CN109137491B - A self-cleaning textile supported with Ag6Si2O7@AgCl@Ag and its finishing method - Google Patents
A self-cleaning textile supported with Ag6Si2O7@AgCl@Ag and its finishing method Download PDFInfo
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
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Abstract
本发明公开了一种负载Ag6Si2O7@AgCl@Ag自清洁纺织品整理方法，包括以下步骤：S01，将织物进行预处理；S02，将S01预处理后的织物进行浸泡处理，具体为：21)，称取九水合偏硅酸钠和硝酸银，分别加入到去离子水中，超声20～40min至完全溶解，分别得到溶液C和溶液D，22)，S01中所得的织物置于溶液C中，振荡100～130min，23)，用胶头滴管逐滴滴加溶液D，继续避光振荡50～70min，24)，取出织物，去离子水清洗，50～70℃烘至干燥；S03，将步骤S02中所得的织物放入到氯化钠溶液中，避光振荡0.5～3h。本发明还公开了一种负载Ag6Si2O7@AgCl@Ag自清洁纺织品，由上述制备方法得到。本发明的一种负载Ag6Si2O7@AgCl@Ag自清洁纺织品及其整理方法，制备方法简单易行、合成条件温和，纺织品具有高效持久的自清洁性。The invention discloses a self-cleaning textile finishing method loaded with Ag 6 Si 2 O 7 @AgCl@Ag, comprising the following steps: S01, pretreating the fabric; S02, soaking the fabric after the S01 pretreatment, specifically: : 21), take sodium metasilicate nonahydrate and silver nitrate, respectively join in deionized water, ultrasonic 20～40min to dissolve completely, obtain solution C and solution D respectively, 22), the fabric of gained in S01 is placed in solution In C, vibrate for 100-130min, 23), add solution D dropwise with a plastic tip dropper, continue to shake in the dark for 50-70min, 24), take out the fabric, rinse with deionized water, and bake at 50-70°C until dry; S03, putting the fabric obtained in step S02 into a sodium chloride solution, and shaking in the dark for 0.5 to 3 hours. The invention also discloses a self-cleaning textile supported by Ag 6 Si 2 O 7 @AgCl@Ag, which is obtained by the above preparation method. The Ag 6 Si 2 O 7 @AgCl@Ag self-cleaning textile supported by the invention and the finishing method thereof have the advantages of simple and easy preparation method, mild synthesis conditions, and high-efficiency and long-lasting self-cleaning properties of the textile.
Description
技术领域technical field
本发明涉及一种负载Ag6Si2O7@AgCl@Ag自清洁纺织品及其整理方法，属于纺织材料及其制备技术领域。The invention relates to a self-cleaning textile supported by Ag 6 Si 2 O 7 @AgCl@Ag and a finishing method thereof, belonging to the technical field of textile materials and their preparation.
背景技术Background technique
纺织品由于其自身的微孔结构，长期以来被人们认为是最适合真菌和细菌等微生物滋生和繁殖的温床，而自清洁纺织品不仅能很好地去除咖啡和红酒等有机污物，而且能有效防止微生物污染。开发负载光催化剂的纺织品，不仅可以减少衣物的洗涤次数或实现衣物免洗，从而减少洗涤剂的使用，最终达到节能、节水和环境友好的目的，而且还具有抗菌、防紫外和抗静电等功能。因此，在当前环境污染日趋严峻的条件下，开发光催化自清洁纺织品将具有非常广阔的市场空间和现实意义。Textiles have long been considered to be the most suitable breeding grounds for microorganisms such as fungi and bacteria due to their own microporous structure, and self-cleaning textiles can not only remove organic contaminants such as coffee and red wine well, but also effectively prevent Microbial contamination. The development of photocatalyst-loaded textiles can not only reduce the number of washings of clothes or realize the no-washing of clothes, thereby reducing the use of detergents, and ultimately achieve the purpose of energy saving, water saving and environmental friendliness, but also have antibacterial, anti-ultraviolet and antistatic properties, etc. Function. Therefore, under the current conditions of increasingly severe environmental pollution, the development of photocatalytic self-cleaning textiles will have a very broad market space and practical significance.
发明内容SUMMARY OF THE INVENTION
本发明要解决的技术问题是，克服现有技术的缺陷，提供一种具有高效持久自清洁性的负载Ag6Si2O7@AgCl@Ag自清洁纺织品及其整理方法。The technical problem to be solved by the present invention is to overcome the defects of the prior art and provide a self-cleaning textile supported by Ag 6 Si 2 O 7 @AgCl@Ag with high efficiency and lasting self-cleaning properties and a finishing method thereof.
