Yellowing-free cotton-like softening agent as well as preparation method and application thereof

Abstract

The invention discloses a non-yellowing cotton-like softening agent as well as a preparation method and application thereof, and belongs to the technical field of daily chemical household products. The invention aims to solve the technical problems of serious yellowing, poor stability, smooth hand feeling and the like of a fabric in the conventional softening agent, and provides a high-stability and yellowing-free softening agent with high cotton-like feeling, so that the fabric has the characteristics of softness, fluffiness, strong cotton feeling and hand feeling, and the yellowing and color change of the fabric are basically not influenced. According to the technical scheme, the non-yellowing cotton-like softening agent is characterized in that the softening agent is prepared from octamethylcyclotetrasiloxane, dodecyl dimethyl tertiary amine, allyl polyether, a polyamine derivative, a pH regulator, an organic solvent and water.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of daily household products, in particular to a non-yellowing, cotton-like softening agent, a preparation method and application thereof. BACKGROUND

[0002] In recent years, with the improvement of people's living standards, the consumption concept of the majority of consumers has changed significantly. The requirement for wearing is not only on aesthetics, but more importantly, comfort and quality. In the future, people's requirements for comfort and quality will be higher and higher, so more functional and excellent performance products need to be continuously developed and optimized. In order to meet the needs of the consumer market, new products need to be developed to cater to the market.

[0003] Clothing accounts for a relatively high proportion of textiles. Soft, delicate, skin-friendly, and strong cotton-like hand feel style are new requirements for clothing, and more and more customers have put forward such requirements. At present, the mainstream softening agent on the market is difficult to achieve such hand feel performance. With the diversification of weaving structure of polyester, nylon and their blended fabrics, it is difficult to prepare new softening agents for high-end chemical fibers and their blended fabrics.

[0004] Among various softening agents, ordinary amino silicone oil has excellent soft and smooth hand feel, but has poor hydrophilicity, easy "yellowing", and poor emulsion stability. In block silicone oil, the introduction of hydrophilic polyether segments can increase the hydrophilicity of silicone oil and enhance the moisture absorption, antistatic property and stability of the finished fabric, but the self-crosslinking film forming ability of polyether and the combination ability with fibers are weak, and the hand feel is poor. Both kinds of silicone oil have advantages and disadvantages.

[0005] The document discloses a composition for degerming, deodorizing, and lasting fragrance and a preparation method thereof. The composition comprises water and the following components in percentage by weight: 0.1%~7% rheological agent, 0.1%~5% deodorizing agent, 0.1%~1% microcapsule fragrance agent, 0.1%~5% softening agent, 0.1%~2% bactericide, and 0.1%~5% surfactant; wherein the mass ratio of the rheological agent to the softening agent is 10:1~1:10; the rheological agent, the deodorizing agent, the bactericide, the microcapsule fragrance agent, the softening agent, and the surfactant are charge compatible. The composition can comprehensively meet the excellent degerming, deodorizing, lasting fragrance, and fabric softening effects, and has low flow viscosity.

[0006] This document, published in China (CN104328665A) on February 4, 2015, discloses a fabric softener composed of the following components by weight: 2-3 parts polyvinylpyrrolidone, 1-2 parts isopropanolamine, 4-5 parts terpineol oil, 8-9 parts alkylphenol polyoxyethylene ether, 1-2 parts hydroxypropyl methylcellulose, 6-7 parts polyethylene ether, 3-4 parts nylon oil, and 1-2 parts nonylphenol ethoxylate. This fabric softener makes fabrics soft, smooth, elastic, and abrasion-resistant.

[0007] This document, published in China (CN102199295A) on August 22, 2012, discloses a method for preparing a polyorganosiloxane amine polyether block copolymer. The method includes the preparation of α,ω-hydrosiloxane intermediates, the preparation of α,ω-diepoxy polysiloxane intermediates, and the preparation of the polyorganosiloxane amine polyether block copolymer.

[0008] The journal title is "Dyeing and Finishing Technology of Polyester Imitation Cotton Fabrics," Volume 38, Publication Date: February 4, 2013. This document discloses that softener M5402 is a linear block silicone oil used in the finishing of polyester imitation cotton fabrics, which can give the fabric a soft and fluffy feel (but slightly less smoothness), with moderate to high hydrophilicity; M-5202 is also a linear block silicone oil, with a primarily soft and smooth feel and moderate hydrophilicity; hydrophilic linear silicone oil M-5401CA does not significantly improve the feel, but can offset some of the smoothness and greatly improve the hydrophilicity of polyester imitation cotton fabrics, achieving instant hydrophilicity; cotton softener M-40 primarily provides a fluffy and elastic feel, can offset some of the smoothness, and has a hydrophilicity time of less than 3 seconds.

[0009] The prior art represented by the aforementioned documents has at least the following unresolved technical problems or defects: (1) After softening polyester and nylon fabrics, the fabric surface is oily and has a strong chemical fiber feel, poor skin feel, and cannot achieve the feel and style of cotton fabrics. The relevant evidence is: Publication No. CN102199295A, which is a "polyorganosiloxane-amine polyether block copolymer". The main chain is mainly composed of siloxane and polyether chains, lacking functional groups that form "cotton fiber hydrogen bonding" with the fiber. Due to the lubricating effect of the heavy siloxane chain, the final result is the typical "slippery and elastic feel" of organosilicon softeners.

[0010] (2) The fabric yellowed severely after treatment, which greatly reduced the service life and sales price of the final garment. The relevant evidence is: Publication No. CN102199295A. The terminal amine polyether used in this literature contains amino functional groups. Although it is a block structure, there is still a possibility of trace oxidation and yellowing.

[0011] (3) Insufficient product stability increases the risk of process production. The relevant evidence is: Publication No. CN102199295A. The stability test in this literature only includes conventional conditions (such as centrifugation at 3000r / min, pH=2-12, and 500ppm hard water), and does not verify extreme scenarios such as "high shear, high temperature setting, and high concentration of additives in the finishing of chemical fiber fabrics". Summary of the Invention

[0012] The purpose of this invention is to provide: A non-yellowing, cotton-like softener, and related technologies, to solve technical problems such as improving the softness, fluffiness, and cotton-like feel of fabrics and avoiding yellowing and discoloration, or combinations thereof.

[0013] Terminology Explanation: Unless otherwise defined, all technical terms used herein have the same meanings as commonly understood by one of ordinary skill in the art to which this subject matter pertains. Unless otherwise stated, all patents, patent inventions, and disclosures cited throughout this document are incorporated herein by reference in their entirety. Where multiple definitions exist for terms herein, the definitions provided in this chapter shall prevail.

[0014] It should be understood that the above brief description and the following detailed description are exemplary and for illustrative purposes only, and do not limit the subject matter of the invention in any way. In this invention, the singular is used in conjunction with the plural unless otherwise specifically stated. It should also be noted that, unless otherwise stated, the use of “or” or “or” means “and / or”. Furthermore, the use of the term “comprising” and other forms such as “including,” “containing,” and “contains” are not limiting.

[0015] Definitions of standard chemical terms can be found in references such as QB / T4535-2013 "Fabric Softeners", "Complete Guide to Formulations of Daily Chemical Products", and "Application of Ester-based Quaternary Ammonium Salts in Civil Softeners".

[0016] Unless otherwise stated, conventional methods within the scope of the art, such as refractive index testing, viscosity testing, and fabric phenolic yellowing testing, shall be used.

[0017] Unless specifically defined herein, the use of all commercially available products herein employs standard techniques. For example, it may be carried out using the manufacturer's instructions for use with the kit, or in accordance with methods known in the art or the description of this invention. The techniques and methods described herein can generally be implemented according to conventional methods well known in the art, based on the descriptions in the various summary and more specific documents cited and discussed in this specification.

[0018] The term "softener" used in this article refers to a class of chemical auxiliaries used in the finishing of textiles. Its core function is to form a lubricating film on the fiber surface, reduce the coefficient of friction between fibers, and give the fabric a soft, fluffy, and smooth feel. At the same time, it improves antistatic properties, washability, and skin-friendliness. It is widely used in clothing, home textiles, industrial textiles and other fields.

[0019] The term "octamethylcyclotetrasiloxane" as used in this article refers to a cyclic organosilicon monomer (molecular structure: (CH3)4Si4O4), which is a core raw material for the preparation of organosilicon fabric softeners. It can undergo ring-opening polymerization under the action of a catalyst to form a linear siloxane chain, providing the core softening properties of the softener, such as slipperiness and wash resistance. A purity of ≥99% and a water content of ≤0.1% are required.

