A surfactant for fabric treatment capable of withstanding low temperatures and a preparation method thereof
By preparing and combining cationic surfactants, the problem of poor bonding strength between surfactants and fabrics in the prior art is solved, and the effect of efficiently treating fabrics under low temperature conditions is achieved, and a variety of properties of the fabrics are enhanced.
Patent Information
- Application Number
- CN202411551379.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-11-01
- Publication Date
- 2025-02-25
- Estimated Expiration
- 2044-11-01
AI Technical Summary
In the prior art, the binding force of surfactants and fabrics is poor, the adsorption efficiency is low, and it is difficult to effectively treat textiles under low temperature conditions.
The cationic surfactant 1 was prepared by using epoxychlorohydrin, modified silicone oil and dibasic acid as raw materials, and combined with carboxyethylthiosuccinic acid to obtain a low temperature-resistant bimini quaternary ammonium surfactant. The surfactant has higher binding sites and adsorption efficiency, and can effectively treat fabrics under low temperature conditions.
It realizes the effect of efficiently treating fabrics under low temperature conditions, enhances the softness, smoothness and antistatic properties of the fabrics, and also has a bactericidal effect.
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Abstract
Description
Technical Field
[0001] The invention belongs to the technical field of fabric treating agents, and in particular relates to a low-temperature resistant surfactant for fabric treating and a preparation method thereof. Background Art
[0002] Textile products are closely related to our lives. Contemporary textiles are not limited to the field of clothing, but are increasingly used in various fields. In traditional cotton printing and dyeing, a pre-treatment at 100°C is required to achieve a certain whiteness and wool effect of the fabric, and then dyeing, soap boiling, and finishing are essential processes. In the current trend of "saving energy and reducing consumption", "reducing sewage discharge", "reducing costs", and "saving resources", it is necessary to develop new auxiliaries for energy saving and emission reduction to meet the needs of market competition in the printing and dyeing industry today.
[0003] The Chinese patent with announcement number CN109267404B discloses a low-temperature post-treatment auxiliary agent for dyeing pure polyester and polyester-containing fabrics and a post-treatment process thereof. The post-treatment auxiliary agent is composed of Rongalit, biological enzyme and Gemini cationic surfactant, which can remove floating color on the surface of the fabric. Rongalit can make the floating color on the surface of the fabric fall off from the fabric, the biological enzyme can remove the floating color on the fabric and degrade and decolorize the floating color that falls into the solution, and the micelle molecules of the Gemini cationic surfactant can remove the floating color on the fabric and accommodate the fallen floating color to prevent re-contamination. The three have an excellent synergistic mechanism in the post-treatment of polyester fabric dyeing, which can not only improve the fastness, reduce the post-treatment temperature, but also reduce the chromaticity value of the wastewater. The Chinese patent with publication number CN105155249A discloses a low-temperature scouring agent, a preparation method thereof and a use thereof. The low-temperature scouring agent consists of a low-temperature bleaching agent and a low-temperature oxygen bleaching activator, wherein the low-temperature bleaching agent consists of alkaline pectinase, sodium butyl ricinoleate sulfate, alkyl alcohol amide polyoxyethylene ether and a silicone defoamer; the low-temperature oxygen bleaching activator consists of cocamidopropyl betaine, a chelating dispersant, an activator promoter, an alkali agent and water. The alkaline pectinase can effectively remove starch and deformed starch from fabrics, is biodegradable, and does not pollute the environment. The surfactant sodium butyl ricinoleate sulfate has a wetting effect and can weaken the adhesion between oil wax and fabrics. The non-ionic surfactant alkyl alcohol amide polyoxyethylene ether has a strong emulsifying ability and can effectively reduce surface tension, improve the permeability of alkali solution and the wettability of cotton fibers.