为解决上述技术问题，本发明采用的技术方案为：In order to solve the above-mentioned technical problems, the technical scheme adopted in the present invention is:
一种负载Ag6Si2O7@AgCl@Ag自清洁纺织品整理方法，包括以下步骤：A self-cleaning textile finishing method loaded with Ag 6 Si 2 O 7 @AgCl@Ag, comprising the following steps:
S01，将织物进行预处理，具体为：S01, the fabric is pretreated, specifically:
11)，将去离子水和无水乙醇按体积比1:1混合后，得到溶液A，11), after deionized water and absolute ethanol are mixed by volume 1:1, solution A is obtained,
12)，加入3-氨基丙基三乙氧基硅烷，在40～60℃时，振荡 50～70min，得到溶胶B，12), add 3-aminopropyltriethoxysilane, and shake at 40～60℃ for 50～70min to obtain sol B,
13)，将洗涤干燥后的织物在溶胶B中避光浸泡100～120min后，取出、轧压，90～100℃烘20～40min，155～175℃烘3～5min，去离子水清洗，50～70℃烘至干燥；13), soak the washed and dried fabric in sol B for 100-120 minutes in the dark, take it out, roll and press, bake at 90-100°C for 20-40 minutes, bake at 155-175°C for 3-5 minutes, rinse with deionized water, 50 Bake to dry at ~70℃;
S02，将S01预处理后的织物进行浸泡处理，具体为：S02, soaking the fabric pretreated in S01, specifically:
21)，称取九水合偏硅酸钠和硝酸银，分别加入到去离子水中，超声20～40min至完全溶解，分别得到溶液C和溶液D，21), take by weighing sodium metasilicate nonahydrate and silver nitrate, add into deionized water respectively, ultrasonicate 20～40min to dissolve completely, obtain solution C and solution D respectively,
22)，S01中所得的织物置于溶液C中，振荡100～130min，22), the fabric obtained in S01 is placed in solution C,
23)，用胶头滴管逐滴滴加溶液D，继续避光振荡50～70min，23), add solution D drop by drop with a plastic tip dropper, continue to shake for 50-70 min in the dark,
24)，取出织物，去离子水清洗，50～70℃烘至干燥；24), take out the fabric, wash with deionized water, and bake at 50-70°C until dry;
S03，将步骤S02中所得的织物放入到氯化钠溶液中，避光振荡 0.5～3h。S03, put the fabric obtained in step S02 into a sodium chloride solution, and oscillate in the dark for 0.5-3h.
S03中，氯化钠的浓度为1～3mmol/L。In S03, the concentration of sodium chloride is 1-3 mmol/L.
S02中，偏硅酸钠和硝酸银的摩尔比1:3。In S02, the molar ratio of sodium metasilicate and silver nitrate is 1:3.
S01中，3-氨基丙基三乙氧基硅烷质量为溶液A质量的3～6％。In S01, the mass of 3-aminopropyltriethoxysilane is 3-6% of the mass of solution A.
S01中，织物轧压的轧余率为95～100％。In S01, the nip rate of the fabric rolling is 95-100%.
一种负载Ag6Si2O7@AgCl@Ag自清洁纺织品，由上述任意所述一种负载Ag6Si2O7@AgCl@Ag自清洁纺织品整理方法制备得到。A self-cleaning textile supported by Ag 6 Si 2 O 7 @AgCl@Ag is prepared by any of the above-mentioned finishing methods for self-cleaning textile supported by Ag 6 Si 2 O 7 @AgCl@Ag.
本发明的有益效果：本发明提供的一种负载 Ag6Si2O7@AgCl@Ag自清洁纺织品及其整理方法，制备方法简单易行、合成条件温和，纺织品具有高效持久的自清洁性。经3-氨基丙基三乙氧基硅烷预处理的纺织品，浸泡硝酸银溶液，氨基与银离子形成配位键；再浸泡九水合偏硅酸钠，银离子与硅酸根离子结合生成焦硅酸银；最后浸泡氯化钠溶液，银离子与氯离子结合，生成 Ag6Si2O7@AgCl，在光照下，银离子被还原成银，从而生成负载Ag6Si2O7@AgCl@Ag纺织品。在可见光下，3-5分钟对甲基橙的降解率达98％。制备的自清洁纺织品，能够多次洗涤，重复使用，降解率保持在95％左右。Beneficial effects of the present invention: The Ag6Si2O7@AgCl@Ag self-cleaning textile and its finishing method provided by the present invention have simple and easy preparation method, mild synthesis conditions, and the textile has efficient and lasting self-cleaning. Textiles pretreated with 3-aminopropyltriethoxysilane are soaked in silver nitrate solution, and the amino groups and silver ions form coordination bonds; then soaked in sodium metasilicate nonahydrate, silver ions combine with silicate ions to form pyrosilicic acid Silver; finally soaked in sodium chloride solution, silver ions combine with chloride ions to form Ag6Si2O7@AgCl, and under light, silver ions are reduced to silver, thereby forming supported Ag6Si2O7@AgCl@Ag textiles. Under visible light, the degradation rate of methyl orange reaches 98% in 3-5 minutes. The prepared self-cleaning textile can be washed and reused for many times, and the degradation rate is maintained at about 95%.