[0020] The term "dodecyl dimethyl tertiary amine" as used in this article refers to: a long-chain alkyl tertiary amine (molecular structure: C 12 H 25 N(CH3)3, in fabric softener, has both emulsifying and modifying functions. It can be protonated to form cationic emulsion intermediates, enhancing the compatibility between the oil phase (such as silicone oil) and the aqueous phase, while also improving the adsorption of the softener to the fiber and improving wash resistance.

[0021] The term "allyl polyether" as used in this article refers to a nonionic compound with allyl (-CH2CH=CH2) groups at the molecular end and a polyoxyethylene / polyoxypropylene ether bond in the main chain, possessing both emulsifying and silicone oil modifying functions. It can undergo addition reactions with organosilicon chains to introduce hydrophilic polyether segments, thereby improving the hydrophilicity and emulsion stability of the softener and preventing the fabric from feeling oily.

[0022] The term "polyamine derivatives" as used in this article refers to polymer-modified products containing multiple amino groups (-NH2, -NH-) (such as polyethylene polyamine alkylbenzene sulfonates and resin block polyetheramines), which are used in softeners to enhance the elastic bond between fibers, improve fabric bulk and washability, and also help improve hydrophilicity and antistatic properties.

[0023] The term "pH adjuster" used in this article refers to chemical additives used to adjust the pH value of softener systems. These are divided into two categories: acidic (such as acetic acid and citric acid) and weakly basic (such as triethanolamine and sodium carbonate). Their core function is to stabilize the emulsion system and prevent ester bond hydrolysis or fiber damage. The system pH is typically controlled between 6.5 and 7.5 (weakly acidic to neutral).

[0024] The term "nonionic surfactant" as used in this article refers to emulsifiers (such as AEO series, Span / Tween series, and alkyl glycosides) whose molecules do not carry a charge and contain hydrophilic polyether chains (-O-CH2CH2-) and hydrophobic alkyl chains. In softeners, they are used to reduce oil-water interfacial tension, synergistically with cationic surfactants to emulsify silicone oils, improve emulsion stability, and reduce irritation.

[0025] The term "cationic surfactant" as used in this article refers to positively charged surface-active substances (such as ester-based quaternary ammonium salts, alkyl trimethyl quaternary ammonium salts, and imidazoline-type quaternary ammonium salts), which are the core active ingredients of fabric softeners. They can strongly bind to negatively charged fibers through electrostatic adsorption to form a lubricating layer, giving fabrics softness and antistatic properties, and are suitable for various fabrics such as cotton, chemical fibers, and protein fibers.

[0026] The term "antibacterial / bacteriostatic agent" as used in this article refers to auxiliaries used to inhibit the growth of bacteria and mold in fabrics or fabric softener systems (such as dodecyl dimethyl benzyl ammonium chloride, polyhexamethylene guanidine hydrochloride, and organosilicon quaternary ammonium salts). They must be compatible with fabric softener systems, effective at low concentrations, and cause no damage to fabrics or irritation to the human body, making them suitable for intimate apparel or public textiles.

[0027] The term "aminosilane coupling agent" as used in this article refers to organosilicon compounds (such as KH550 and KH792) whose molecules simultaneously contain amino groups (-NH2, -NH-) and hydrolyzable siloxane groups (-Si(OR)3). In bulk polymerization, the siloxane groups polymerize with the silicone oil chain, and the amino groups react with the hydroxyl / carboxyl groups of the fibers to form chemical bridges between the silicone oil and the fibers, thereby improving the wash resistance and hand feel uniformity of the fabric softener.

[0028] The term "capping agent" used in this article refers to a key additive (such as hexamethyldisiloxane MM and trimethylethoxysilane TMES) that controls the molecular weight of silicone oil. By binding to the active sites at the ends of siloxane chains, it terminates the polymerization reaction, fixes the silicone oil chain length, avoids emulsion stratification or a stiff feel caused by excessively large molecular weight, and precisely controls the viscosity of silicone oil.

[0029] The term "emulsification" as used in this article refers to the process of uniformly dispersing an oil phase (such as silicone oil or cationic surfactants) in an aqueous phase to form a stable O / W (oil-in-water) emulsion. Phase inversion emulsification is commonly used in softener preparation. This method breaks up oil phase droplets through high-speed shearing, dispersing the oil phase as tiny particles (1~10 μm) in the aqueous phase to ensure product stability.

[0030] The term "mixing" as used in this article refers to the process of uniformly dispersing different materials (such as monomers, additives, and oil / water phases) through mechanical stirring, gas purging, or other methods. This process runs throughout the entire softener preparation process, including raw material mixing during bulk polymerization, oil-water phase mixing during emulsification, and gentle mixing during compound addition. The core objective is to ensure material homogeneity.

[0031] The term "compounding" as used in this article refers to the process of mixing two or more raw materials with different functions (such as cationic and nonionic surfactants, silicone oil and polyamine derivatives, softening ingredients and antibacterial agents) in a certain proportion to achieve synergistic effects. Softeners, through compounding, optimize their overall performance, including hand feel, stability, and antibacterial properties, to meet the needs of different fabrics.

[0032] The term "bulk polymerization" as used in this article refers to the reaction in which monomers (such as D4) are directly polymerized under the action of a catalyst to form polymers (such as silicone oil) in the absence of solvents or with a small amount of solvent.

[0033] The term "homogenization and refinement" used in this article refers to the further processing of the emulsified coarse emulsion to refine the particle size of the oil phase droplets. High-pressure homogenizers (20~30MPa pressure) or colloid mills are commonly used to refine the coarse emulsion particle size from 1~10μm to 0.1~5μm, thereby improving emulsion stability, preventing stratification and emulsion breakage during storage or use, and ensuring a uniform fabric hand feel.

[0034] In a first aspect, the present invention provides: a non-yellowing, cotton-like softener, wherein the softener comprises octamethylcyclotetrasiloxane, dodecyl dimethyl tertiary amine, allyl polyether, polyamine derivatives, pH adjuster, organic solvent and water.

[0035] The technical features include: octamethylcyclotetrasiloxane, dodecyl dimethyl tertiary amine, allyl polyether, polyamine derivatives, pH adjuster, and organic solvent.

[0036] The polyamine derivative is selected from at least one of polyethylene polyamine alkylbenzene sulfonate amine, alkyl polyoxyethylene ether quaternary ammonium salt, and resin block polyether amine; The polyamine derivative is preferably at least one of alkyl polyoxyethylene ether quaternary ammonium salt and resin block polyether amine; The polyamine derivative is further preferably a resin-block polyetheramine; The pH adjuster is at least one of organic alkaline substances and inorganic alkaline substances; The pH adjuster is preferably at least one of acetic acid, sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, triethanolamine, diethanolamine, tetramethylammonium hydroxide, and morpholine. The pH adjuster is further preferably at least one of acetic acid, sodium hydroxide, sodium carbonate, sodium bicarbonate, triethanolamine, diethanolamine, and tetramethylammonium hydroxide; The pH adjuster is more preferably acetic acid; The water includes, but is not limited to, at least one of distilled water, mineral water, drinking water, purified water, tap water, deionized water, and ultrapure water; The water is preferably deionized water; The organic solvent is at least one selected from isopropanol, toluene, ethylene glycol monobutyl ether, and diethylene glycol monobutyl ether. The organic solvent is preferably at least one of isopropanol, ethylene glycol monobutyl ether, and diethylene glycol monobutyl ether; the organic solvent is more preferably isopropanol. Preferably, the softener further comprises cationic surfactants, nonionic surfactants, and antibacterial / bacteriostatic agents; More preferably, the cationic surfactant is selected from at least one of octadecyltrimethylammonium chloride, hexadecyltrimethylammonium chloride, dodecyltrimethylammonium chloride, dodecyldimethylbenzylammonium chloride, and distearate ethyl glycidyl quaternary ammonium chloride; More preferably, the cationic surfactant is distearate ethyl glycidyl quaternary ammonium salt; More preferably, the nonionic surfactant is at least one of fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, and sorbitan ester and its polyoxyethylene ether; For example, the fatty alcohol polyoxyethylene ether is selected from at least one of AEO-3, AEO-7 and AEO-9; The alkylphenol polyoxyethylene ether is selected from at least one of TX-10, TX-7, and TX-8; The sorbitan ester and its polyoxyethylene ether are selected from at least one of sorbitan monostearate and polysorbate 85; More preferably, the nonionic surfactant is a fatty alcohol polyoxyethylene ether; More preferably, the antibacterial / bacteriostatic agent is at least one of quaternary ammonium salt antibacterial agents, organosilicon quaternary ammonium salts, natural antibacterial agents, and thiazolinones; More preferably, the antibacterial / bacteriostatic agent is a quaternary ammonium salt antibacterial agent; More preferably, the antibacterial / bacteriostatic agent is at least one of dodecyl dimethyl benzyl ammonium chloride and polyhexamethylene guanidine hydrochloride; Most preferably, the antibacterial / bacteriostatic agent is dodecyl dimethyl benzyl ammonium chloride.