[0004] However, the existing surfactants have poor binding force with fabrics and low adsorption efficiency. Therefore, the development of efficient, environmentally friendly and energy-saving surfactants for fabric treatment is an urgent problem to be solved in the current textile dyeing and finishing industry. Summary of the invention
[0005] In order to solve the problems existing in the prior art, the present invention provides a surfactant for fabric treatment that can withstand low temperatures and a preparation method thereof. A cationic surfactant is prepared by using epichlorohydrin, modified silicone oil and dibasic acid as raw materials, and is further compounded with carboxyethyl thiosuccinic acid to obtain a surfactant for fabric treatment that can withstand low temperatures.
[0006] In order to achieve the above object, the present invention provides the following technical solutions:
[0007] A method for preparing a surfactant for fabric treatment that is resistant to low temperatures, comprising the following steps:
[0008] S1. Add hydrogen-containing silicone oil to a reaction bottle, stir and heat it to 75-85°C, add 3-(dimethylamino) propyl acrylate, stir evenly and add the catalyst, raise the temperature to 100-110°C after the addition is completed and maintain the reaction for 6-8h to ensure that the reaction is fully carried out, and distill under reduced pressure after the reaction is completed to obtain modified silicone oil; wherein the catalyst is a mixture of chloroplatinic acid and isopropanol in proportion; the mass ratio of chloroplatinic acid to isopropanol is 1:95-105; the catalyst is added dropwise to prevent the reaction from releasing heat and causing the temperature to rise too quickly; the molar ratio of silicon-hydrogen bond to olefin double bond n (Si-H): n (C=C) is 1:1.1-1.5; the amount of the catalyst is 3.5-6.5 mg / L;
[0009] In this step, hydrogenated silicone oil and 3-(dimethylamino)propyl acrylate are used as raw materials, chloroplatinic acid is used as a catalyst, and modified silicone oil is prepared by hydrosilylation reaction. The main chain of organic silicon is a spiral straight-chain molecular structure, composed of alternating silicon and oxygen atoms, and the energy of rotation around the Si-O bond is zero, and it can rotate 360 degrees freely, so that the main chain of polysiloxane has good flexibility; the flexibility of the main chain of Si-O bond reduces the static friction coefficient between fabric fibers, and the fibers can start to slide with less force, which can make the fabric have a soft and smooth touch; in addition, ester groups are introduced in the modification process, and surfactants with ester groups in the structure have lower irritation and higher biodegradability than traditional surfactants;
[0010] S2. Under an inert atmosphere, add epichlorohydrin to the reactor, heat it to 85-95°C, add dibasic acid, stir evenly, add acidic cationic resin, raise the temperature to 95-110°C, heat and react for 15-20h, perform vacuum distillation after the reaction is completed, separate excess epichlorohydrin, and wash the residue with petroleum ether for 3-5 times to obtain an intermediate; wherein the mass ratio of epichlorohydrin, suberic acid and acidic cationic resin is 24-30:8-12:1;
[0011] S3. Add solvent A, intermediate, modified silicone oil and sodium carbonate to the reactor under stirring, heat to 135-150°C and reflux for reaction for 4-8h; after the reaction, remove the solvent by distillation under reduced pressure, and obtain a cationic surfactant 1 after recrystallization of the residue from acetone; wherein the recrystallization times are 2-3 times; the mass ratio of the intermediate, modified silicone oil and sodium carbonate is 7-10:18-25:0.2-0.5, and the amount of sodium carbonate in acetone is 0.008-0.012g / mL;
[0012] Surfactant is a chemical substance that can effectively reduce the surface tension of a solvent by adding a small amount. The molecular structure of surfactant is usually composed of a solvent-loving group (hydrophilic group) and a solvent-hating group (hydrophobic group). Existing surfactants are usually single-chain and have insufficient bonding strength with fabrics. Therefore, in steps S2 and S3, epichlorohydrin, dibasic acid and modified silicone oil are used to obtain a gemini quaternary ammonium salt surfactant. Compared with traditional single-chain surfactants, it has more binding sites with fabrics and increases the contact area, so it has better surface activity and biological activity. The two charged groups contained in it can be adsorbed on the fabric surface faster, so it has a higher adsorption efficiency on the fabric surface than single-charged surfactants; the synthesized surfactant easily absorbs water and forms a conductive solution layer on the fabric surface, which has an antistatic effect; in addition, since the quaternary ammonium salt surfactant is a cationic surfactant, it can adsorb negatively charged bacteria through electrostatic force, hydrogen bonding force and hydrophobic bonding between surfactant molecules and protein molecules, and aggregate on the cell wall, producing a chamber resistance effect, resulting in bacterial growth inhibition and death, so it has a bactericidal effect;
[0013] S4. Add cationic surfactant 1 and carboxyethyl thiosuccinic acid into solvent B in proportion, mix and stir evenly to obtain the surfactant for fabric treatment; wherein the mass ratio of cationic surfactant 1 to carboxyethyl thiosuccinic acid is 2-5:1; the amount of carboxyethyl thiosuccinic acid in solvent B is 0.4-0.8 g / mL, and solvent B is deionized water.