附图说明Description of drawings
图1是棉织物和负载Ag6Si2O7@AgCl@Ag棉织物的X射线衍射图谱；Figure 1 is the X-ray diffraction pattern of cotton fabric and Ag 6 Si 2 O 7 @AgCl@Ag cotton fabric;
图2是织物的扫描电子显微镜照片；Fig. 2 is the scanning electron microscope photograph of fabric;
图3是在可见光下对甲基橙的降解率；Fig. 3 is the degradation rate to methyl orange under visible light;
图4是在可见光下负载Ag6Si2O7@AgCl@Ag棉织物对甲基橙的重复降解率。Figure 4 is the repeated degradation rate of methyl orange on the Ag 6 Si 2 O 7 @AgCl@Ag cotton fabric supported under visible light.
具体实施方式Detailed ways
下面结合附图对本发明作进一步描述，以下实施例仅用于更加清楚地说明本发明的技术方案，而不能以此来限制本发明的保护范围。The present invention will be further described below with reference to the accompanying drawings. The following embodiments are only used to more clearly illustrate the technical solutions of the present invention, and cannot be used to limit the protection scope of the present invention.
本发明通过制备多组分、多相复合的负载Ag6Si2O7@AgCl@Ag 自清洁纺织品，能够发挥各组分的优势，从而提高自清洁性能。By preparing multi-component and multi-phase composite loaded Ag 6 Si 2 O 7 @AgCl@Ag self-cleaning textiles, the present invention can exert the advantages of each component, thereby improving the self-cleaning performance.
具体实施例1Specific Example 1
一种负载Ag6Si2O7@AgCl@Ag自清洁纺织品整理方法，包括以下步骤：A self-cleaning textile finishing method loaded with Ag 6 Si 2 O 7 @AgCl@Ag, comprising the following steps:
步骤一，将织物进行预处理，具体为：
11)，将去离子水和无水乙醇按体积比1:1混合后，得到溶液A，11), after deionized water and absolute ethanol are mixed by volume 1:1, solution A is obtained,
12)，向溶液A中加入3-氨基丙基三乙氧基硅烷，3-氨基丙基三乙氧基硅烷质量为溶液A质量的3～6％，优选为3％，在40℃时，振荡50min，得到溶胶B，12), adding 3-aminopropyl triethoxysilane to solution A, the mass of 3-aminopropyl triethoxysilane is 3 to 6% of the mass of solution A, preferably 3%, at 40°C, Shake for 50min to obtain sol B,
13)，将洗涤干燥后的织物在溶胶B中避光浸泡100min后，取出、轧压，轧余率为95～100％，优选为95％。90℃烘20min，155℃烘3min，去离子水清洗，50℃烘至干燥。13), soak the washed and dried fabric in the sol B for 100 minutes in the dark, then take it out, roll and press, and the overage rate is 95-100%, preferably 95%. Bake at 90°C for 20 minutes, bake at 155°C for 3 minutes, rinse with deionized water, and bake at 50°C until dry.
步骤二，将步骤1预处理后的织物进行浸泡处理，具体为：
21)，称取九水合偏硅酸钠和硝酸银，偏硅酸钠和硝酸银的摩尔比1:3。分别加入到去离子水中，超声20min至完全溶解，分别得到溶液C和溶液D，21), weigh sodium metasilicate nonahydrate and silver nitrate, and the molar ratio of sodium metasilicate and silver nitrate is 1:3. were added to deionized water, ultrasonicated for 20min to complete dissolution, respectively, to obtain solution C and solution D,
22)，步骤1中所得的织物置于溶液C中，振荡100min，22), the fabric obtained in
23)，用胶头滴管逐滴滴加溶液D，继续避光振荡50min，23), add solution D dropwise with a plastic tip dropper, continue to shake for 50min in the dark,
24)，取出织物，去离子水清洗，50℃烘至干燥。24), take out the fabric, wash with deionized water, and bake at 50°C until dry.