[0037] Preferably, the softener comprises, by weight, 20-30 parts octamethylcyclotetrasiloxane, 2-4 parts dodecyl dimethyl tertiary amine, 2-4 parts allyl polyether, 0.5-2 parts polyamine derivative, 0.5-1 part pH adjuster, 5-10 parts organic solvent and 49-70 parts water; For example, the ingredients of the softener, by weight, include: 20-25 parts, 25-30 parts, 21-29 parts, 22-28 parts, 23-27 parts, 24-26 parts, 25-29 parts, 23-26 parts, 20-21 parts or 22-25 parts of octamethylcyclotetrasiloxane; 2-3 parts, 3-4 parts, or 2-4 parts of dodecyl dimethyl tertiary amine; 2-3 parts, 3-4 parts, or 2-4 parts allyl polyether; 0.5-1 part, 0.5-1.5 part, 1-1.5 part, 1-2 part, 1.5-2 part, 1.1-2 part or 0.7-2 part of polyamine derivatives; 5-9 parts, 6-9 parts, 6-8 parts, 7-8 parts, 6-9 parts, 6-10 parts, or 7-9 parts of organic solvent; And 49-55, 60-70, 60-65, 58-62, 68-70, 55-70 or 56-68 parts water; As a further example, the ingredients of the softener, by weight, include: 20, 21, 22, 23, 24, 25, 26, 27, 28, 29 or 30 parts of octamethylcyclotetrasiloxane; 2, 3, or 4 parts of dodecyl dimethyl tertiary amine; 2 parts, 3 parts, or 4 parts of allyl polyether; 0.5 parts, 0.6 parts, 0.7 parts, 0.8 parts, 0.9 parts, 1 part, 1.5 parts, or 2 parts of polyamine derivatives; 0.5 parts, 0.6 parts, 0.7 parts, 0.8 parts, 0.9 parts, or 1 part of pH adjuster; 5, 6, 7, 8, 9, or 10 parts of organic solvent; And 49, 50, 55, 60, 65, or 70 portions of water; More preferably, the softener comprises, by weight, 20-30 parts octamethylcyclotetrasiloxane, 2-4 parts dodecyl dimethyl tertiary amine, 2-4 parts allyl polyether, 0.5-2 parts polyamine derivative, 0-1 part cationic surfactant, 0-3 parts nonionic surfactant, 0-0.5 parts antibacterial / bacteriostatic agent, 0.5-1 part pH adjuster, 5-10 parts organic solvent, and 44.5-70 parts water; For example, the ingredients of the softener, by weight, include: 20-25 parts, 25-30 parts, 21-29 parts, 22-28 parts, 23-27 parts, 24-26 parts, 25-29 parts, 23-26 parts, 20-21 parts or 22-25 parts of octamethylcyclotetrasiloxane; 2-3 parts, 3-4 parts, or 2-4 parts of dodecyl dimethyl tertiary amine; 2-3 parts, 3-4 parts, or 2-4 parts allyl polyether; 0.5-1 part, 0.5-1.5 part, 1-1.5 part, 1-2 part, 1.5-2 part, 1.1-2 part or 0.7-2 part of polyamine derivatives; 0.5-0.9 parts, 0.6-0.8 parts, 0.7-0.8 parts, 0.9-1 part, 0.5-0.8 parts, or 0.7-0.9 parts of cationic surfactant; 2-2.5 parts, 2.5-3 parts, 2.1-2.9 parts, 2.2-2.8 parts, 2.3-2.7 parts, 2.4-2.6 parts, or 2.1-2.8 parts of nonionic surfactant; 0.1-0.5 parts, 0.1-0.4 parts, 0.2-0.3 parts, 0.3-0.5 parts, 0.4-0.5 parts, 0.3-0.4 parts or 0.2-0.5 parts of antibacterial / bacteriostatic agent; 0.5-0.9 parts, 0.6-0.8 parts, 0.7-0.8 parts, 0.9-1 part, 0.5-0.8 parts, or 0.7-0.9 parts pH adjuster; 5-9 parts, 6-9 parts, 6-8 parts, 7-8 parts, 6-9 parts, 6-10 parts, or 7-9 parts of organic solvent; And 44.5-72 parts, 60-70 parts, 60-65 parts, 58-62 parts, 68-70 parts, 55-70 parts or 56-68 parts of water; As a further example, the ingredients of the softener, by weight, include: 20, 21, 22, 23, 24, 25, 26, 27, 28, 29 or 30 parts of octamethylcyclotetrasiloxane; 2, 3, or 4 parts of dodecyl dimethyl tertiary amine; 2 parts, 3 parts, or 4 parts of allyl polyether; 0.5 parts, 0.6 parts, 0.7 parts, 0.8 parts, 0.9 parts, 1 part, 1.5 parts, or 2 parts of polyamine derivatives; 0.5 parts, 0.6 parts, 0.7 parts, 0.8 parts, 0.9 parts, or 1 part of cationic surfactant; 2 parts, 2.1 parts, 2.2 parts, 2.3 parts, 2.4 parts, 2.5 parts, 2.6 parts, 2.7 parts, 2.8 parts, 2.9 parts, or 3 parts of nonionic surfactant; 0.1, 0.2, 0.3, 0.4, or 0.5 parts of antibacterial / bacteriostatic agent; 0.5 parts, 0.6 parts, 0.7 parts, 0.8 parts, 0.9 parts, or 1 part of pH adjuster; 5, 6, 7, 8, 9, or 10 parts of organic solvent; And 44.5, 44.6, 44.7, 44.8, 44.9, 45, 50, 55, 60, 65, or 70 parts water; More preferably, the softener comprises, by weight, 25 parts octamethylcyclotetrasiloxane, 3 parts dodecyl dimethyl tertiary amine, 3 parts allyl polyether, 1 part polyamine derivative, 0.8 parts cationic surfactant, 2.5 parts nonionic surfactant, 0.3 parts antibacterial / bacteriostatic agent, 0.8 parts pH adjuster, 8 parts organic solvent and 55.6 parts water.

[0038] Based on further solutions to the technical problems of the present invention, or simultaneous solutions to multiple technical problems, the preferred solution in the technical solution provided in the first aspect of the present invention includes: The first preferred option is that the polyamine derivative is selected from at least one of polyethylene polyamine alkylbenzene sulfonate amine, alkyl polyoxyethylene ether quaternary ammonium salt, and resin block polyether amine; preferably at least one of alkyl polyoxyethylene ether quaternary ammonium salt and resin block polyether amine; more preferably resin block polyether amine. This technical solution, while addressing the technical problem of "improving the softness and fluffiness of fabrics and avoiding yellowing and discoloration," further addresses the technical problem of "further improving the softness and fluffiness of fabrics and avoiding yellowing and discoloration."

[0039] The second preferred embodiment: the pH adjuster is at least one of organic alkaline substances and inorganic alkaline substances; preferably at least one of acetic acid, sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, triethanolamine, diethanolamine, tetramethylammonium hydroxide, and morpholine; further preferably at least one of acetic acid, sodium hydroxide, sodium carbonate, sodium bicarbonate, triethanolamine, diethanolamine, and tetramethylammonium hydroxide; and even more preferably acetic acid. This technical solution, while addressing the technical problem of "improving the softness and fluffiness of fabrics and preventing yellowing and discoloration," further addresses the technical problem of "further improving the softness and fluffiness of fabrics and preventing yellowing and discoloration."

[0040] The third preferred embodiment: Preferably, the softener further comprises a cationic surfactant, a nonionic surfactant, and an antibacterial / bacteriostatic agent; the cationic surfactant is selected from at least one of octadecyltrimethylammonium chloride, hexadecyltrimethylammonium chloride, dodecyltrimethylammonium chloride, dodecyldimethylbenzylammonium chloride, and disteaamide ethyl glycidyl quaternary ammonium chloride; more preferably, the cationic surfactant is disteaamide ethyl glycidyl quaternary ammonium chloride. This technical solution, while addressing the technical problem of "improving the softness and fluffiness of fabrics and preventing yellowing and discoloration," further solves the technical problem of "further improving the softness and fluffiness of fabrics and preventing yellowing and discoloration."