[0014] Carboxyethyl thiosuccinic acid contains a strong polar sulfur group with strong electron-withdrawing ability, which can weaken the attraction between normal alkanes in the cotton wax structure, make the alkane molecules in the solid wax crystals loosely arranged, and can quickly soften paraffin under low temperature conditions, destroying the continuous wax film layer on the fabric surface; by compounding carboxyethyl thiosuccinic acid with a cationic surfactant, a relatively excellent fabric treatment effect can be obtained under low temperature conditions.
[0015] Furthermore, in step S2, the structural formula of the dibasic acid is COOH-(CH2) n -COOH, wherein n is a positive integer not less than 4 and not more than 10; preferably n is 8.
[0016] Furthermore, in step S2, the inert atmosphere is a nitrogen atmosphere or an argon atmosphere; preferably an argon atmosphere.
[0017] Furthermore, in step S3, the solvent A is any one of acetone, acetonitrile, ethanol, and isopropanol; preferably acetone.
[0018] The present invention also provides a low-temperature resistant surfactant for fabric treatment, wherein the surfactant for fabric treatment is obtained by using the preparation method of any one of the above technical solutions.
[0019] The present invention has the following beneficial effects:
[0020] The present invention uses epichlorohydrin, modified silicone oil and dibasic acid as raw materials to prepare a cationic surfactant, and further compounding with carboxyethyl thiosuccinic acid to obtain a low-temperature resistant gemini quaternary ammonium surfactant for fabric treatment. Hydrogen-containing silicone oil and 3-(dimethylamino)propyl acrylate are used as raw materials, chloroplatinic acid is used as a catalyst, and the modified silicone oil is prepared by hydrosilylation reaction; the polysiloxane main chain has good flexibility, can effectively reduce the static friction coefficient between fabric fibers, and makes the fabric soft and smooth to the touch; in addition, an ester group is introduced, so that the prepared surfactant has lower irritation and higher biodegradability. Compared with traditional single-chain surfactants, the prepared surfactant has two charged groups and can be adsorbed on the surface of fabrics more quickly, with higher adsorption efficiency; the synthesized surfactant easily absorbs water to form a conductive solution layer on the surface of the fabric, and has an antistatic effect; in addition, since the quaternary ammonium salt surfactant belongs to a cationic surfactant, it can adsorb negatively charged bacteria through electrostatic force, hydrogen bond force, and hydrophobic binding between surfactant molecules and protein molecules, and aggregate on the cell wall to produce a chamber resistance effect, resulting in the inhibition of bacterial growth and death, and thus has a bactericidal effect; on the other hand, the addition of carboxyethyl thiosuccinic acid introduces a strong polar sulfur group with strong electron-withdrawing ability, which can weaken the attraction between normal alkanes in the cotton wax structure, can quickly soften paraffin under low temperature conditions, and destroy the continuous wax film layer on the surface of the fabric; by compounding carboxyethyl thiosuccinic acid with a cationic surfactant, a relatively excellent fabric treatment effect can be obtained under low temperature conditions. DETAILED DESCRIPTION
[0021] The following will be combined with the embodiments of the present application to clearly and completely describe the technical solutions in the embodiments of the present application. Obviously, the described embodiments are only part of the embodiments of the present application, not all of the embodiments. Based on the embodiments in the present application, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of this application.