步骤三，将步骤步骤2中所得的织物放入到氯化钠溶液中，氯化钠的浓度为1～3mmol/L，优选为1mmol/L，避光振荡0.5h。
一种负载Ag6Si2O7@AgCl@Ag自清洁纺织品，由上述一种负载 Ag6Si2O7@AgCl@Ag自清洁纺织品整理方法制备得到。A self-cleaning textile supported by Ag 6 Si 2 O 7 @AgCl@Ag is prepared by the above-mentioned finishing method of self-cleaning textile supported by Ag 6 Si 2 O 7 @AgCl@Ag.
具体实施例2
一种负载Ag6Si2O7@AgCl@Ag自清洁纺织品整理方法，包括以下步骤：A self-cleaning textile finishing method loaded with Ag 6 Si 2 O 7 @AgCl@Ag, comprising the following steps:
步骤一，将织物进行预处理，具体为：
11)，将去离子水和无水乙醇按体积比1:1混合后，得到溶液A，11), after deionized water and absolute ethanol are mixed by volume 1:1, solution A is obtained,
12)，向溶液A中加入3-氨基丙基三乙氧基硅烷，3-氨基丙基三乙氧基硅烷质量为溶液A质量的3～6％，优选为4.5％，在50℃时，振荡60min，得到溶胶B，12), adding 3-aminopropyl triethoxysilane to solution A, the mass of 3-aminopropyl triethoxysilane is 3-6% of the mass of solution A, preferably 4.5%, at 50°C, Shake for 60min to obtain sol B,
13)，将洗涤干燥后的织物在溶胶B中避光浸泡110min后，取出、轧压，轧余率为95～100％，优选为98％。95℃烘30min，165℃烘4min，去离子水清洗，60℃烘至干燥。13), soak the washed and dried fabric in the sol B for 110 minutes in the dark, then take it out, roll and press, and the overage rate is 95-100%, preferably 98%. Bake at 95°C for 30 minutes, 165°C for 4 minutes, rinse with deionized water, and bake at 60°C until dry.
步骤二，将步骤1预处理后的织物进行浸泡处理，具体为：
21)，称取九水合偏硅酸钠和硝酸银，偏硅酸钠和硝酸银的摩尔比1:3。分别加入到去离子水中，超声30min至完全溶解，分别得到溶液C和溶液D，21), weigh sodium metasilicate nonahydrate and silver nitrate, and the molar ratio of sodium metasilicate and silver nitrate is 1:3. were added to deionized water, ultrasonicated for 30min to completely dissolve, respectively, to obtain solution C and solution D,
22)，步骤1中所得的织物置于溶液C中，振荡115min，22), the fabric obtained in
23)，用胶头滴管逐滴滴加溶液D，继续避光振荡60min，23), add solution D dropwise with a plastic tip dropper, continue to shake in the dark for 60min,
24)，取出织物，去离子水清洗，60℃烘至干燥。24), take out the fabric, wash with deionized water, and bake at 60°C until dry.
步骤三，将步骤步骤2中所得的织物放入到氯化钠溶液中，氯化钠的浓度为1～3mmol/L，优选为2mmol/L，避光振荡1.5h。
一种负载Ag6Si2O7@AgCl@Ag自清洁纺织品，由上述一种负载 Ag6Si2O7@AgCl@Ag自清洁纺织品整理方法制备得到。A self-cleaning textile supported by Ag 6 Si 2 O 7 @AgCl@Ag is prepared by the above-mentioned finishing method of self-cleaning textile supported by Ag 6 Si 2 O 7 @AgCl@Ag.
具体实施例3
一种负载Ag6Si2O7@AgCl@Ag自清洁纺织品整理方法，包括以下步骤：A self-cleaning textile finishing method loaded with Ag 6 Si 2 O 7 @AgCl@Ag, comprising the following steps:
步骤一，将织物进行预处理，具体为：
11)，将去离子水和无水乙醇按体积比1:1混合后，得到溶液A，11), after deionized water and absolute ethanol are mixed by volume 1:1, solution A is obtained,
12)，向溶液A中加入3-氨基丙基三乙氧基硅烷，3-氨基丙基三乙氧基硅烷质量为溶液A质量的3～6％，优选为6％，在,60℃时，振荡70min，得到溶胶B，12), add 3-aminopropyl triethoxysilane to solution A, the mass of 3-aminopropyl triethoxysilane is 3 to 6% of the mass of solution A, preferably 6%, at 60° C. , shake for 70min to obtain sol B,
13)，将洗涤干燥后的织物在溶胶B中避光浸泡120min后，取出、轧压，轧余率为100％，优选为。100℃烘40min，175℃烘 5min，去离子水清洗，70℃烘至干燥。13), soak the washed and dried fabric in the sol B for 120 minutes in the dark, then take it out, roll and press, and the overage rate is 100%, preferably . Bake at 100°C for 40 minutes, 175°C for 5 minutes, rinse with deionized water, and bake at 70°C until dry.
