Novel fluffy softening agent extremely resistant to salt, alkali and high temperature and preparation method of novel fluffy softening agent

Abstract

The invention discloses a novel fluffy softening agent extremely resistant to salt, alkali and high temperature, a preparation method and application, and relates to the technical field of textile printing and dyeing auxiliaries. The fluffy softening agent is prepared from the following raw materials in parts by weight: 30 to 50 parts of octamethylcyclotetrasiloxane, 10 to 20 parts of polyether epoxy end-capping reagent, 5 to 15 parts of organic silicon derivative, 1 to 3 parts of emulsifier, 2 to 6 parts of surfactant, 0.5 to 2 parts of bacteriostatic agent, 0.05 to 0.1 part of pH regulator and 40 to 70 parts of solvent. The fluffy softener prepared by the method can endow a fabric with an excellent soft, fluffy and elegant hand feeling style, has extremely salt-alkali-resistant and high-temperature-resistant stability performance, and has no obvious influence on the whiteness, color light and fastness of the dyed fabric.

Description

Technical Field

[0001] This invention belongs to the field of textile dyeing and finishing technology, specifically relating to a novel extremely salt-alkali-resistant and high-temperature-resistant fluffing and softening agent and its preparation method. Background Technology

[0002] In the textile printing and dyeing process of cotton fabrics, a large amount of salt and alkali are present in the pretreatment, dyeing and soaping processes. If the dyeing plant does not wash the fabric thoroughly, a large amount of salt and alkali will remain on the fabric during the finishing process. When the fabric is introduced into the softener working solution, it will react with the softener, resulting in phenomena such as demulsification and lint. Ultimately, this will lead to defects such as silicone oil spots on the finished fabric, which seriously affects the quality of the fabric. Therefore, the softening process in the finishing of cotton requires extremely high stability of the softener.

[0003] Currently, most fabric softeners on the market are made from amino silicone oil or amino-modified silicone oil. They are generally synthesized using the hydrosilylation method, which involves ring-opening polymerization of octamethylcyclotetrasiloxane with a corresponding silane coupling agent under the action of an alkaline catalyst. After equilibration, a stable amino silicone oil is generated. However, the amino group (-NH2 / -NHR) in this type of softener is easily protonated to -NH3 under alkaline conditions (pH>10). + It attacks the siloxane backbone (Si-O-Si), triggering chain scission degradation, which leads to emulsion demulsification and oil separation.

[0004] The following problems exist with conventional silicone oils on the market: (1) poor softness and fluffy feel; (2) poor hydrophilicity, resulting in water repellency of the fabric after treatment; (3) poor resistance to extreme salt and alkali, which can easily cause demulsification and oil floating during use; (4) it will affect the color and fastness of the fabric, seriously affecting the quality of the final fabric.

[0005] Therefore, it is necessary to develop a new type of extremely salt-alkali-resistant and high-temperature-resistant fluffing softener to give fabrics a soft, fluffy, and skin-friendly feel, while also having excellent hydrophilic properties and extremely high stability. It is also self-emulsifying, easy to use, and will not affect the whiteness, color, or fastness of dyed fabrics. Summary of the Invention

[0006] To address the shortcomings of existing technologies, this invention provides a novel extremely salt- and alkali-resistant and high-temperature-resistant fluffing and softening agent and its preparation method.

[0007] To achieve the above-mentioned objectives of this invention, the specific technical solution adopted by this invention is as follows: A novel, extremely salt- and alkali-resistant, high-temperature-resistant fluffing and softening agent, comprising, by weight, the following raw materials: 30-50 parts of octamethylcyclotetrasiloxane, 10-20 parts of polyether epoxy end-capping agent, 5-15 parts of organosilicon derivative, 1-3 parts of emulsifier, 2-6 parts of surfactant, 0.5-2 parts of antibacterial agent, 0.05-0.1 parts of pH adjuster, and 40-70 parts of solvent.