[0022] The hydrogen-containing silicone oil (industrial grade, 0.8% hydrogen content) used in the present invention was purchased from Zhejiang Hengyecheng Silicone Co., Ltd.; 3-(dimethylamino)propyl acrylate (purity 95%) and suberic acid (analytical grade) were purchased from Shanghai Aladdin Biochemical Technology Co., Ltd.; chloroplatinic acid hexahydrate (analytical grade) was purchased from Shanghai Titan Technology Co., Ltd.; isopropanol (analytical grade) was purchased from Xilong Science Co., Ltd.; epichlorohydrin, petroleum ether, acetone, and sodium carbonate were all analytically pure and purchased from Xi'an Sanpu Chemical Reagent Company; acidic cationic resin (industrial grade) was purchased from Cangzhou Baoen Company; carboxyethyl thiosuccinic acid (industrial grade) was purchased from Shanghai Xihe Fine Chemical Co., Ltd. All reagents are commercially available.
[0023] Embodiment 1
[0024] A method for preparing a surfactant for fabric treatment that is resistant to low temperatures, comprising the following steps:
[0025] S1. Add hydrogen-containing silicone oil to a reaction bottle, stir and heat it to 80°C, add 3-(dimethylamino) propyl acrylate, stir evenly and then add the catalyst. After the addition is completed, increase the temperature to 105°C and maintain the reaction for 8 hours to ensure that the reaction is fully carried out. After the reaction is completed, perform vacuum distillation to obtain modified silicone oil; wherein the catalyst is a mixture of chloroplatinic acid and isopropanol in proportion; the mass ratio of chloroplatinic acid to isopropanol is 1:100; the catalyst is added dropwise to prevent the reaction from releasing heat and causing the temperature to rise too quickly; wherein the molar ratio of silicon-hydrogen bond to olefin double bond n (Si-H): n (C=C) is 1:1.2; the amount of the catalyst is 5 mg / L;
[0026] S2. Under an argon atmosphere, epichlorohydrin was added to the reactor, the temperature was raised to 90°C, suberic acid was added, the acidic cationic resin was added after stirring, the temperature was raised to 100°C, and the reaction was heated for 18 hours. After the reaction was completed, the excess epichlorohydrin was separated by distillation under reduced pressure, and the residue was washed with petroleum ether 5 times to obtain an intermediate; wherein the mass ratio of epichlorohydrin, suberic acid, and acidic cationic resin was 25:9:1;
[0027] S3. Under stirring, add acetone, intermediate, modified silicone oil and sodium carbonate to the reactor, heat to 145°C and reflux for 6 hours; after the reaction, remove the solvent by distillation under reduced pressure, and obtain a cationic surfactant 1 by recrystallization of the residue from acetone; wherein the recrystallization times are 2 times; wherein the mass ratio of the intermediate, modified silicone oil and sodium carbonate is 8:21:0.3, and the amount of sodium carbonate in acetone is 0.010 g / mL;
[0028] S4. Add cationic surfactant 1 and carboxyethyl thiosuccinic acid into deionized water, mix and stir evenly to obtain a surfactant for fabric treatment; wherein the mass ratio of cationic surfactant 1 to carboxyethyl thiosuccinic acid is 4:1; and the amount of carboxyethyl thiosuccinic acid in deionized water is 0.6 g / mL.