步骤二，将步骤1预处理后的织物进行浸泡处理，具体为：
21)，称取九水合偏硅酸钠和硝酸银，偏硅酸钠和硝酸银的摩尔比1:3。分别加入到去离子水中，超声40min至完全溶解，分别得到溶液C和溶液D，21), weigh sodium metasilicate nonahydrate and silver nitrate, and the molar ratio of sodium metasilicate and silver nitrate is 1:3. were added to deionized water respectively, and ultrasonicated for 40min to completely dissolve, respectively, to obtain solution C and solution D,
22)，步骤1中所得的织物置于溶液C中，振荡130min，22), the fabric of gained in
23)，用胶头滴管逐滴滴加溶液D，继续避光振荡70min，23), add solution D drop by drop with a plastic tip dropper, continue to shake for 70min in the dark,
24)，取出织物，去离子水清洗，70℃烘至干燥。24), take out the fabric, wash with deionized water, and bake at 70°C until dry.
步骤三，将步骤步骤2中所得的织物放入到氯化钠溶液中，氯化钠的浓度为1～3mmol/L，优选为3mmol/L，避光振荡3h。
一种负载Ag6Si2O7@AgCl@Ag自清洁纺织品，由上述一种负载 Ag6Si2O7@AgCl@Ag自清洁纺织品整理方法制备得到。A self-cleaning textile supported by Ag 6 Si 2 O 7 @AgCl@Ag is prepared by the above-mentioned finishing method of self-cleaning textile supported by Ag 6 Si 2 O 7 @AgCl@Ag.
如图1所示，(a)是棉织物的X射线衍射图谱，(b)是负载 Ag6Si2O7@AgCl@Ag棉织物的X射线衍射图谱。As shown in Figure 1, (a) is the X-ray diffraction pattern of the cotton fabric, and (b) is the X-ray diffraction pattern of the Ag 6 Si 2 O 7 @AgCl@Ag cotton fabric supported.
如图2所示，(a)为棉织物；(b)为负载Ag6Si2O7棉织物；(c) 为负载Ag6Si2O7@AgCl@Ag棉织物As shown in Figure 2, (a) is cotton fabric; (b) is Ag 6 Si 2 O 7 supported cotton fabric; (c) is Ag 6 Si 2 O 7 @AgCl@Ag supported cotton fabric
如图3所示，(a)对应负载Ag6Si2O7棉织物；(b)对应负载Ag6Si2O7@AgCl@Ag棉织物，从图中可以看出，负载 Ag6Si2O7@AgCl@Ag棉织物对甲基橙的降解率远高于负载Ag6Si2O7棉织物，基本接近100％。As shown in Figure 3, (a) corresponds to the loaded Ag 6 Si 2 O 7 cotton fabric; (b) corresponds to the loaded Ag 6 Si 2 O 7 @AgCl@Ag cotton fabric. It can be seen from the figure that the loaded Ag 6 Si 2 The degradation rate of O 7 @AgCl@Ag cotton fabric to methyl orange is much higher than that of Ag 6 Si 2 O 7 loaded cotton fabric, which is basically close to 100%.
如图4所示，经过三次重复使用后，Ag6Si2O7@AgCl@Ag棉织物对甲基橙的降解率依然很高，可以循环再生使用。As shown in Figure 4, after three repeated uses, the Ag 6 Si 2 O 7 @AgCl@Ag cotton fabric still has a high degradation rate of methyl orange and can be recycled.
以上所述仅是本发明的优选实施方式，应当指出：对于本技术领域的普通技术人员来说，在不脱离本发明原理的前提下，还可以做出若干改进和润饰，这些改进和润饰也应视为本发明的保护范围。The above is only the preferred embodiment of the present invention, it should be pointed out: for those skilled in the art, under the premise of not departing from the principle of the present invention, several improvements and modifications can also be made, and these improvements and modifications are also It should be regarded as the protection scope of the present invention.
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