CN1908291A - TiO2 nano-sized hydrosol, preparation process thereof and textile finish method - Google Patents
TiO2 nano-sized hydrosol, preparation process thereof and textile finish method Download PDFInfo
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- CN1908291A CN1908291A CN 200610048573 CN200610048573A CN1908291A CN 1908291 A CN1908291 A CN 1908291A CN 200610048573 CN200610048573 CN 200610048573 CN 200610048573 A CN200610048573 A CN 200610048573A CN 1908291 A CN1908291 A CN 1908291A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- 238000000034 method Methods 0.000 title claims abstract description 13
- 239000002105 nanoparticle Substances 0.000 title claims 7
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title abstract description 16
- 239000004753 textile Substances 0.000 title description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims abstract description 60
- 229960000583 acetic acid Drugs 0.000 claims abstract description 30
- 239000012362 glacial acetic acid Substances 0.000 claims abstract description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 29
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000004744 fabric Substances 0.000 claims abstract description 15
- 239000002904 solvent Substances 0.000 claims abstract description 14
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 12
- 239000003054 catalyst Substances 0.000 claims abstract description 10
- 230000007062 hydrolysis Effects 0.000 claims abstract description 8
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 8
- 238000006068 polycondensation reaction Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims description 27
- 239000003153 chemical reaction reagent Substances 0.000 claims description 12
- 229910010413 TiO 2 Inorganic materials 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 8
- 239000007788 liquid Substances 0.000 claims description 7
- 238000003860 storage Methods 0.000 claims description 2
- 238000009988 textile finishing Methods 0.000 claims description 2
- 230000015572 biosynthetic process Effects 0.000 claims 3
- 230000003115 biocidal effect Effects 0.000 claims 1
- 239000002243 precursor Substances 0.000 abstract description 9
- 230000000844 anti-bacterial effect Effects 0.000 abstract description 8
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 239000000675 fabric finishing Substances 0.000 abstract description 3
- 238000009962 finishing (textile) Methods 0.000 abstract description 3
- 231100000252 nontoxic Toxicity 0.000 abstract description 3
- 230000003000 nontoxic effect Effects 0.000 abstract description 3
- 231100000344 non-irritating Toxicity 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 46
- 238000001035 drying Methods 0.000 description 8
- 229920000742 Cotton Polymers 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229920000728 polyester Polymers 0.000 description 3
- 239000002253 acid Substances 0.000 description 2
- 150000007513 acids Chemical class 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000004043 dyeing Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000007730 finishing process Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000002834 transmittance Methods 0.000 description 1
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Abstract
本发明涉及一种TiO2纳米水溶胶及其制备方法及对织物的整理方法，以钛酸丁酯为前驱物，冰乙酸为催化剂，水为溶剂，经过水解、缩聚反应形成的TiO2纳米溶胶整理剂，其组分和重量百分比含量为：钛酸丁酯占1～15％；无水乙醇占1％～20％；冰乙酸占5％～15％；水余量，具有耐洗性、无毒、无刺激、成本低廉、制作工艺简单可靠的优点，可实现对对织物的抗紫外、抗菌、抗静电功能整理。The present invention relates to a kind of TiO2 nano water sol and its preparation method and fabric finishing method, take butyl titanate as precursor, glacial acetic acid as catalyst, water as solvent, the TiO2 nano sol formed by hydrolysis and polycondensation reaction Finishing agent, its components and weight percentage content are: butyl titanate accounts for 1-15%; absolute ethanol accounts for 1%-20%; glacial acetic acid accounts for 5%-15%; With the advantages of non-toxic, non-irritating, low cost, simple and reliable manufacturing process, it can realize the anti-ultraviolet, anti-bacterial and anti-static functional finishing of fabrics.
Description
技术领域technical field
本发明属于化学技术、纺织技术、物理技术相互交叉技术领域，涉及到试剂材料的选取、试剂的制作，尤其涉及一种TiO2纳米水溶胶及其制备方法及对织物的整理方法。The invention belongs to the intercrossing technical fields of chemical technology, textile technology and physical technology, and relates to the selection of reagent materials and the production of reagents, in particular to a TiO2 nanometer water sol and its preparation method and fabric finishing method.