[0041] The fourth preferred option is that the nonionic surfactant is at least one of fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, and sorbitan ester and its polyoxyethylene ether; more preferably, the nonionic surfactant is fatty alcohol polyoxyethylene ether. This technical solution, while addressing the technical problem of "improving the softness and fluffiness of fabrics and preventing yellowing and discoloration," further addresses the technical problem of "further improving the softness and fluffiness of fabrics and preventing yellowing and discoloration."

[0042] The fifth preferred option is that the antibacterial / bacteriostatic agent is at least one of quaternary ammonium salt antibacterial agents, organosilicon quaternary ammonium salts, natural antibacterial agents, and thiazolinones; preferably a quaternary ammonium salt antibacterial agent; further preferably at least one of dodecyl dimethyl benzyl ammonium chloride and polyhexamethylene guanidine hydrochloride; and even more preferably dodecyl dimethyl benzyl ammonium chloride. This technical solution, while addressing the technical problem of "improving the softness and fluffiness of fabrics and avoiding yellowing and discoloration," further addresses the technical problem of "further improving the softness and fluffiness of fabrics and avoiding yellowing and discoloration."

[0043] The sixth preferred embodiment: the softener, by weight, comprises 20-30 parts octamethylcyclotetrasiloxane, 2-4 parts dodecyl dimethyl tertiary amine, 2-4 parts allyl polyether, 0.5-2 parts polyamine derivative, 0-1 part cationic surfactant, 0-3 parts nonionic surfactant, 0-0.5 parts antibacterial / bacteriostatic agent, 0.5-1 part pH adjuster, 5-10 parts organic solvent, and 44.5-70 parts water; preferably, the softener, by weight, comprises 25 parts octamethylcyclotetrasiloxane, 3 parts dodecyl dimethyl tertiary amine, 3 parts allyl polyether, 1 part polyamine derivative, 0.8 parts cationic surfactant, 2.5 parts nonionic surfactant, 0.3 parts antibacterial / bacteriostatic agent, 0.8 parts pH adjuster, 8 parts organic solvent, and 55.6 parts water. This technical solution, having already addressed the technical problem of "improving the softness and fluffiness of fabrics and preventing yellowing and discoloration," further addresses the technical problem of "further improving the softness and fluffiness of fabrics and preventing yellowing and discoloration."

[0044] Secondly, the present invention provides a method for preparing the softener, comprising the steps of: (1) Bulk polymerization: Octamethylcyclotetrasiloxane, aminosilane coupling agent, capping agent, catalyst and organic solvent are reacted to obtain silicone oil-based polymer; (2) Emulsification stage: The silicone oil-based polymer obtained in step (1) is mixed with cationic surfactant and nonionic surfactant and emulsified to obtain an emulsion; (3) Compounding adjustment: The emulsion obtained in step (2) is mixed with dodecyl dimethyl tertiary amine, allyl polyether and polyamine derivative to obtain a compound emulsion; (4) System adjustment: The compound emulsion obtained in step (3) is mixed with pH adjuster and water to obtain the softener.

[0045] The technical features include: aminosilane coupling agent, end-capping agent, catalyst, emulsification, mixing, and compounding.

[0046] The aminosilane coupling agent is selected from at least one of γ-aminopropyltriethoxysilane, N-β-aminoethyl-γ-aminopropyltrimethoxysilane, N-β-aminoethyl-γ-aminopropylmethyldimethoxysilane, and γ-ureopropyltriethoxysilane. The aminosilane coupling agent is preferably at least one of γ-aminopropyltriethoxysilane and N-β-aminoethyl-γ-aminopropyltrimethoxysilane; The aminosilane coupling agent is further preferably γ-aminopropyltriethoxysilane; The end-capping agent is selected from at least one of hexamethyldisiloxane, trimethylethoxysilane, dimethylvinylchlorosilane, and trimethylchlorosilane; The sealing agent is preferably hexamethyldisiloxane; The catalyst is selected from at least one of tetramethylammonium hydroxide, potassium hydroxide, potassium silanolate, sulfuric acid, and trifluoromethanesulfonic acid; The catalyst is preferably at least one of tetramethylammonium hydroxide and potassium hydroxide; The catalyst is further preferably tetramethylammonium hydroxide; Preferably, the bulk polymerization in step (1) is carried out under nitrogen protection; More preferably, the bulk polymerization in step (1) is carried out under dry nitrogen protection; Preferably, the reaction conditions in step (1) are: a reaction temperature of 100-130℃ and a reaction time of 3-6h; More preferably, the reaction conditions are: a reaction temperature of 110-130℃ and a reaction time of 4-6 hours; More preferably, the reaction conditions are: a reaction temperature of 120°C and a reaction time of 5 hours; Preferably, the reaction endpoint in step (1) is a system viscosity in the range of 2000-10000 mPa or a refractive index in the range of 1.400-1.410; Preferably, after the reaction in step (1) is completed, a purification operation is also included; More preferably, the purification is selected from at least one of vacuum distillation, acid washing and neutralization, alkali washing and neutralization, molecular distillation, filtration, and adsorption, and the purification path is selected according to the type of silicone oil polymerization; More preferably, the purification path is vacuum distillation → acid washing and neutralization → activated carbon adsorption → filtration; More preferably, the reaction conditions for vacuum distillation are: reaction temperature of 150-180℃, vacuum degree of -0.09~-0.1MPa, and reaction time of 1-2h.

[0047] The reaction conditions for acid washing and neutralization are as follows: dilute acid (such as H2SO4), heating (80°C), multi-stage washing, and neutralization to neutral (pH=6-7). Preferably, the mixing sequence in step (2) is as follows: the silicone oil-based polymer obtained in step (1) is first mixed with a portion of the cationic surfactant and nonionic surfactant to obtain an oil phase system; the remaining cationic surfactant and nonionic surfactant are mixed with water to obtain an aqueous phase system. More preferably, the mixing sequence is to slowly add the aqueous phase system to the oil phase system; More preferably, the mixing temperature for preparing the oil phase system is 50~60℃; More preferably, the mixing temperature for preparing the aqueous system is 50~60℃; More preferably, the aqueous system further comprises an antibacterial / bacteriostatic agent; The mixing method described in step (2) includes, but is not limited to, at least one of stirring mixing, high-speed shear mixing, and colloid mill mixing; The preferred mixing method in step (2) is high-speed shear mixing; The mixing method described in step (2) is further preferably high-speed shear mixing, with a rotation speed of 2000~3000 r / min; Preferably, step (2) further includes a homogenization and refining operation after emulsification; More preferably, the homogenization and refining method includes, but is not limited to, at least one of high-pressure homogenization and colloid mill grinding. More preferably, the homogenization and refining method is high-pressure homogenization; Most preferably, the pressure at which the high-pressure homogenizer refines the homogenizer is 20~30MPa; The mixing method described in step (3) includes, but is not limited to, at least one of stirring mixing, high-speed shear mixing, and colloid mill mixing; The preferred mixing method in step (3) is stirring. The mixing method described in step (3) is further preferably a stirring and mixing process at a speed of 100~200 r / min; Preferably, step (3) further includes a step of cooling the system before mixing; More preferably, the system is cooled to 30~40℃; Preferably, in step (4), the pH of the system is adjusted to 6.5-7.5 by adding a pH adjuster; The mixing method described in step (4) includes, but is not limited to, at least one of stirring mixing, high-speed shear mixing, and colloid mill mixing; The preferred mixing method in step (4) is stirring. The mixing method described in step (4) is further preferably a stirring and mixing process at a rotation speed of 100~200 r / min; Preferably, the mixing operation in step (4) further includes a filtering step; More preferably, the filtration method includes, but is not limited to, at least one of mesh filtration, precision filtration, plate and frame filtration, and vacuum filtration; More preferably, the filtration method is mesh filtration; Most preferably, the filtration method is filtration using a 100-200 mesh filter.