[0008] Preferably, the polyether epoxy end-capping agent is a single-end epoxy end-capping product of ethylene oxide-propylene oxide block copolymer with a molecular weight of 1000-3000, and the organosilicon derivative is an acrylate-modified siloxane containing long-chain alkyl groups, wherein the long-chain alkyl groups have 12-18 carbon atoms.

[0009] Preferably, the emulsifier is selected from at least one of nonionic polymeric emulsifiers and fatty alcohol polyoxyethylene ethers; Preferably, the nonionic polymeric emulsifier is a polyoxyethylene-polyoxypropylene block copolymer with a molecular weight of 2000-5000; the fatty alcohol carbon chain length in the fatty alcohol polyoxyethylene ether is C 12 -C 18 The addition number of ethylene oxide is 5-20.

[0010] Preferably, the surfactant is selected from at least one of alkyl glycosides and isomeric tridecyl alcohol ethers; Preferably, the alkyl carbon chain length in the alkyl glycoside is C8-C9. 14 The isomeric tridecyl alcohol ether is isomeric tridecyl alcohol polyoxyethylene ether, with an ethylene oxide addition number of 7-12.

[0011] Preferably, the solvent is selected from one or more of isopropanol, propylene glycol, and isododecane.

[0012] Preferably, the antibacterial agent is selected from one or more of benzyl chloride, polyhexamethylene biguanide hydrochloride, and 2-n-octyl-4-isothiazolin-3-one.

[0013] Preferably, the pH adjuster is selected from at least one of acetic acid and citric acid.

[0014] This invention also relates to a method for preparing the above-mentioned fluffing and softening agent, comprising the following steps: (1) Mix octamethylcyclotetrasiloxane and organosilicon derivatives, add polyether epoxy end-capping agent, heat and react to obtain product A; (2) Mix product A, emulsifier, surfactant and solvent, heat and emulsify to form a uniform emulsion; (3) Cool the emulsion, add antibacterial agent and pH adjuster, homogenize, filter, and obtain the fluffing softener.

[0015] Preferably, in step (1), the temperature is raised to 75-85℃ and the reaction is carried out for 3-5 hours. After the reaction, the vacuum is evacuated for 30-50 minutes at a vacuum degree of -0.096MPa to -0.099MPa. In step (2), the temperature is raised to 60-70℃, the emulsification rate is 6000-10000rpm, and the emulsification time is 30-60 minutes.

[0016] Preferably, in step (3), the temperature is reduced to below 40°C, and the homogenization conditions are: homogenization is performed at 15-25 MPa and a rotation speed of 2000-4000 rpm for 10-30 minutes.

[0017] Compared with the prior art, the present invention has the following beneficial effects: (1) The fluffing and softening agent in this invention gives the fabric an excellent softness, fluffiness and skin-friendly feel, among which the softness and fluffiness are particularly prominent.

[0018] (2) The fluffing and softening agent in this invention has excellent resistance to salt and alkali and high temperature, and can still be produced stably under extreme environments.

[0019] (3) The fluffing and softening agent in this invention has excellent hydrophilic properties, and the treated fabric has excellent hydrophilic effect.

[0020] (4) The fluffing and softening agent in this invention has low or even no yellowing properties and can be used on white / light-colored fabrics.

[0021] (5) The fluffing and softening agent in this invention has excellent stability and is safe to use. Detailed Implementation

[0022] The present invention will be further described in detail below with reference to specific embodiments. The following embodiments are not intended to limit the present invention, but only to illustrate the present invention. Unless otherwise specified, the experimental methods used in the following embodiments are generally performed under conventional conditions. Unless otherwise specified, the materials and reagents used in the following embodiments are commercially available.