[0029] Embodiment 2
[0030] Compared with the first embodiment, this embodiment has the following differences:
[0031] In step S1, hydrogen-containing silicone oil is added to a reaction bottle, stirred and heated to 75°C, and after adding the catalyst, the temperature is raised to 100°C and the reaction is maintained for 6 hours, wherein the catalyst is a mixture of chloroplatinic acid and isopropanol in proportion; the mass ratio of chloroplatinic acid to isopropanol is 1:95; the molar ratio of silicon-hydrogen bond to olefin double bond n (Si-H): n (C=C) is 1:1.1; the amount of the catalyst is 3.5 mg / L;
[0032] In step S2, epichlorohydrin is added to the reactor, the temperature is raised to 85° C., suberic acid is added, and the acidic cationic resin is added, the temperature is raised to 95° C., and the reaction is heated for 15 hours. The residue is washed with petroleum ether three times to obtain an intermediate; wherein the mass ratio of epichlorohydrin, suberic acid, and acidic cationic resin is 24:8:1;
[0033] In step S3, solvent A, intermediate, modified silicone oil and sodium carbonate are added to the reactor and then heated to 135° C. for reflux reaction for 4 hours; the number of recrystallizations is 2 times; the mass ratio of the intermediate, modified silicone oil and sodium carbonate is 7:18:0.2, and the amount of sodium carbonate in acetone is 0.008 g / mL;
[0034] In step S4, the mass ratio of cationic surfactant 1 to carboxyethyl thiosuccinic acid is 2:1; the amount of carboxyethyl thiosuccinic acid in solvent B is 0.4 g / mL.
[0035] Embodiment 3
[0036] Compared with the first embodiment, this embodiment has the following differences:
[0037] In step S1, hydrogen-containing silicone oil is added to a reaction bottle, stirred and heated to 85°C, and after adding the catalyst, the temperature is raised to 110°C and the reaction is maintained for 8 hours, wherein the catalyst is a mixture of chloroplatinic acid and isopropanol in proportion; the mass ratio of chloroplatinic acid to isopropanol is 1:105; the molar ratio of silicon-hydrogen bond to olefin double bond n (Si-H): n (C=C) is 1:1.5; the amount of the catalyst is 6.5 mg / L;
[0038] In step S2, epichlorohydrin is added to the reactor, the temperature is raised to 95° C., suberic acid is added, and the acidic cationic resin is added, the temperature is raised to 110° C., and the reaction is heated for 20 hours. The residue is washed with petroleum ether for 5 times to obtain an intermediate; wherein the mass ratio of epichlorohydrin, suberic acid, and acidic cationic resin is 30:12:1;
[0039] In step S3, solvent A, intermediate, modified silicone oil and sodium carbonate are added to the reactor and then heated to 150° C. for reflux reaction for 8 hours; the number of recrystallizations is 3 times; the mass ratio of the intermediate, modified silicone oil and sodium carbonate is 10:25:0.5, and the amount of sodium carbonate in acetone is 0.012 g / mL;
[0040] In step S4, the mass ratio of cationic surfactant 1 to carboxyethyl thiosuccinic acid is 5:1; the amount of carboxyethyl thiosuccinic acid in solvent B is 0.8 g / mL.
[0041] Embodiment 4
[0042] Compared with the first embodiment, this embodiment has the following differences:
[0043] In step S1, hydrogen-containing silicone oil is added to a reaction bottle, stirred and heated to 80°C, and after adding the catalyst, the temperature is raised to 100°C and the reaction is maintained for 8 hours, wherein the catalyst is a mixture of chloroplatinic acid and isopropanol in proportion; the mass ratio of chloroplatinic acid to isopropanol is 1:102; the molar ratio of silicon-hydrogen bond to olefin double bond n (Si-H): n (C=C) is 1:1.3; the amount of the catalyst is 4.5 mg / L;
[0044] In step S2, epichlorohydrin is added to the reactor, the temperature is raised to 90° C., suberic acid is added, and the acidic cationic resin is added, the temperature is raised to 100° C., and the reaction is heated for 20 hours. The residue is washed with petroleum ether for 5 times to obtain an intermediate; wherein the mass ratio of epichlorohydrin, suberic acid, and acidic cationic resin is 28:11:1;
[0045] In step S3, solvent A, intermediate, modified silicone oil and sodium carbonate are added to the reactor and then heated to 140° C. for reflux reaction for 8 hours; the number of recrystallizations is 2 times; the mass ratio of the intermediate, modified silicone oil and sodium carbonate is 8:222:0.25, and the amount of sodium carbonate in acetone is 0.009 g / mL;
[0046] In step S4, the mass ratio of cationic surfactant 1 to carboxyethyl thiosuccinic acid is 3.5:1; the amount of carboxyethyl thiosuccinic acid in solvent B is 0.55 g / mL.