背景技术Background technique
利用溶胶-凝胶技术制备TiO2水溶胶作为抗紫外、抗菌、抗静电功能整理剂。目前织物的抗紫外、抗菌、抗静电功能整理以有机物为主，其存在以下缺陷：(1)大多有机物存在毒性对人身体有害；(2)有机物之间很难进行功能复配。采用溶胶-凝胶技术进行织物功能整理的相关研究也在进行，但存在以下缺点：(1)制备的TiO2溶胶大多为醇溶胶，工业化生产过程中比较危险；(2)使用强酸，如盐酸，对织物强力影响较大。TiO 2 hydrosol was prepared by sol-gel technology as an anti-ultraviolet, antibacterial and antistatic functional finishing agent. At present, the anti-ultraviolet, antibacterial and antistatic functions of fabrics are mainly made of organic substances, which have the following defects: (1) most organic substances are toxic and harmful to human body; (2) it is difficult to carry out functional compounding between organic substances. Relevant research on fabric functional finishing using sol-gel technology is also underway, but there are the following disadvantages: (1) Most of the prepared TiO sols are alcohol sols, which are dangerous in the industrial production process; (2) strong acids such as hydrochloric acid are used , which has a great influence on the strength of the fabric.
发明内容Contents of the invention
本发明的目的在于克服上述现有技术中存在的不足而制备一种具有抗紫外、抗菌、抗静电功能，且无毒、无刺激、成本低廉，耐洗性较好，制作工艺简单的TiO2纳米水溶胶及其制备方法及对织物的整理方法，此功能整理剂是以钛酸丁酯为前驱物，利用溶胶技术制备的功能整理液。The purpose of the present invention is to overcome the deficiencies in the above-mentioned prior art and prepare a TiO2 with anti-ultraviolet, antibacterial, antistatic functions, non-toxic, non-irritating, low cost, good washability, and simple manufacturing process. Nano water sol and its preparation method and fabric finishing method, the functional finishing agent is a functional finishing liquid prepared by sol technology using butyl titanate as a precursor.
本发明的目的是这样实现的：一种TiO2纳米水溶胶，以钛酸丁酯为前驱物，冰乙酸为催化剂，水为溶剂，经过水解、缩聚反应形成的TiO2纳米溶胶整理剂，其组分和重量百分比含量为：钛酸丁酯占1～15％；无水乙醇占1％～20％；冰乙酸占5％～15％；水余量。The object of the present invention is achieved like this: a kind of TiO Nano water sol, take butyl titanate as precursor, glacial acetic acid is catalyst, water is solvent, through the TiO that forms through hydrolysis, polycondensation reaction Nano sol finishing agent, its The components and weight percentages are as follows: 1-15% of butyl titanate; 1-20% of absolute ethanol; 5-15% of glacial acetic acid; and the balance of water.
一种TiO2纳米水溶胶的制备工艺，其制备工艺如下：A kind of TiO The preparation technology of nanometer hydrosol, its preparation technology is as follows:
1)试剂材料的选取：前驱物选取钛酸丁酯，催化剂选取冰乙酸，水为溶剂，无水乙醇为钛酸丁酯的溶剂，1) Selection of reagent materials: butyl titanate is selected as the precursor, glacial acetic acid is selected as the catalyst, water is the solvent, and absolute ethanol is the solvent of butyl titanate.
2)各种预备溶液的配置：将水、1/3的无水乙醇、1/4的冰乙酸搅拌形成A溶液，钛酸丁酯、余量的无水乙醇、3/4的冰乙酸搅拌均匀形成B溶液，2) Configuration of various preparatory solutions: Stir water, 1/3 absolute ethanol, and 1/4 glacial acetic acid to form A solution, stir butyl titanate, the balance of absolute ethanol, and 3/4 glacial acetic acid A solution B is formed uniformly,
3)滴加：在A溶液搅拌的情况下，搅拌速度为1000转/分钟～2000转/分钟，将B溶液缓慢倒入A溶液中，形成C溶液，3) Adding dropwise: when solution A is stirred, the stirring speed is 1000 rpm to 2000 rpm, slowly pour solution B into solution A to form solution C,
4)将C溶液再搅拌30分钟～3小时，形成具有抗紫外、抗菌、抗静电的TiO2纳米水溶胶整理液。4) Stir the C solution for another 30 minutes to 3 hours to form a TiO 2 nanometer hydrosol finishing solution with anti-ultraviolet, antibacterial and antistatic properties.
试剂的水解、缩聚反应温度控制在0℃～30℃，制备出的纳米溶胶整理液存放温度为0～20℃。The temperature of the hydrolysis and polycondensation reaction of the reagent is controlled at 0°C to 30°C, and the storage temperature of the prepared nano-sol finishing solution is 0°C to 20°C.