[0048] Preferably, the method for preparing the softener includes the following steps: (1) Bulk polymerization: Under dry nitrogen protection, octamethylcyclotetrasiloxane, aminosilane coupling agent, capping agent, catalyst and organic solvent are mixed and heated to 100-130℃ for 3-6 hours. The reaction endpoint is monitored by measuring refractive index or viscosity. After the reaction is completed, the temperature is raised to 150-180℃, the vacuum degree is -0.09~-0.1MPa, and the reaction time is 1-2 hours. Low-boiling substances are removed and the catalyst is destroyed under vacuum to obtain silicone oil-based polymer. (2) Emulsification stage: The silicone oil base polymer obtained in step (1) is mixed with some cationic surfactants and nonionic surfactants at a temperature of 50~60℃ to obtain an oil phase system; the remaining cationic surfactants and nonionic surfactants are mixed with water and antibacterial / bacteriostatic agents at a temperature of 50~60℃ to obtain an aqueous phase system; the aqueous phase system is slowly added to the oil phase system under high-speed shearing at a speed of 2000~3000r / min to obtain a crude emulsion; (3) Homogenization and refinement: The crude emulsion obtained in step (2) is homogenized and refined in a high-pressure homogenizer at a pressure of 20~30MPa to obtain an emulsion; (4) Compounding adjustment: The emulsion system obtained in step (3) is cooled to 30~40℃ and mixed with dodecyl dimethyl tertiary amine, allyl polyether and polyamine derivatives to obtain a compound emulsion; (5) System adjustment: Mix the compound emulsion obtained in step (4) with a pH adjuster to adjust the pH to 6.5~7.5, then mix with water and filter through a 100-200 mesh filter to obtain the softener.

[0049] Based on further solutions to the technical problems of the present invention, or simultaneous solutions to multiple technical problems, the preferred solution in the technical solution provided in the second aspect of the present invention includes: The first preferred option is that the sealing agent is selected from at least one of hexamethyldisiloxane, trimethylethoxysilane, dimethylvinylchlorosilane, and trimethylchlorosilane; preferably hexamethyldisiloxane. This technical solution, while addressing the technical problem of "improving the softness and fluffiness of the fabric and preventing yellowing and discoloration," further solves the technical problem of "further improving the softness and fluffiness of the fabric and preventing yellowing and discoloration."

[0050] The second preferred option is that the catalyst is selected from at least one of tetramethylammonium hydroxide, potassium hydroxide, potassium silanolate, sulfuric acid, and trifluoromethanesulfonic acid; preferably at least one of tetramethylammonium hydroxide and potassium hydroxide; and more preferably tetramethylammonium hydroxide. This technical solution, while addressing the technical problem of "improving the softness and fluffiness of fabrics and preventing yellowing and discoloration," further addresses the technical problem of "further improving the softness and fluffiness of fabrics and preventing yellowing and discoloration."

[0051] The third preferred option is as follows: the reaction conditions in step (1) are: a reaction temperature of 100-130℃ and a reaction time of 3-6h; preferably: a reaction temperature of 110-130℃ and a reaction time of 4-6h; and even more preferably: a reaction temperature of 120℃ and a reaction time of 5h. This technical solution, while solving the technical problem of "improving the softness and fluffiness of the fabric and avoiding yellowing and discoloration", further solves the technical problem of "further improving the softness and fluffiness of the fabric and avoiding yellowing and discoloration".

[0052] The fourth preferred option: The mixing sequence in step (2) is as follows: the silicone oil-based polymer obtained in step (1) is first mixed with a portion of the cationic surfactant and nonionic surfactant to obtain an oil phase system; the remaining cationic surfactant and nonionic surfactant are mixed with water to obtain an aqueous phase system; preferably, the mixing sequence is to slowly add the aqueous phase system to the oil phase system; more preferably, the mixing temperature for preparing the oil phase system is 50~60℃; more preferably, the mixing temperature for preparing the aqueous phase system is 50~60℃; more preferably, the aqueous phase system also contains an antibacterial / bacteriostatic agent; the mixing method in step (2) includes, but is not limited to, at least one of stirring mixing, high-speed shear mixing, and colloid mill mixing; preferably, high-speed shear mixing; more preferably, high-speed shear mixing with a rotation speed of 2000~3000 r / min. This technical solution, based on solving the technical problem of "improving the softness and fluffiness of the fabric and avoiding yellowing and discoloration", further solves the technical problem of "further improving the softness and fluffiness of the fabric and avoiding yellowing and discoloration".

[0053] Thirdly, the present invention provides the application of the softener in the washing and care of textiles.

[0054] This includes technical features: textile washing and care, and applications.

[0055] The textiles include, but are not limited to, at least one of cotton / linen fabrics, silk / wool fabrics, polyester, nylon, acrylic, and blended fabrics; The textile is preferably at least one of cotton / linen fabric, silk / wool fabric, and polyester; The textile is further preferably polyester; Preferably, the application is as follows: it is suitable for polyester and blended fabrics, which can improve the stiffness of clothes after washing, reduce wrinkles, improve wearing comfort, and reduce the problem of static electricity attracting dust; it can give the fabric an excellent soft, fluffy and delicate hand feel, and can achieve the hand feel style of cotton fabrics; it has virtually no impact on the whiteness, color and color fastness of textiles, and is particularly suitable for use on white / light-colored fabrics and chemical fiber fabrics with high fastness requirements.

[0056] Examples 1-7 of this invention at least support the protection scope of technical features such as "polyamine derivatives", "organic solvents", and "pH adjusters".

[0057] The technical feature “polyamine derivatives” is summarized from the aforementioned explanation and / or the corresponding technical features in Examples 1-7, such as “20 parts by weight of octamethylcyclotetrasiloxane, 2 parts by weight of dodecyl dimethyl tertiary amine, 2 parts by weight of allyl polyether, 0.5 parts by weight of polyethylene polyamine alkylbenzene sulfonate amine, 0.5 parts by weight of acetic acid, 5 parts by weight of isopropanol and 70 parts by weight of water”, and “the polyamine derivatives are selected from at least one of polyethylene polyamine alkylbenzene sulfonate amine, alkyl polyoxyethylene ether quaternary ammonium salt, and resin block polyether amine”, through the common feature “polymer modified products containing multiple amino groups (-NH2, -NH-). Therefore, those skilled in the art can reasonably presume that the technical feature "polyamine derivative", its subordinate concepts, its substantially equivalent technical means, and technical means that can replace "polyamine derivative" based on existing technical levels and conventional technical means and common knowledge should all fall within the protection scope of the technical feature "polyamine derivative". For example, replacing "polyamine derivative" with "polyethylene polyamine alkylbenzene sulfonate amine" while keeping other technical features unchanged still falls within the protection scope of this invention.

[0058] The technical feature "organic solvent" is summarized from the foregoing explanation and / or the corresponding technical feature in Examples 1-7, such as "the organic solvent is at least one of isopropanol, toluene, ethylene glycol monobutyl ether, and diethylene glycol monobutyl ether." Therefore, those skilled in the art can reasonably presume that the technical feature "organic solvent," its subordinate concepts, its substantially equivalent technical means, and technical means that can replace "organic solvent" based on existing technology and conventional technical means and common knowledge should all fall within the protection scope of the technical feature "organic solvent." For example, replacing "organic solvent" with "isopropanol," "toluene," etc., while keeping other technical features unchanged, still falls within the protection scope of this invention.

[0059] The technical feature "pH adjuster" is derived from the aforementioned explanation and / or the corresponding technical features in Examples 1-7, such as "at least one of organic alkaline substances and inorganic alkaline substances" or "at least one of acetic acid, sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, triethanolamine, diethanolamine, tetramethylammonium hydroxide, and morpholine," through the common feature "chemical auxiliaries used to adjust the pH value of softener systems." Therefore, those skilled in the art can reasonably presume that the technical feature "pH adjuster," its subordinate concepts, its substantially equivalent technical means, and technical means that can replace "pH adjuster" based on existing technology and conventional technical means and common knowledge should all fall within the protection scope of the technical feature "pH adjuster." For example, replacing "pH adjuster" with "sodium carbonate," "sodium bicarbonate," etc., while keeping other technical features unchanged, still falls within the protection scope of this invention.

[0060] The technical feature “the composition of the softener, by weight, includes 20-30 parts octamethylcyclotetrasiloxane, 2-4 parts dodecyl dimethyl tertiary amine, 2-4 parts allyl polyether, 0.5-2 parts polyamine derivative, 0.5-1 part pH adjuster, 5-10 parts organic solvent and 49-70 parts water” is summarized from the foregoing explanation and / or the corresponding technical feature in Examples 1-7, “the composition of the softener, by weight, includes 25 parts octamethylcyclotetrasiloxane, 3 parts dodecyl dimethyl tertiary amine, 3 parts allyl polyether, 1 part polyamine derivative, 0.8 parts cationic surfactant, 2.5 parts nonionic surfactant, 0.3 parts antibacterial / bacteriostatic agent, 0.8 parts pH adjuster, 8 parts organic solvent and 55.6 parts water”. Therefore, based on reasonable presumption, those skilled in the art can determine that the technical feature “the components of the softener, by weight, include 20-30 parts of octamethylcyclotetrasiloxane, 2-4 parts of dodecyl dimethyl tertiary amine, 2-4 parts of allyl polyether, 0.5-2 parts of polyamine derivatives, 0.5-1 parts of pH adjuster, 5-10 parts of organic solvent and 49-70 parts of water”, its subordinate concepts, its essentially equivalent technical means, and technical means that can replace it based on the existing level of technology and within the scope of conventional technical means and common knowledge, should all fall within the scope of protection of the technical feature “the components of the softener, by weight, include 20-30 parts of octamethylcyclotetrasiloxane, 2-4 parts of dodecyl dimethyl tertiary amine, 2-4 parts of allyl polyether, 0.5-2 parts of polyamine derivatives, 0.5-1 parts of pH adjuster, 5-10 parts of organic solvent and 49-70 parts of water”.