[0023] Polyether epoxy end-capping agent (ethylene oxide-propylene oxide block copolymer with single-ended epoxy end-capping, molecular weight 1500), purchased from Dow Chemical Company, model: DOW EP-1500; Organosilicon derivative (hexadecyl acrylate modified siloxane), purchased from Wacker Chemie, model: Wacker Silicone MA-168; Nonionic polymeric emulsifier (polyoxyethylene-polyoxypropylene block copolymer, molecular weight 3000), purchased from BASF, model: Pluronic F-38; Fatty alcohol polyoxyethylene ether, purchased from Clariant Chemicals (China) Co., Ltd., model: Clariant Lutensol A 10; Alkyl glycoside, purchased from Henkel (China) Investment Co., Ltd., model: Henkel APG 1214; Isotridecyl alcohol ether (isotridecyl alcohol polyoxyethylene ether, EO=9), purchased from BASF, model: BASF Lutensol XP 90; Polyhexamethylene biguanide hydrochloride, purchased from Shanghai Maclin Biochemical Technology Co., Ltd., model: Maclin. PHMB-50% (50% aqueous solution).

[0024] Example 1 A novel, extremely salt- and alkali-resistant, high-temperature-resistant fluffing and softening agent, by weight, comprises the following raw materials: 40 parts of octamethylcyclotetrasiloxane, 15 parts of polyether epoxy end-capping agent, 10 parts of organosilicon derivative, 2 parts of nonionic polymeric emulsifier, 4 parts of alkyl glycoside, 1 part of benzyl chloride, 0.08 parts of acetic acid, and 55 parts of isopropanol.

[0025] The preparation method of the above-mentioned fluffing and softening agent is as follows: (1) Add octamethylcyclotetrasiloxane and organosilicon derivative to the reaction vessel, stir evenly, add polyether epoxy end-capping agent, heat to 80℃ and react for 4 hours, then vacuum at -0.096MPa for 40 minutes to remove unreacted monomers and low molecular weight by-products in the reaction system to obtain product A. (2) Add product A, nonionic polymeric emulsifier, alkyl glycoside and isopropanol to the emulsification kettle, heat to 65°C, and emulsify at 8000 rpm for 40 minutes to form a uniform emulsion. (3) Cool the emulsion to 35°C, add benzyl chloride and acetic acid, homogenize it for 20 minutes at 3000 rpm under 20 MPa pressure, filter it to obtain a fluffing softener.

[0026] Example 2 A novel, extremely salt- and alkali-resistant, high-temperature-resistant fluffing and softening agent, by weight, comprises the following raw materials: 35 parts of octamethylcyclotetrasiloxane, 12 parts of polyether epoxy end-capping agent, 8 parts of organosilicon derivative, 1.5 parts of fatty alcohol polyoxyethylene ether, 3 parts of isomeric tridecyl alcohol ether, 0.8 parts of polyhexamethylene biguanide hydrochloride, 0.06 parts of citric acid, and 45 parts of propylene glycol.

[0027] The preparation method of the above-mentioned fluffing and softening agent is as follows: (1) Add octamethylcyclotetrasiloxane and organosilicon derivative to the reaction vessel, stir evenly, add polyether epoxy end-capping agent, heat to 75℃ and react for 5 hours, then vacuum at -0.095MPa for 30 minutes to remove unreacted monomers and low molecular weight by-products remaining in the reaction system, and obtain product A. (2) Add product A, fatty alcohol polyoxyethylene ether, isomeric tridecyl alcohol ether and propylene glycol to the emulsification kettle, heat to 60°C, and emulsify at 6000 rpm for 60 minutes to form a uniform emulsion. (3) Cool the emulsion to 30°C, add polyhexamethylene biguanide hydrochloride and citric acid, homogenize it for 25 minutes at 2500 rpm under 15 MPa pressure, filter it to obtain a fluffing softener.

[0028] Example 3 A novel, extremely salt- and alkali-resistant, high-temperature-resistant fluffing and softening agent, comprising the following raw materials by weight: 45 parts octamethylcyclotetrasiloxane, 18 parts polyether epoxy end-capping agent, 12 parts organosilicon derivative, 2.5 parts nonionic polymeric emulsifier, 5 parts isomeric alkyl glycoside, 1.2 parts 2-n-octyl-4-isothiazolin-3-one, 0.09 parts acetic acid, and 60 parts isopropanol.

