 10-16 parts of polyetheramine, 8-16 parts of allyl glycidyl ether, 13-17 parts of isopropanol, 8-12 parts of diethylene glycol butyl ether, 0.4-0.6 parts of a capping agent, and 0.4-0.6 parts of a catalyst.

5. The silicone oil composition according to claim 4, characterized in that The mass ratio of the secondary aminated polyetheramine, allyl epoxy polyether, polyetheramine and allyl glycidyl ether is 0.6-2:0.6-2:1-2:

1.

6. The silicone oil composition according to claim 5, characterized in that The preparation method of the modified silicone oil comprises the following steps: S1. Under a nitrogen atmosphere, octamethylcyclotetrasiloxane and tetramethylethylenediamine are mixed, reacted, a catalyst and isopropanol are added, the reaction is continued, a capping agent is added, the reaction is continued, and after the reaction is completed, the catalyst and isopropanol are removed to obtain amino silicone oil; S2. Adding secondary aminated polyetheramine, allyl epoxy polyether, polyetheramine, allyl glycidyl ether and diethylene glycol butyl ether to the amino silicone oil for reaction, removing the diethylene glycol butyl ether after the reaction is completed, and obtaining modified amino silicone oil.

7. The silicone oil composition according to claim 6, characterized in that Step S1 is specifically as follows: under a nitrogen protective atmosphere, octamethylcyclotetrasiloxane and tetramethylethylenediamine are mixed, reacted at 75-85° C. for 1-3 hours, a catalyst and isopropanol are added, stirred and heated to 90-95° C. and the reaction is continued for 7-9 hours, a capping agent is added, and the reaction is continued for 0.5-1.5 hours. After the reaction is completed, the catalyst and isopropanol are removed to obtain amino silicone oil.

8. The silicone oil composition according to claim 7, characterized in that Step S2 is specifically as follows: adding secondary aminated polyetheramine, allyl epoxy polyether, polyetheramine, allyl glycidyl ether and diethylene glycol butyl ether to amino silicone oil to react at 75-85° C. for 4-6 hours, and removing diethylene glycol butyl ether after the reaction to obtain modified amino silicone oil.

9. The method for preparing the silicone oil composition according to any one of claims 1 to 8, characterized in that: The following steps are involved: A mixed solution of water and a pH adjuster is added dropwise to the modified amino silicone oil, and after the addition is completed, an anionic surfactant, a nonionic surfactant and an antibacterial agent are added, and the mixture is stirred to obtain a silicone oil composition.

10. Use of the silicone oil composition according to any one of claims 1 to 8 in fabric treatment.

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