[0061] Examples 1-7 of this invention at least support the protection scope of "bulk polymerization", "emulsification" and "compound".

[0062] The technical feature "bulk polymerization" is derived from the aforementioned explanation and / or the corresponding technical feature in Examples 1-7, such as "under dry nitrogen protection, octamethylcyclotetrasiloxane, γ-aminopropyltriethoxysilane, hexamethyldisiloxane, tetramethylammonium hydroxide, and isopropanol are mixed and heated to 100-130°C for 3-6 hours," which is summarized by the common feature "a reaction in which monomers (such as D4) directly polymerize to form polymers (such as silicone oil) under the action of a catalyst in the absence of solvent or with a small amount of solvent." Therefore, those skilled in the art can reasonably presume that the technical feature "bulk polymerization," its subordinate concepts, its substantially equivalent technical means, and technical means that can replace the technical feature "bulk polymerization" based on existing technology and conventional technical means and common knowledge should all fall within the protection scope of the technical feature "bulk polymerization." For example, replacing the technical feature "bulk polymerization" with "polymerization" while keeping other technical features unchanged still falls within the protection scope of this invention.

[0063] The technical feature “emulsification” is derived from the aforementioned explanation and / or the corresponding technical feature in Examples 1-7, such as “mixing and emulsifying the silicone oil-based polymer obtained in step (1) with cationic surfactants and nonionic surfactants to obtain an emulsion,” and is summarized by the common feature “the process of uniformly dispersing the oil phase (such as silicone oil and cationic surfactants) in the aqueous phase to form a stable O / W type (oil-in-water) emulsion.” Therefore, those skilled in the art can reasonably presume that the technical feature “emulsification,” its subordinate concepts, its essentially equivalent technical means, and technical means that can replace the technical feature “emulsification” based on the existing level of technology within the scope of conventional technical means and common knowledge should all fall within the protection scope of the technical feature “emulsification.”

[0064] The technical feature “compounding” is derived from the aforementioned explanation and / or the corresponding technical feature in Examples 1-7, “compounding adjustment: cooling the emulsion system obtained in step (3) to 30-40°C and mixing it with dodecyl dimethyl tertiary amine, allyl polyether, and polyethylene polyamine alkylbenzene sulfonate amine to obtain a compound emulsion,” which is summarized by the common feature “the process of mixing two or more raw materials with different functions (such as cationic and nonionic surfactants, silicone oil and polyamine derivatives, softening ingredients and antibacterial agents) in a certain proportion to achieve synergistic effects.” Therefore, those skilled in the art can reasonably presume that the technical feature “compounding,” its subordinate concepts, its essentially equivalent technical means, and technical means that can replace the technical feature “compounding” within the scope of conventional technical means and common knowledge based on the existing level of technology should all fall within the protection scope of the technical feature “compounding.”

[0065] The beneficial effects of this invention are as follows: The present invention has at least the following beneficial effects: 1. Compared with the prior art, the present invention provides a technical solution with a different technical concept, and its technical effect is equivalent to or slightly improved with the prior art. The difference between the technical concept of the present invention and the prior art includes, but is not limited to, "preparing softeners by using organosilicon chemical structures in conjunction with multifunctional modifiers through bulk polymerization, emulsification, compounding, etc."

[0066] Furthermore, based on the present invention: 1. Based on the comparison of Examples 1-7 and Comparative Examples 1-4, the present invention purposefully selects from the broad range of "amino silicone oil and block silicone oil" disclosed in the prior art a narrow range of "octamethylcyclotetrasiloxane, dodecyl dimethyl tertiary amine, allyl polyether, polyamine derivatives, and pH adjusters" not mentioned in the prior art, and achieves unexpected technical effects such as "providing a softener with better hand feel and minimal impact on fabric yellowing and color change". Detailed Implementation

[0067] The following non-limiting embodiments are intended to enable those skilled in the art to gain a more comprehensive understanding of the present invention, but do not limit the invention in any way. The following content is merely an exemplary description of the scope of protection claimed by the present invention, and those skilled in the art can make various changes and modifications to the present invention based on the disclosed content, and such changes should also fall within the scope of protection claimed by the present invention.

[0068] The present invention will be further described below by way of specific embodiments. Unless otherwise specified, all instruments, devices, equipment, reagents, products, etc., used in the embodiments of the present invention are obtained through conventional commercial means.

[0069] Specific raw material information is shown in Table 1: Table 1. Raw Material Information

[0070] Preparation of the softener described in Example 1 Raw material preparation: 20 parts by weight of octamethylcyclotetrasiloxane, 2 parts by weight of dodecyl dimethyl tertiary amine, 2 parts by weight of allyl polyether, 0.5 parts by weight of polyethylene polyamine alkylbenzene sulfonate amine, 0.5 parts by weight of acetic acid, 5 parts by weight of isopropanol and 70 parts by weight of water; (1) Bulk polymerization: Under dry nitrogen protection, octamethylcyclotetrasiloxane, γ-aminopropyltriethoxysilane, hexamethyldisiloxane, tetramethylammonium hydroxide and isopropanol are mixed and heated to 100-130℃ for 3-6 hours. The reaction endpoint is monitored by measuring refractive index or viscosity. After the reaction is completed, the temperature is raised to 150-180℃, the vacuum degree is -0.09~-0.1MPa, and the reaction time is 1-2 hours. Low-boiling substances are removed and the catalyst is destroyed under vacuum to obtain silicone oil-based polymer. (2) Homogenization and refinement: The silicone oil base polymer obtained in step (2) is homogenized and refined under a high pressure homogenizer at a pressure of 20~30MPa to obtain an emulsion; (3) Compounding adjustment: The emulsion system obtained in step (2) is cooled to 30~40℃ and mixed with dodecyl dimethyl tertiary amine, allyl polyether, and polyethylene polyamine alkylbenzene sulfonate amine to obtain a compound emulsion; (5) System adjustment: Mix the compound emulsion obtained in step (4) with acetic acid to adjust the pH to 6.5~7.5, then mix with water and filter through a 100-200 mesh filter to obtain the softener.

[0071] Example 2 The difference from Example 1 is that the raw materials are "30 parts by weight of octamethylcyclotetrasiloxane, 4 parts by weight of dodecyl dimethyl tertiary amine, 4 parts by weight of allyl polyether, 2 parts by weight of alkyl polyoxyethylene ether quaternary ammonium salt, 1 part by weight of acetic acid, 10 parts by weight of isopropanol and 49 parts by weight of water", and the rest are the same.

[0072] Example 3 The difference from Example 1 is that the raw materials are "25 parts octamethylcyclotetrasiloxane, 3 parts dodecyl dimethyl tertiary amine, 3 parts allyl polyether, 1 part resin block polyetheramine, 0.8 parts acetic acid, 8 parts isopropanol and 59.2 parts water", and the rest are the same.

