聚酯低温等离子体表面改性及喷墨印花应用性能研究
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摘要
聚酯纤维经过半个多世纪的发展,已经成为纺织纤维的重要原料,不仅在民用纺织品领域使用广泛,工业方面的应用也日益重要。传统聚酯织物的印花主要使用分散染料色浆进行,印花后要采用高温高压蒸化法、热熔法或常压高温连续蒸化法进行固色,固色后还需水洗去除未固色的染料和印花糊料。不仅耗用大量的染化料、蒸汽和水,环境污染严重,而且加工流程长,对花难度大,易产生搭色、渗化等疵病。采用喷墨印花技术对聚酯织物进行印花,可以减轻废水排放及能源消耗,是一种清洁印花方法,而且对纺织品印花技术的升级换代及整个行业的发展具有非常重要意义,前景广阔。
目前聚酯织物喷墨印花工艺主要有三种,一种是分散染料直接喷墨印花,另一种是分散染料转移印花,第三种是颜料墨水喷墨印花。分散染料直接喷墨印花生产工艺复杂,织物需要预处理,印花后需要汽蒸、水洗等后处理,存在一定程度的环境污染。分散染料转移印花是将印花图案直接打印在转移纸上,再通过加热使染料从纸上转移到织物上。不需要预处理,也不需要汽蒸、水洗等后处理,没有污水排放,工艺简单。但是染料利用率不高,印制深浓色图案困难。大量使用的转移印花纸同样会对环境产生污染。颜料墨水喷墨印花原则上不需要预处理,但是聚酯分子结构紧密,对称性高,结晶度高,吸湿性低,在进行喷墨印花时图案容易模糊,表面颜色深度差,为了提高喷墨印花效果需要进行预处理。
聚酯织物颜料墨水喷墨印花的预处理一般采用传统印花糊料(如海藻酸钠、羧甲基纤维素等)或阳离子助剂(如十二烷基三甲基氯化铵、甲基苄基氯化铵、苄基三乙基氯化铵等)进行化学湿加工,存在污染。低温等离子体技术用于织物喷墨印花的预处理加工,不使用水和化学品,仅对纤维材料极浅表面产生作用,纤维整体性能不受影响,是环境友好加工方法。采用不同的等离子体处理方法对聚酯织物进行表面改性,可以提高颜料墨水喷墨印花效果。
射频辉光放电低温O2等离子体处理能改变聚酯织物的表面性能,作用强度和等离子体操作参数有关,较适处理条件是40Pa、80W、7min。改性后织物润湿性能提高,和未处理织物相比,润湿时间下降到52s左右。ATR FT-IR和XPS结果表明,织物表面元素含量发生变化,含C量由75.9%下降到59.3%,含O量由24.1%增加到40.7%,极性含氧官能团增加。SEM和AFM研究揭示纤维表面发生明显刻蚀,光滑表面变得粗糙,有利吸附更多水分子,改善润湿性能。处理后的织物喷墨印花图案边缘线条界面精细度发生变化,经向和纬向喷墨打印直线宽度分别下降35.3%和43.9%;图案表面颜色深度K/S值则增加约54%;实际喷墨印花图案轮廓清晰,表面颜色较深,质量提高。但射频辉光放电是低气压放电,需要真空设备,能耗和成本高,无法连续化加工,实用性受到一定限制。
聚酯织物进行常压介质阻挡放电低温等离子体表面改性,通过在空气中进行放电处理可以降低织物表面的疏水性。改变等离子体处理时间及功率,研究相关参数的变化对织物颜料墨水喷墨印花性能的影响。常压介质阻挡放电低温等离子体处理可以对织物产生刻蚀,使之失重,润湿性能提高。在试验范围内较适处理条件是200W、3min,可以使织物失重约0.86%,润湿时间下降到148s左右。SEM和AFM分析显示,低温等离子体处理可以使织物表面形貌发生变化,粗糙度增加;ATR FT-IR和XPS研究表明处理后织物表面C元素含量下降11.7%,O元素含量上升7.4%。处理后织物喷墨印花图案边缘线条清晰,经、纬向喷墨打印直线宽度分别下降34.8%和40.7%,表面颜色深度提高39.5%,打印效果明显提高,其改性效果接近射频辉光放电低温O2等离子体,但由于该放电使用自然状态的空气产生气体放电等离子体,工艺简单方便,成本低。
等离子体改性后织物表面性能的变化随放置时间延长会逐渐衰退,即具有经时效应。因而织物进行等离子体处理后必须立即喷墨印花,给加工带来很大不便。可以使用等离子体引发亲水性单体表面接枝加以解决。对聚酯织物进行RFGDP表面接枝改性,较适条件为:丙烯酸和丙烯酰胺单体浓度35%,温度30°C,浸渍3h;马来酸酐单体浓度15%,温度70°C,浸渍3h。接枝后的织物表面引入极性羧基或酰胺基,润湿性能提高。经不同单体丙烯酸、丙烯酰胺和马来酸酐接枝后,润湿时间由未处理的大约20min,分别下降到6.44分钟、4.39分钟和2.81分钟;接触角也明显下降。同时对聚酯织物进行APDBDP引发表面接枝改性,改性条件为:丙烯酸和丙烯酰胺单体浓度35%,温度30°C,浸渍3h;马来酸酐单体浓度15%,温度70°C,浸渍3h。改性后织物的润湿性能提高且不随放置时间延长而衰退,效果持久。等离子体表面接枝改性后织物表面形貌发生变化,光滑的表面变得粗糙,喷墨印花时能快速均匀地吸收墨水,使喷墨打印经、纬向直线的宽度减小,表面颜色深度增加,印花图案轮廓鲜明、清晰,喷墨印花质量改善。更为重要的是没有经时效应,可以根据实际使用需要进行后续喷墨印花加工,操作更加方便。
对聚酯织物等离子体改性的经时效应进行了探讨。结果表明,单独的等离子体表面改性具有明显的经时效应,主要是由于织物表面引入的极性基团从表面向本体反转,反转的难易程度受织物放置环境影响很大。温度和湿度是影响等离子体表面处理效果经时效应的重要因素。放置在温度较高、相对湿度较大的环境中,经时效应较明显。而等离子体表面接枝改性所获得的效果则较稳定,不随放置时间的延长而衰减。