在制备过程中，试剂的搅拌速度控制在1000转/分钟～2000转/分钟。During the preparation process, the stirring speed of the reagent is controlled at 1000 rpm to 2000 rpm.
在制备过程中，B溶液缓慢倒入A溶液中，1滴/每秒～100滴/每秒。During the preparation process, solution B is slowly poured into solution A, 1 drop/second to 100 drops/second.
一种利用权利要求1所述的纺织品整理试剂对织物的整理方法，其工艺过程如下：A kind of finishing method that utilizes the textile finishing reagent described in claim 1 to fabric, and its technological process is as follows:
1)浸轧，带液量为60％～80％，1) Padding, with liquid volume of 60% to 80%,
2)烘干，烘干温度为80℃，时间为3分钟，2) drying, the drying temperature is 80°C, and the drying time is 3 minutes,
3)焙烘，焙烘温度为130℃～210℃，3) Baking, the baking temperature is 130℃～210℃,
4)热水洗，温度为60℃，时间2-5分钟，4) Washing with hot water at 60°C for 2-5 minutes,
5)烘干，烘干温度为80℃，时间为3分钟。5) Drying, the drying temperature is 80° C., and the drying time is 3 minutes.
本发明具有如下积极效果：The present invention has following positive effects:
所制备的抗静电功能整理剂乙醇用量较少，在制备过程中没有使用盐酸等强酸，对织物的机械性能影响较小。使用的材料TiO2为无毒材料，用其处理过的纺织品符合国家环保标准。本发明采用的工艺比较简单，投资非常少，所用的材料采购容易，适合大规模化生产。所整理过的棉织物紫外效果明显增加，UVA和UVB段的紫外透过率分别从22.83％和14.85％降为14.37％和0.67％，UPF值从6.03上升为56.7，按照欧洲标准草案规定，UPF级为50+，具有很好的抗紫外效果。整理后的棉织物抑菌率为99％。整理过的涤纶织物在相对湿度为40％条件下表面电阻从1014降到1011，整理后的棉织物的白度CIE值由原来的66.5变为67.7，涤纶织物的白度CIE值由原来的84.2变为80.8，整理剂对织物白度影响不大，基本不影响织物的后续染色性能。The prepared antistatic functional finishing agent uses less ethanol, does not use strong acids such as hydrochloric acid in the preparation process, and has little influence on the mechanical properties of the fabric. The material TiO 2 used is a non-toxic material, and the textiles treated with it meet the national environmental protection standard. The technology adopted in the invention is relatively simple, the investment is very small, the materials used are easy to purchase, and are suitable for large-scale production. The UV effect of the finished cotton fabric was significantly increased, the UV transmittance of UVA and UVB segments decreased from 22.83% and 14.85% to 14.37% and 0.67% respectively, and the UPF value increased from 6.03 to 56.7. According to the draft European standard, UPF The grade is 50+ , which has very good anti-ultraviolet effect. The antibacterial rate of the finished cotton fabric is 99%. The surface resistance of the finished polyester fabric decreased from 10 14 to 10 11 at a relative humidity of 40%, the whiteness CIE value of the finished cotton fabric changed from 66.5 to 67.7, and the whiteness CIE value of the polyester fabric changed from the original 84.2 to 80.8, the finishing agent has little effect on the whiteness of the fabric, and basically does not affect the subsequent dyeing performance of the fabric.
具体实施方式Detailed ways
实施例1：以钛酸丁酯为前驱物，冰乙酸为催化剂，水为溶剂，经过水解、缩聚反应形成的TiO2纳米溶胶整理剂，其组分和重量含量为：钛酸丁酯占1克；无水乙醇占1克；冰乙酸占5克；水93克。Embodiment 1: with butyl titanate as precursor, glacial acetic acid as catalyst, water as solvent, through hydrolysis, the TiO2 nano-sol finishing agent that polycondensation reaction forms, its component and weight content are: butyl titanate accounts for 1 grams; 1 gram of absolute ethanol; 5 grams of glacial acetic acid; 93 grams of water.
其制备工艺如下：Its preparation process is as follows:
1)试剂材料的选取：前驱物选取钛酸丁酯，催化剂选取冰乙酸，水为溶剂，无水乙醇为钛酸丁酯的溶剂，1) Selection of reagent materials: butyl titanate is selected as the precursor, glacial acetic acid is selected as the catalyst, water is the solvent, and absolute ethanol is the solvent of butyl titanate.