[0029] The preparation method of the above-mentioned fluffing and softening agent is as follows: (1) Octamethylcyclotetrasiloxane and organosilicon derivatives were added to the reaction vessel and stirred evenly. Then, polyether epoxy end-capping agent was added and the temperature was raised to 85°C for 3 hours. Then, vacuum was applied at -0.096MPa for 40 minutes to remove the unreacted monomers and low molecular weight by-products remaining in the reaction system, and product A was obtained. (2) Add product A, nonionic polymeric emulsifier, alkyl glycoside and isopropanol to the emulsification kettle, heat to 70°C, and emulsify at 10,000 rpm for 30 minutes to form a uniform emulsion; (3) Cool the emulsion to 35°C, add 2-n-octyl-4-isothiazolin-3-one and acetic acid, homogenize it for 15 minutes at 3500 rpm under 20 MPa pressure, filter it to obtain a fluffy softener.

[0030] Comparative Example 1 The only difference between this comparative example and Example 1 is the ratio of raw materials, specifically: By weight, the raw materials are: 60 parts of octamethylcyclotetrasiloxane, 5 parts of polyether epoxy end-capping agent, 20 parts of organosilicon derivative, 2 parts of nonionic polymeric emulsifier, 4 parts of alkyl glycoside, 1 part of benzyl chloride, 0.08 parts of acetic acid, and 50 parts of isopropanol.

[0031] The preparation method is completely consistent with that in Example 1.

[0032] Comparative Example 2 The only difference between this comparative example and Example 1 is the emulsification system. Specifically, the nonionic polymeric emulsifier and alkyl glycoside are replaced with Span-80 and sodium dodecyl sulfate, respectively.

[0033] Comparative Example 3 The only difference between this comparative example and Example 1 is that the organosilicon derivative is replaced with amino silicone oil (Dow Corning DC-366, a conventional amino-modified silicone oil).

[0034] Effect test Test Example 1: Fabric Hand Feel Test Formula: Softener X g / L (see Table 1 for details), working solution pH: 4-6; Fabric: white cotton knitted fabric; Process: Two dips and two rolls (liquid content: 75%) → Shaping (160℃×90s) → Evaluate hand feel.

[0035] Table 1. Evaluation Table of Fabric Hand Feel

[0036] 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.

[0037] As can be seen from Table 1 above, the novel salt-alkali-resistant and high-temperature-resistant fluffing softener of the present invention has excellent softness, fluffiness, and skin-friendly feel, which is significantly better than representative softeners on the market.

[0038] Test Example 2: Stability of different softeners against salt, alkali, and high temperatures Formula: 100g / L of softener, other conditions are detailed in Table 2.

[0039] Table 2. Stability test results of different softeners against salt, alkali and high temperature.

[0040] As can be seen from Table 2 above, the novel salt-alkali-resistant and high-temperature-resistant fluffing and softening agent of the present invention has excellent stability against salt, alkali and high temperatures.

[0041] Test Example 3: Stability Test of Different Softeners Formula: 100g / L softener, other conditions are detailed in Table 3.

[0042] Table 3. Stability Test Results of Different Softeners

[0043] As can be seen from Table 3 above, the novel salt-alkali-resistant and high-temperature-resistant fluffing and softening agent of the present invention not only exhibits good stability in salt-alkali resistance and high-temperature resistance, but also shows good stability in co-bath with fixing agents and whitening agents.

[0044] Test Example 4: Yellowing Test of Fabrics Treated with Different Softeners Formula: Softener X g / L (see Table 4 for details), working solution pH: 4-6; Fabric: 40×40 / 133×76 whitening cotton woven fabric; Process: Two dips and two rolls (liquid content: 65%) → Shaping (160℃×90s) → Whiteness test.

[0045] Table 4 Test Table for Yellowing of Fabrics

[0046] As can be seen from Table 4 above, the fabrics treated with the novel salt, alkali and high temperature resistant fluffing and softening agent of this invention show virtually no yellowing.