[0047] Comparative Example 1
[0048] Compared with Example 1, in the preparation process, the modified silicone oil was replaced with a long-chain alkane, and the rest was referred to Example 1, as follows:
[0049] A method for preparing a surfactant for fabric treatment that is resistant to low temperatures, comprising the following steps:
[0050] S1. Under argon atmosphere, epichlorohydrin was added to the reactor, and suberic acid was added after heating to 90°C. After stirring, an acidic cationic resin was added, and the temperature was raised to 100°C for heating and reaction for 18 hours. After the reaction was completed, the excess epichlorohydrin was separated by distillation under reduced pressure, and the residue was washed with petroleum ether 5 times to obtain an intermediate; wherein the mass ratio of epichlorohydrin, suberic acid, and acidic cationic resin was 25:9:1;
[0051] S2. Under stirring, acetone, intermediate, octadecyl dimethyl ammonium and sodium carbonate were added to the reactor, and the mixture was heated to 145° C. and refluxed for 6 hours; after the reaction, the solvent was removed by distillation under reduced pressure, and the residue was recrystallized from acetone to obtain a cationic surfactant II; wherein the recrystallization was performed twice; wherein the mass ratio of the intermediate, octadecyl dimethyl ammonium and sodium carbonate was 8:21:0.3, and the amount of sodium carbonate in acetone was 0.010 g / mL;
[0052] S3. Add cationic surfactant II and carboxyethyl thiosuccinic acid into deionized water, mix and stir evenly to obtain a surfactant for fabric treatment; wherein the mass ratio of cationic surfactant II to carboxyethyl thiosuccinic acid is 4:1; and the amount of carboxyethyl thiosuccinic acid in deionized water is 0.6 g / mL.
[0053] Comparative Example 2
[0054] Compared with Example 1, in the preparation process, carboxyethyl thiosuccinic acid was not added, and the prepared cationic surfactant 1 was used as the surfactant for fabric treatment, and the rest was referred to Example 1.
[0055] Comparative Example 3
[0056] Compared with Example 1, this comparative example does not modify the hydrogen-containing silicone oil during the preparation process, and the rest is referred to Example 1, as follows:
[0057] S1. Under argon atmosphere, epichlorohydrin was added to the reactor, and suberic acid was added after heating to 90°C. After stirring, an acidic cationic resin was added, and the temperature was raised to 100°C for heating and reaction for 18 hours. After the reaction was completed, the excess epichlorohydrin was separated by distillation under reduced pressure, and the residue was washed with petroleum ether 5 times to obtain an intermediate; wherein the mass ratio of epichlorohydrin, suberic acid, and acidic cationic resin was 25:9:1;
[0058] S2, add acetone, intermediate, 3-(dimethylamino) propyl acrylate, hydrogen-containing silicone oil and sodium carbonate into the reactor, heat to 145 ° C and reflux for 6 hours; after the reaction, remove the solvent by distillation under reduced pressure, and obtain cationic surfactant three by recrystallization of the residue from acetone; wherein the number of recrystallizations is 2 times; wherein the mass ratio of the intermediate, 3-(dimethylamino) propyl acrylate, hydrogen-containing silicone oil and sodium carbonate is 8:12:4:0.3, and the amount of sodium carbonate in acetone is 0.010 g / mL;
[0059] S3. Add cationic surfactant III, hydrogen-containing silicone oil and carboxyethyl thiosuccinic acid into deionized water, mix and stir evenly to obtain a surfactant for fabric treatment; wherein the mass ratio of cationic surfactant III, hydrogen-containing silicone oil and carboxyethyl thiosuccinic acid is 4:2:1; and the amount of carboxyethyl thiosuccinic acid in deionized water is 0.6 g / mL.