2)各种预备溶液的配置：将水、1/3的无水乙醇、1/4的冰乙酸搅拌形成A溶液，钛酸丁酯、余量的无水乙醇、3/4的冰乙酸搅拌均匀形成B溶液，2) Configuration of various preparatory solutions: Stir water, 1/3 absolute ethanol, and 1/4 glacial acetic acid to form A solution, stir butyl titanate, the balance of absolute ethanol, and 3/4 glacial acetic acid A solution B is formed uniformly,
3)滴加：在A溶液搅拌的情况下，搅拌速度为1000转/分钟～2000转/分钟，将B溶液缓慢倒入A溶液中，形成C溶液，3) Adding dropwise: when solution A is stirred, the stirring speed is 1000 rpm to 2000 rpm, slowly pour solution B into solution A to form solution C,
4)将C溶液再搅拌30分钟～3小时，形成具有抗紫外、抗菌、抗静电的TiO2纳米水溶胶整理液。4) Stir the C solution for another 30 minutes to 3 hours to form a TiO 2 nanometer hydrosol finishing solution with anti-ultraviolet, antibacterial and antistatic properties.
实施例2：以钛酸丁酯为前驱物，冰乙酸为催化剂，水为溶剂，经过水解、缩聚反应形成的TiO2纳米溶胶整理剂，其组分和重量含量为：钛酸丁酯占15克；无水乙醇占20克；冰乙酸占15克；水50克。Embodiment 2: with butyl titanate as precursor, glacial acetic acid as catalyst, water as solvent, through hydrolysis, the TiO2 nanometer sol finishing agent that polycondensation reaction forms, its component and weight content are: butyl titanate accounts for 15 grams; 20 grams of absolute ethanol; 15 grams of glacial acetic acid; 50 grams of water.
其制备工艺如下：Its preparation process is as follows:
1)试剂材料的选取：前驱物选取钛酸丁酯，催化剂选取冰乙酸，水为溶剂，无水乙醇为钛酸丁酯的溶剂，1) Selection of reagent materials: butyl titanate is selected as the precursor, glacial acetic acid is selected as the catalyst, water is the solvent, and absolute ethanol is the solvent of butyl titanate.
2)各种预备溶液的配置：将水、1/3的无水乙醇、1/4的冰乙酸搅拌形成A溶液，钛酸丁酯、余量的无水乙醇、3/4的冰乙酸搅拌均匀形成B溶液，2) Configuration of various preparatory solutions: Stir water, 1/3 absolute ethanol, and 1/4 glacial acetic acid to form A solution, stir butyl titanate, the balance of absolute ethanol, and 3/4 glacial acetic acid A solution B is formed uniformly,
3)滴加：在A溶液搅拌的情况下，搅拌速度为1000转/分钟～2000转/分钟，将B溶液缓慢倒入A溶液中，形成C溶液，3) Adding dropwise: when solution A is stirred, the stirring speed is 1000 rpm to 2000 rpm, slowly pour solution B into solution A to form solution C,
4)将C溶液再搅拌30分钟～3小时，形成具有抗紫外、抗菌、抗静电的TiO2纳米水溶胶整理液。4) Stir the C solution for another 30 minutes to 3 hours to form a TiO 2 nanometer hydrosol finishing solution with anti-ultraviolet, antibacterial and antistatic properties.
实施例3：以钛酸丁酯为前驱物，冰乙酸为催化剂，水为溶剂，经过水解、缩聚反应形成的TiO2纳米溶胶整理剂，其组分和重量含量为：钛酸丁酯占2.08g；无水乙醇占3.16克；冰乙酸占12.22克；水82.54克。Embodiment 3: with butyl titanate as precursor, glacial acetic acid as catalyst, water as solvent, through hydrolysis, the TiO2 nano-sol finishing agent that polycondensation reaction forms, its component and weight content are: butyl titanate accounts for 2.08 g; absolute ethanol accounts for 3.16 grams; glacial acetic acid accounts for 12.22 grams; water 82.54 grams.
其制作工艺如下：Its production process is as follows:
1)将1.05g无水乙醇、3.06g冰乙酸和82.54g水混合，在温度为10℃左右，转速为1600转/分的磁力搅拌器上搅拌一段时间后形成均匀、透明的A溶液。1) Mix 1.05g of absolute ethanol, 3.06g of glacial acetic acid and 82.54g of water, and stir for a period of time on a magnetic stirrer with a temperature of about 10°C and a speed of 1600 rpm to form a uniform and transparent A solution.