[0047] Test Example 5: Testing the hydrophilicity of fabrics treated with different softeners. Formula: Softener X g / L (see Table 5 for details), working solution pH: 4-6; Fabric: 40×40 / 133×76 whitening cotton woven fabric; Process: Two dips and two rolls (liquid content: 65%) → Shaping (160℃×90s) → Hydrophilicity test.

[0048] Table 5. Test Table for Hydrophilicity of Fabrics

[0049] As can be seen from Table 5 above, the hydrophilicity of fabrics treated with the novel salt, alkali and high temperature resistant fluffing softener of this invention is basically not reduced or only slightly reduced, which is better than representative softeners on the market.

[0050] 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 novel, extremely salt- and alkali-resistant, high-temperature-resistant fluffing and softening agent, characterized in that, The raw materials of the fluffing and softening agent, by weight, include: 30-50 parts of octamethylcyclotetrasiloxane, 10-20 parts of polyether epoxy end-capping agent, 5-15 parts of organosilicon derivative, 1-3 parts of emulsifier, 2-6 parts of surfactant, 0.5-2 parts of antibacterial agent, 0.05-0.1 parts of pH adjuster, and 40-70 parts of solvent.

2. The fluffing and softening agent according to claim 1, characterized in that, The polyether epoxy end-capping agent is a single-end epoxy end-capped product of ethylene oxide-propylene oxide block copolymer with a molecular weight of 1000-3000, and the organosilicon derivative is an acrylate-modified siloxane containing long-chain alkyl groups, wherein the long-chain alkyl groups have 12-18 carbon atoms.

3. The fluffing and softening agent according to claim 1, characterized in that, The emulsifier is selected from at least one of nonionic polymeric emulsifiers and fatty alcohol polyoxyethylene ethers; And / or, the nonionic polymeric emulsifier is a polyoxyethylene-polyoxypropylene block copolymer with a molecular weight of 2000-5000; the fatty alcohol carbon chain length in the fatty alcohol polyoxyethylene ether is C 12 -C 18 The addition number of ethylene oxide is 5-20.

4. The fluffing and softening agent according to claim 1, characterized in that, The surfactant is selected from at least one of alkyl glycosides and isotridecyl alcohol ethers; And / or, the alkyl carbon chain length in the alkyl glycoside is C8-C9. 14 The isomeric tridecyl alcohol ether is isomeric tridecyl alcohol polyoxyethylene ether, with an ethylene oxide addition number of 7-12.

5. The fluffing and softening agent according to claim 1, characterized in that, The solvent is selected from one or more of isopropanol, propylene glycol, and isododecane.

6. The fluffing and softening agent according to claim 1, characterized in that, The antibacterial agent is selected from one or more of benzyl chloride, polyhexamethylene biguanide hydrochloride, and 2-n-octyl-4-isothiazolin-3-one.

7. The fluffing and softening agent according to claim 1, characterized in that, The pH adjuster is selected from at least one of acetic acid and citric acid.

8. A method for preparing the fluffy softener according to any one of claims 1-7, characterized in that, Includes the following steps: (1) Mix octamethylcyclotetrasiloxane and organosilicon derivatives, add polyether epoxy end-capping agent, heat and react to obtain product A; (2) Mix product A, emulsifier, surfactant and solvent, heat and emulsify to form a uniform emulsion; (3) Cool the emulsion, add antibacterial agent and pH adjuster, homogenize, filter, and obtain the fluffing softener.

9. The preparation method according to claim 8, characterized in that, In step (1), the temperature is raised to 75-85℃ and the reaction is carried out for 3-5 hours. After the reaction, the vacuum is evacuated for 30-50 minutes at a vacuum degree of -0.096MPa to -0.099MPa. In step (2), the temperature is raised to 60-70℃, the emulsification rate is 6000-10000rpm, and the emulsification time is 30-60 minutes.

10. The preparation method according to claim 8, characterized in that, In step (3), the temperature is reduced to below 40°C, and the homogenization conditions are: homogenization is performed at 15-25 MPa and a rotation speed of 2000-4000 rpm for 10-30 minutes.

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