[0060] Comparative Example 4
[0061] Compared with Example 1, this comparative example does not add hydrogen-containing silicone oil during the preparation process, and the rest is referred to Example 1, as follows:
[0062] S1. Under argon atmosphere, epichlorohydrin was added to the reactor, and suberic acid was added after heating to 90°C. After stirring, an acidic cationic resin was added, and the temperature was raised to 100°C for heating and reaction for 18 hours. After the reaction was completed, the excess epichlorohydrin was separated by distillation under reduced pressure, and the residue was washed with petroleum ether 5 times to obtain an intermediate; wherein the mass ratio of epichlorohydrin, suberic acid, and acidic cationic resin was 25:9:1;
[0063] S2, add acetone, intermediate, 3-(dimethylamino) propyl acrylate and sodium carbonate into the reactor, heat to 145 ℃ and reflux for 6h; after the reaction, remove the solvent by distillation under reduced pressure, and obtain cationic surfactant four after the residue is recrystallized from acetone; wherein the number of recrystallizations is 2 times; wherein the mass ratio of the intermediate, 3-(dimethylamino) propyl acrylate and sodium carbonate is 8:15:0.3, and the amount of sodium carbonate in acetone is 0.010g / mL;
[0064] S3. Add cationic surfactant tetrakis and carboxyethyl thiosuccinic acid into deionized water, mix and stir evenly to obtain a surfactant for fabric treatment; wherein the mass ratio of cationic surfactant tetrakis and carboxyethyl thiosuccinic acid is 4:1; and the amount of carboxyethyl thiosuccinic acid in deionized water is 0.6 g / mL.
[0065] Related tests:
[0066] Fabric treatment: The white cotton grey cloth was cut into square pieces of 120 mm × 120 mm, corresponding to Examples 1 to 4, Comparative Examples 1 to 4 and a blank control group, respectively; the fabrics were respectively dipped and rolled in the surfactants for fabric treatment prepared in each embodiment and comparative example, using one dip and one roll, with a liquid rate of 60%-70%, and then dried for use, wherein the blank control group was not treated. The test results are shown in Table 1.
[0067] Test standard:
[0068] 1. Breaking strength: The breaking strength is measured using a YG601 strength meter in accordance with GB / T3923.1-1997 "Textile fabrics - Determination of breaking strength and elongation at break - Strip method";
[0069] 2. Fabric whiteness test: Fabric whiteness test is carried out in accordance with GB / T 8424.2-2001 "Textiles - Tests for colour fastness - Instrumental evaluation method for relative whiteness", using SC-80 automatic colourimeter;
[0070] 3. Fabric softness test: Fabric softness is tested using the DCP-RRY1000 computer-controlled softness tester. The force required to fold the fabric is used as the test index. The smaller the force required, the better the softness of the fabric.
[0071] 4. Fabric abrasion resistance test: The abrasion resistance of fabric is tested using a Y522 disc type fabric flat abrader, with the number of revolutions when the first hole appears in the fabric as the test index.
[0072] Table 1 Performance test results
[0073]
[0074] From the above test results, it can be found that the test results of Examples 1 to 4 are better than those of Comparative Examples 1 to 4, among which the test result of Example 1 is the best; from the test results of breaking strength, it can be seen that the breaking strength of the fabric after being finished with the surfactant prepared by the present invention is increased, because the surfactant prepared by the present invention can penetrate into the interior of the cotton fabric, and the siloxane main chain has relatively excellent flexibility, and can form a protective layer on the surface of the cotton fiber, reduce the friction between the fibers, and enable them to be effectively gathered when subjected to external force, increase the ability to resist external force, thereby effectively improving the breaking strength of the fabric, and at the same time, the presence of the siloxane main chain effectively improves the softness of the fabric; from the whiteness test results, it can be seen that the effect of surfactant finishing on the whiteness of the fabric is not significant; from the wear resistance test, it can be seen that after being finished with surfactant, it can form a protective film on the surface of the fabric, reduce the friction between the fabric and external objects, and increase the wear resistance of the fabric.