[0073] Example 4 Raw material preparation: 30 parts by weight of octamethylcyclotetrasiloxane, 4 parts by weight of dodecyl dimethyl tertiary amine, 4 parts by weight of allyl polyether, 2 parts by weight of polyethylene polyamine alkylbenzene sulfonate amine, 1 part by weight of distearate ethyl glycidyl quaternary ammonium salt, 3 parts by weight of AEO-3, 0.5 parts by weight of dodecyl dimethyl benzyl ammonium chloride, 1 part by weight of acetic acid, 10 parts by weight of isopropanol and 44.5 parts by weight of water; (1) Bulk polymerization: Under dry nitrogen protection, octamethylcyclotetrasiloxane, γ-aminopropyltriethoxysilane, hexamethyldisiloxane, tetramethylammonium hydroxide and isopropanol are mixed and heated to 100-130℃ for 3-6 hours. The reaction endpoint is monitored by measuring refractive index or viscosity. After the reaction is completed, the temperature is raised to 150-180℃, the vacuum degree is -0.09~-0.1MPa, and the reaction time is 1-2 hours. Low-boiling substances are removed and the catalyst is destroyed under vacuum to obtain silicone oil-based polymer. (2) Emulsification stage: The silicone oil base polymer obtained in step (1) is mixed with part of the chlorinated distearate ethyl glycidyl quaternary ammonium salt and AEO-3 at a temperature of 50~60℃ to obtain an oil phase system; the remaining chlorinated distearate ethyl glycidyl quaternary ammonium salt and AEO-3 are mixed with water and dodecyl dimethyl benzyl ammonium chloride at a temperature of 50~60℃ to obtain an aqueous phase system; the aqueous phase system is slowly added to the oil phase system under high-speed shearing at a speed of 2000~3000r / min to obtain a crude emulsion; (3) Homogenization and refinement: The crude emulsion obtained in step (2) is homogenized and refined in a high-pressure homogenizer at a pressure of 20~30MPa to obtain an emulsion; (4) Compounding adjustment: Cool the emulsion system obtained in step (3) to 30~40℃, and mix it with dodecyl dimethyl tertiary amine, allyl polyether, and polyethylene polyamine alkylbenzene sulfonate amine to obtain a compound emulsion; (5) System adjustment: Mix the compound emulsion obtained in step (4) with acetic acid to adjust the pH to 6.5~7.5, then mix with water and filter through a 100-200 mesh filter to obtain the softener.

[0074] Example 5 The difference from Example 4 is that the raw materials are "25 parts by weight of octamethylcyclotetrasiloxane, 3 parts by weight of dodecyl dimethyl tertiary amine, 3 parts by weight of allyl polyether, 1 part by weight of polyethylene polyamine alkylbenzene sulfonate amine, 0.8 parts by weight of distearate ethyl glycidyl quaternary ammonium salt, 2.5 parts by weight of AEO-3, 0.3 parts by weight of dodecyl dimethyl benzyl ammonium chloride, 0.8 parts by weight of acetic acid, 8 parts by weight of isopropanol and 55.6 parts by weight of water", and the rest are the same.

[0075] Example 6 The difference from Example 5 is that "polyethylene polyamine alkylbenzene sulfonate amine" is replaced with "alkyl polyoxyethylene ether quaternary ammonium salt", otherwise they are the same.

[0076] Example 7 The difference from Example 5 is that "polyethylene polyamine alkylbenzene sulfonate amine" is replaced with "resin block polyether amine", otherwise they are the same.

[0077] Comparative Example 1 The difference from Example 3 is that "octamethylcyclotetrasiloxane" is replaced with "decamethylcyclopentasiloxane", otherwise they are the same.

[0078] Comparative Example 2 The difference from Example 3 is that “octamethylcyclotetrasiloxane” is replaced with “polyoxyethylene-polyoxypropylene modified silicone oil”, and all other aspects are the same.

[0079] Comparative Example 3 The difference from implementation 3 is that "dodecyl dimethyl tertiary amine" is replaced with "hexadecyl trimethyl ammonium chloride", otherwise they are the same.

[0080] Comparative Example 4 The difference from Implementation 3 is that "dodecyl dimethyl tertiary amine" is replaced with "octadecyl trimethyl ammonium chloride", otherwise they are the same.

[0081] Comparative Example 5 The difference from Example 5 is that the raw materials are "40 parts by weight of octamethylcyclotetrasiloxane, 5 parts by weight of dodecyl dimethyl tertiary amine, 5 parts by weight of allyl polyether, 3 parts by weight of polyethylene polyamine alkylbenzene sulfonate amine, 2 parts by weight of distearate ethyl glycidyl quaternary ammonium salt, 4 parts by weight of AEO-3, 1 part by weight of dodecyl dimethyl benzyl ammonium chloride, 2 parts by weight of acetic acid, 15 parts by weight of isopropanol and 23 parts by weight of water", and the rest are the same.

[0082] Comparative Example 6 The difference from Example 5 is that the raw materials are "15 parts by weight of octamethylcyclotetrasiloxane, 1 part by weight of dodecyl dimethyl tertiary amine, 1 part by weight of allyl polyether, 0.1 parts by weight of polyethylene polyamine alkylbenzene sulfonate amine, 0.8 parts by weight of distearate ethyl glycidyl quaternary ammonium salt, 2.5 parts by weight of AEO-3, 0.3 parts by weight of dodecyl dimethyl benzyl ammonium chloride, 0.1 parts by weight of acetic acid, 3 parts by weight of isopropanol and 76.2 parts by weight of water", and the rest are the same.

[0083] Test Example 1: Fabric Hand Feel Test Formula: Softener X g / L (see Table 2 for details), working solution pH: 4-6; Fabric: 150D plain weave whitening polyester chiffon yarn; Process: Two dips and two rolls (liquid content: 75%) → Shaping (160℃×90s) → Evaluate hand feel; The test results are shown in the table below: Table 2. Evaluation of fabric hand feel after treatment with different softeners.

[0084] Note: The rating is based on a 100-point scale and is given by professionals who assess the feel of the controls. The higher the score, the better the feel, and the lower the score, the worse the feel.

[0085] As can be seen from the table above, the softener prepared in the embodiments of this application has excellent softness and fluffy feel, which is significantly better than representative softeners on the market.

[0086] Test Example 2: Yellowing of Fabrics Formula: Softener X g / L (see Table 3 for details), working solution pH: 4-6; Fabric: 150D plain weave whitening polyester chiffon yarn; Process: Two dips and two nips (liquid content: 65%) → Setting (160℃×90s) → Testing GB / T 29778-2013 "Textiles - Tests for Color Fastness - Evaluation of Potential Phenolic Yellowing"; The test results are shown below: Table 3. Test results for yellowing of fabrics treated with different softeners.

[0087] As can be seen from the table above, the fabrics treated with the softener prepared in the embodiments of this application show virtually no yellowing, especially Example 5, which shows a more significant effect.

[0088] Test Example 3: Fabric Color Change Test Formula: Softener 30g / L (see Table 4 for details), working solution pH: 4-6; Fabric: black polyester Oxford cloth; Process: Two dips and two nips (liquid content: 75%) → Setting (160℃×90s) → Testing GB / T 30669—2014 "Textiles - Tests for color fastness - Fastness to light yellowing"; The test results are shown below: Table 4. Test results of color change in fabrics treated with different softeners.

[0089] As can be seen from the table above, the fabric treated with the softener prepared in the embodiments of this application has virtually no effect on the fabric's color.

[0090] Test Example 4: Test of the hydrophilicity of fabrics Formula: Softener X g / L (see Table 5 for details), working solution pH: 4-6; Fabric: 300D black polyester Oxford cloth; Process: Two dips and two rolls (liquid content: 65%) → Shaping (160℃×90s) → Hydrophilicity test; The test results are shown below: Table 5. Test results of hydrophilicity of fabrics treated with different softeners.

[0091] As can be seen from the table above, the fabric treated with the softener prepared in the embodiments of this application has significantly improved hydrophilicity, which is better than that of representative softeners on the market.

[0092] Test Example 5: Fabric fastness test Formula: Softener X g / L (see Table 6 for details), working solution pH: 4-6; Fabric: 150D plain weave whitening polyester chiffon yarn; Process: Two dips and two nips (liquid content: 75%) → Setting (160℃×90s) → Testing GB / T 3921-2008 "Textiles - Tests for color fastness to soaping"; The test results are shown below: Table 6. Test results of wash fastness of fabrics treated with different softeners.

[0093] As can be seen from the table above, the fabric treated with the softener prepared in the embodiments of this application shows a very slight decrease in wash fastness.

[0094] Stability test of Example 6 Formula: 100g / L softener (see Table 7 for details), other conditions are detailed in the table; Table 7. Stability Test Results of Different Softeners

[0095] Notes: High safety standard: Stable at pH=11, temperature 70℃, rotation speed 2000 rpm / min for 30 min, and stable after standing for 7 days; Medium safety standard: Stable at pH=10.5, temperature 70℃, rotation speed 2000 rpm / min for 20 min, and stable after standing for 7 days; Basic safety standard: Stable at pH=9, temperature 50℃, rotation speed 2000 rpm / min for 10 min, and stable after standing for 7 days.

[0096] As can be seen from the table above, the softener prepared in the embodiments of this application has excellent stability.

[0097] Verification of technical effectiveness and / or analysis of technical problem solving The above data analysis and comparison show that the novel organosilicon chemical structure of this invention, combined with multifunctional modification, prepares a highly stable, non-yellowing softener with a high cotton-like feel, giving the fabric a soft, fluffy, and cotton-like hand feel, while having virtually no effect on the yellowing or discoloration of the fabric.