经等离子体表面及亲水性单体接枝改性后聚酯织物表面性能发生较大变化,光滑的纤维表面由于等离子体的刻蚀作用变得凹凸不平,含氧极性基团的引入使润湿性能提高,从而有利于改善喷墨印花质量,为颜料墨水喷墨印花技术的推广和应用开辟了新途径。
After half a century of development, polyester fiber has become an important raw material of textile industry. Polyester fiber is not only widely used in civilian areas, and industrial applications are increasingly important. In the conventional textile printing of polyester fabric, the disperse dye is applied with other additional chemicals in the form of a print paste. The print is then normally steamed to fix the dye onto the fabric and then washed thoroughly to remove any unfixed dye, chemicals and thickener. It was high consumption of dye, chemicals, water, steam and energy. And also it is ease to produce taking colour and bleeding, and so on. Polyester fabric inkjet printing technology is a clean printing method and it can reduce waste emissions and energy consumption. This technology can also promote the development of the whole textile printing. The prospects are broad.
The technology of polyester fabric inkjet printing is usually classified into three categories: disperse dye inkjet printing, disperse dye transfer printing and pigment inkjet printing. It is necessary for disperse dye inkjet printing to undertake special pretreatment on the fabric before printing, and the final products must be achieved by steaming and washing. Disperse dye transfer printing is to print directly in the transfer paper, and then the dye transferred from paper to polyester fabric by heat sublimation. The technology has no pretreatment, steam washing and other post-treatment. There is no sewage disposal, and it is a simple process. But the dye utilization is not high and there are some difficulties in printing deep color patterns. A large amount of transfer printing paper will produce the pollution. Pigment-based inks printing undertake no special pretreatment on the fabric before printing. But the molecular structure of the poly(ethylene terephthalate) lacks polar groups, which causes it to have low surface free energy and poor wettability. When polyester fabric is printed with pigment-based inks, the printed patterns have poor color yield and easily bleeding, especially for thin fabric. As a result, the pretreatment process is necessary for the polyester fabric inkjet printing.