[0075] It should be noted that, in this article, relational terms such as first and second, etc. are only used to distinguish one entity or operation from another entity or operation, and do not necessarily require or imply any such actual relationship or order between these entities or operations. Moreover, the terms "include", "comprise" or any other variants thereof are intended to cover non-exclusive inclusion, so that a process, method, article or device including a series of elements includes not only those elements, but also other elements not explicitly listed, or also includes elements inherent to such process, method, article or device.
[0076] Although the embodiments of the present application have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present application, and that the scope of the present application is defined by the appended claims and their equivalents.
Claims
1. A method for preparing a surfactant for fabric treatment that is resistant to low temperatures, characterized in that: The following steps are involved: S1. Add hydrogen-containing silicone oil to a reaction bottle, stir and heat to 75-85°C, add 3-(dimethylamino)propyl acrylate, stir evenly and then add a catalyst, raise the temperature to 100-110°C after the addition is completed, react for 6-8h, and perform reduced pressure distillation after the reaction is completed to obtain modified silicone oil; S2. In an inert atmosphere, epichlorohydrin is added to the reactor, and after heating to the reflux temperature, a dibasic acid is added, and after stirring evenly, an acidic cationic resin is added, and the reaction is heated. After the reaction is completed, the reaction is distilled under reduced pressure, and an intermediate is obtained after separation and washing; S3, adding solvent A, intermediate, modified silicone oil and sodium carbonate to the reactor under stirring, heating and reflux reaction; after the reaction, distill under reduced pressure, and obtain cationic surfactant 1 after recrystallization; S4. Add cationic surfactant 1 and carboxyethyl thiosuccinic acid into solvent B in proportion, mix and stir evenly to obtain the surfactant for fabric treatment.
2. The method for preparing the low-temperature resistant surfactant for fabric treatment according to claim 1, characterized in that: In step S1, the catalyst is prepared by mixing chloroplatinic acid and isopropanol in a certain proportion.
3. The method for preparing the low-temperature resistant surfactant for fabric treatment according to claim 1, characterized in that: In step S1, the catalyst is added dropwise.
4. The method for preparing the low-temperature resistant surfactant for fabric treatment according to claim 1, characterized in that: In step S2, the structural formula of the dibasic acid is COOH-(CH2) n -COOH, wherein n is a positive integer not less than 4 and not more than 8.
5. The method for preparing the low-temperature resistant surfactant for fabric treatment according to claim 1, characterized in that: In step S2, the inert atmosphere is a nitrogen atmosphere or an argon atmosphere.
6. The method for preparing the low-temperature resistant surfactant for fabric treatment according to claim 1, characterized in that: In step S2, petroleum ether is used for washing 3-5 times.
7. The method for preparing the low-temperature resistant surfactant for fabric treatment according to claim 1, characterized in that: In step S3, the solvent A is any one of acetone, acetonitrile, ethanol and isopropanol.
8. The method for preparing the low-temperature resistant surfactant for fabric treatment according to claim 1, characterized in that: In step S4, the mass ratio of the cationic surfactant 1 to carboxyethyl thiosuccinic acid is 2-5:
1.
9. The method for preparing the low-temperature resistant surfactant for fabric treatment according to claim 1, characterized in that: In step S4, solvent B is deionized water.
10. A surfactant for fabric treatment that is resistant to low temperatures, characterized in that: The surfactant for fabric treatment is obtained by the preparation method according to any one of claims 1 to 9.
Citation Information
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