[0098] Finally, it should be noted that the above content is only used to illustrate the technical solution of the present invention, and is not intended to limit the scope of protection of the present invention. Simple modifications or equivalent substitutions made by those skilled in the art to the technical solution of the present invention do not depart from the essence and scope of the technical solution of the present invention.

Claims

1. A non-yellowing, cotton-like fabric softener, characterized in that, It includes octamethylcyclotetrasiloxane, dodecyl dimethyl tertiary amine, allyl polyether, polyamine derivatives, pH adjusters, organic solvents, and water.

2. The softener according to claim 1, characterized in that, The polyamine derivative is selected from at least one of polyethylene polyamine alkylbenzene sulfonate amine, alkyl polyoxyethylene ether quaternary ammonium salt and resin block polyether amine; preferably at least one of alkyl polyoxyethylene ether quaternary ammonium salt and resin block polyether amine; more preferably resin block polyether amine. The pH adjuster is at least one of organic alkaline substances and inorganic alkaline substances; preferably at least one of acetic acid, sodium hydroxide, potassium hydroxide, sodium carbonate, sodium bicarbonate, triethanolamine, diethanolamine, tetramethylammonium hydroxide and morpholine; more preferably at least one of acetic acid, sodium hydroxide, sodium carbonate, sodium bicarbonate, triethanolamine, diethanolamine and tetramethylammonium hydroxide; and even more preferably acetic acid; The organic solvent is at least one of isopropanol, toluene, ethylene glycol monobutyl ether, and diethylene glycol monobutyl ether; preferably at least one of isopropanol, ethylene glycol monobutyl ether, and diethylene glycol monobutyl ether; more preferably isopropanol.

3. The softener according to claim 1, characterized in that, The softener also contains cationic surfactants, nonionic surfactants, and antibacterial / bacteriostatic agents. The cationic surfactant is selected from at least one of octadecyltrimethylammonium chloride, hexadecyltrimethylammonium chloride, dodecyltrimethylammonium chloride, dodecyldimethylbenzylammonium chloride, and disteaamide ethyl glycidyl quaternary ammonium chloride; preferably, disteaamide ethyl glycidyl quaternary ammonium chloride. The nonionic surfactant is at least one of fatty alcohol polyoxyethylene ether, alkylphenol polyoxyethylene ether, and sorbitan ester and its polyoxyethylene ether; preferably fatty alcohol polyoxyethylene ether. The antibacterial / bacteriostatic agent is at least one of quaternary ammonium salt antibacterial agents, organosilicon quaternary ammonium salts, natural antibacterial agents, and thiazolinones; preferably a quaternary ammonium salt antibacterial agent; more preferably at least one of dodecyl dimethyl benzyl ammonium chloride and polyhexamethylene guanidine hydrochloride; and even more preferably dodecyl dimethyl benzyl ammonium chloride.

4. The softener according to claim 1, characterized in that, By weight, it comprises 20-30 parts octamethylcyclotetrasiloxane, 2-4 parts dodecyl dimethyl tertiary amine, 2-4 parts allyl polyether, 0.5-2 parts polyamine derivatives, 0.5-1 parts pH adjuster, 5-10 parts organic solvent and 49-70 parts water; More preferably, the softener comprises, by weight, 20-30 parts octamethylcyclotetrasiloxane, 2-4 parts dodecyl dimethyl tertiary amine, 2-4 parts allyl polyether, 0.5-2 parts polyamine derivative, 0-1 part cationic surfactant, 0-3 parts nonionic surfactant, 0-0.5 parts antibacterial / bacteriostatic agent, 0.5-1 part pH adjuster, 5-10 parts organic solvent, and 44.5-70 parts water; More preferably, the softener comprises, by weight, 25 parts octamethylcyclotetrasiloxane, 3 parts dodecyl dimethyl tertiary amine, 3 parts allyl polyether, 1 part polyamine derivative, 0.8 parts cationic surfactant, 2.5 parts nonionic surfactant, 0.3 parts antibacterial / bacteriostatic agent, 0.8 parts pH adjuster, 8 parts organic solvent and 55.6 parts water.

5. A method for preparing the softener according to any one of claims 1-4, characterized in that, Including the following steps: (1) Bulk polymerization: Octamethylcyclotetrasiloxane, aminosilane coupling agent, capping agent, catalyst and organic solvent are reacted to obtain silicone oil-based polymer; (2) Emulsification stage: The silicone oil-based polymer obtained in step (1) is mixed with cationic surfactant and nonionic surfactant and emulsified to obtain an emulsion; (3) Compounding adjustment: The emulsion obtained in step (2) is mixed with dodecyl dimethyl tertiary amine, allyl polyether and polyamine derivative to obtain a compound emulsion; (4) System adjustment: The compound emulsion obtained in step (3) is mixed with pH adjuster and water to obtain the softener.

6. The preparation method according to claim 5, characterized in that, The aminosilane coupling agent is selected from at least one of γ-aminopropyltriethoxysilane, N-β-aminoethyl-γ-aminopropyltrimethoxysilane, N-β-aminoethyl-γ-aminopropylmethyldimethoxysilane and γ-ureopropyltriethoxysilane; The end-capping agent is selected from at least one of hexamethyldisiloxane, trimethylethoxysilane, dimethylvinylchlorosilane, and trimethylchlorosilane; The catalyst is selected from at least one of tetramethylammonium hydroxide, potassium hydroxide, potassium silanolate, sulfuric acid, and trifluoromethanesulfonic acid.

7. The preparation method according to claim 5 or 6, characterized in that, The reaction conditions in step (1) are: reaction temperature of 100-130℃ and reaction time of 3-6h; preferably: reaction temperature of 110-130℃ and reaction time of 4-6h; more preferably: reaction temperature of 120℃ and reaction time of 5h. The endpoint of the reaction described in step (1) is a system viscosity of 2000-10000 mPa or a refractive index of 1.400-1.410; Preferably, after the reaction in step (1) is completed, a purification operation is also included; More preferably, the purification is selected from at least one of vacuum distillation, acid washing and neutralization, alkali washing and neutralization, molecular distillation, filtration and adsorption, and the purification path is selected according to the type of silicone oil polymerization; More preferably, the purification path consists of vacuum distillation, acid washing and neutralization, activated carbon adsorption, and filtration. More preferably, the reaction conditions for vacuum distillation are: a reaction temperature of 150-180℃, a vacuum degree of -0.09~-0.1MPa, and a reaction time of 1-2h. The reaction conditions for acid washing and neutralization are: heating the dilute acid and then performing multi-stage washing and neutralization until neutral.

8. The preparation method according to claim 5, characterized in that, The mixing sequence in step (2) is as follows: the silicone oil base polymer obtained in step (1) is first mixed with some cationic surfactants and nonionic surfactants to obtain an oil phase system; the remaining cationic surfactants and nonionic surfactants are mixed with water to obtain an aqueous phase system. More preferably, the mixing sequence is to slowly add the aqueous phase system to the oil phase system; More preferably, the mixing temperature for preparing the oil phase system is 50~60℃; More preferably, the mixing temperature for preparing the aqueous system is 50~60℃; More preferably, the aqueous phase system further includes an antibacterial / bacteriostatic agent; The mixing method in step (2) is selected from at least one of stirring mixing, high-speed shear mixing and colloid milling; preferably high-speed shear mixing; more preferably high-speed shear mixing with a rotation speed of 2000~3000 r / min; Preferably, step (2) further includes a homogenization and refining operation after emulsification; More preferably, the homogenization and refining is selected from at least one of high-pressure homogenization and colloid mill grinding; even more preferably, high-pressure homogenization is used; most preferably, the pressure of the high-pressure homogenization is 20~30MPa.

9. The preparation method according to claim 5, characterized in that, The mixing in step (3) is selected from at least one of stirring mixing, high-speed shear mixing and colloid milling; preferably stirring mixing; more preferably stirring mixing at a speed of 100~200 r / min; Preferably, step (3) further includes a cooling step of the system before mixing; More preferably, the system is cooled to 30~40℃; Preferably, the amount of pH adjuster added in step (4) is sufficient to adjust the pH of the system to 6.5-7.5; The mixing in step (4) is selected from at least one of stirring mixing, high-speed shear mixing and colloid milling; preferably stirring mixing; more preferably stirring mixing at a speed of 100~200 r / min; Preferably, the mixing operation in step (4) is followed by a filtering step; More preferably, the filter is selected from at least one of mesh filtration, precision filtration, plate and frame filtration and vacuum filtration; even more preferably, it is mesh filtration; most preferably, the filter is a 100-200 mesh filter.

10. The use of the softener according to any one of claims 1-4 in the washing and care of textiles.

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