2)将2.08g钛酸丁酯加入到2.11g无水乙醇和9.16g冰乙酸混合溶液中，搅拌均匀后，形成滴加液B。2) Add 2.08g of butyl titanate into a mixed solution of 2.11g of absolute ethanol and 9.16g of glacial acetic acid, and stir evenly to form a dropwise solution B.
3)将B溶液缓慢倒入A溶液中，倒入过程中磁力搅拌器一直搅拌。倒完后继续搅拌1.5小时即形成抗静电溶胶整理液，存放在广口瓶中，密封包存。存放温度在6℃。3) Slowly pour solution B into solution A, and keep stirring with a magnetic stirrer during the pouring process. After pouring, continue to stir for 1.5 hours to form an antistatic sol finishing solution, store it in a jar, and keep it sealed. Store at 6°C.
实施例4：功能整理剂制备实例，其制作工艺如下：Embodiment 4: the preparation example of functional finishing agent, its preparation process is as follows:
1)将4.36g无水乙醇、2.53g冰乙酸和68.22g水混合，在温度为10℃左右，转速为1600转/分的磁力搅拌器上搅拌一段时间后形成均匀、透明的A溶液。1) Mix 4.36g of absolute ethanol, 2.53g of glacial acetic acid and 68.22g of water, and stir for a period of time on a magnetic stirrer with a temperature of about 10°C and a speed of 1600 rpm to form a uniform and transparent A solution.
2)将8.60g钛酸丁酯加入到8.71g无水乙醇和7.58g冰乙酸混合溶液中，搅拌均匀后，形成滴加液B。2) Add 8.60 g of butyl titanate into a mixed solution of 8.71 g of absolute ethanol and 7.58 g of glacial acetic acid, and stir evenly to form a dropwise solution B.
3)将B溶液缓慢倒入A溶液中，倒入过程中磁力搅拌器一直搅拌。倒完后继续搅拌1.5小时即形成抗静电溶胶整理液，存放在广口瓶中，密封包存。存放温度在6℃。3) Slowly pour solution B into solution A, and keep stirring with a magnetic stirrer during the pouring process. After pouring, continue to stir for 1.5 hours to form an antistatic sol finishing solution, store it in a jar, and keep it sealed. Store at 6°C.
实施例5：功能整理剂制备实例，其制作工艺如下：Embodiment 5: the preparation example of functional finishing agent, its preparation process is as follows:
1)将5.86g无水乙醇、2.66g冰乙酸和57.34g水混合，在温度为10℃左右，转速为1600转/分的磁力搅拌器上搅拌一段时间后形成均匀、透明的A溶液。1) Mix 5.86g of absolute ethanol, 2.66g of glacial acetic acid and 57.34g of water, and stir for a period of time on a magnetic stirrer with a temperature of about 10°C and a speed of 1600 rpm to form a uniform and transparent A solution.
2)将14.44g钛酸丁酯加入到11.73g无水乙醇和7.97g冰乙酸混合溶液中，搅拌均匀后，形成滴加液B。2) Add 14.44g of butyl titanate into a mixed solution of 11.73g of absolute ethanol and 7.97g of glacial acetic acid, and stir evenly to form a dropwise solution B.
3)将B溶液缓慢倒入A溶液中，倒入过程中磁力搅拌器一直搅拌。倒完后继续搅拌1.5小时即形成抗静电溶胶整理液，存放在广口瓶中，密封包存。存放温度在6℃。3) Slowly pour solution B into solution A, and keep stirring with a magnetic stirrer during the pouring process. After pouring, continue to stir for 1.5 hours to form an antistatic sol finishing solution, store it in a jar, and keep it sealed. Store at 6°C.
使用上述功能整理液对织物的整理工艺：The finishing process of the fabric using the above-mentioned functional finishing liquid:
首先将功能整理液稀释到一定浓度(0.2～0.4mol/L)，然后采用下列工艺过程：浸轧(带液量70～80％)→烘干(80℃，3min)→焙烘(170℃，棉150℃，涤纶170℃，3min)→热水洗→烘干(80℃，3min)First, dilute the functional finishing solution to a certain concentration (0.2-0.4mol/L), and then adopt the following process: padding (with liquid amount of 70-80%)→drying (80°C, 3min)→baking (170°C , cotton 150°C, polyester 170°C, 3min) → hot water washing → drying (80°C, 3min)
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