Traditional pretreatment method was to use printing paste(such as sodium alginate, carboxymethyl cellulose, and so on) or cationic auxiliary (dodecyl trimethyl ammonium chloride, methyl benzyl ammonium chloride, benzyl triethyl ammonium chloride, and so forth). Although chemical modification of the fibers has been somewhat successful, there are environmental concerns related to the disposal of chemicals after treatment. Plasma treatment of polymeric fibers only affects their surface layer, and does not decrease intrinsic mechanical properties of textile materials. Plasma treatment is a clean, dry and environmental friendly physical technique.
The radio frequency glow discharge low-temperature oxygen plasma treatment can change the surface properties of polyester fabric and the effect of plasma is related to the operating parameters. The optimum treatment condition was as follows: the power 80W, the processing time 7 min, and the pressure 40Pa. Compared to the untreated fabric, the wettability of the modified fabric was improved, and the wetting time was declined to 52s. Attenuated total reflection Fourier infrared spectroscopy (ATR FT-IR) and X-ray photoelectron spectroscopy (XPS) analyses revealed that the element content of the fabric surface was changed. The C element content was decreased from the 75.9% to 59.3%, and the O element content was increased from 24.1% to 40.7%. The polar oxygen group was also increased. These polar groups will incorporate with moisture through hydrogen bonding and help moisture penetration and binding on the fabric surface, which enhances the wettability. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) photographs showed that the surface of fiber was etched and the smooth surface became rough. The warp and weft line width was decreased 35.3% and 43.9%, and the K/S values were increased by approximately 54%. So the pattern effect of ink jet printing was markedly improved. However, the radio frequency glow discharge is low pressure discharge, and it requires vacuum equipment. The energy consumption and costs are high. It is not a continuous process, and the practical applicability is limited.
The atmospheric pressure dielectric barrier discharge plasma treatment can improve the hydrophilicity of the fabric surface by discharge treatment in air. The plasma treatment time and power was changed, and the performance of the pigment-based ink jet printing fabric was researched. In the experimental range, the optimum processing condition was as follows: the power 200W and the processing time l min. After plasma treatment, the weight loss of fabric was about 0.86%, and the wetting time was about 148s. The wettability of polyester fabric was increased. SEM and AFM photographs showed that plasma treatment caused the increase of surface roughness. XPS analyses revealed that plasma treatment introduced an amount of the oxygen containing polar groups on the fabric surface. At the same time, the warp line width was decreased 34.8%, and the weft line width was decreased 40.7%. Therefore, the inkjet printing performance of the fabric was improved. The surface modification effect and quality of ink jet printing was the same as of radio frequency discharge plasma treatment. The discharge was produced using ambient air and the process is simple and convenient, but also the cost is low.
Plasma surface modification has obviously aging effect. It is necessary for the fabric to be inkjet printed after treatment. The inkjet printing effect of polyester fabric can be increased after plasma grafting treatment and also there is no aging effect. It is a convenient and simple pretreatment method. The optimum processing condition of RFGEP surface grafting was as follows: The concentration of acrylic acid and acrylamide was 35%, temperature of 30℃, and dipping 3h. The concentration of maleic anhydride was 15%, temperature of 70℃, and dipping 3h. The enhanced wettability was mainly contributed by some polar groups such as carboxyl and hydroxyl groups induced onto fabric surface through plasma grafting treatment. After grafting, the wetting time was decreased from about 20min to 6.44min, 4.39min and 2.81min respectively, and the contact angle was also decreased. The morphology of fiber and the surface chemical composition was changed, respectively. The warp and the weft line width were greatly decreased and the K/S values were enhanced. The inkjet printing performance was improved. APDBDP surface grafting has the same effect as of RFGEP surface grafting.
In this paper,we also investigate the aging behavior of the plasma treated polyester fabric. The results showed that the surface modification of plasma treatment show the aging process. The fabric surface show a gradual hydrophobicity recovery over the time and the surface properties simultaneously decreases to the original value after plasma treatment. This is due to that the polar groups of the fabric surface were inversed to the body from the surface. The temperature and humidity that the fabric is stored play an important role in the aging process. As the temperature and the humidity are high,the sample exhibits a significant aging process. There is no obviously aging behavior for plasma grafting treated surface. This result indicates that the effect of plasma grafting is more stable than that of plasma surface processing.
The surface performance of the polyester fabric was changed greatly after the plasma modification and plasma grafting. Due to the plasma etching smooth fiber surface became uneven. The wetting properties of the fabric were improved owing to the introduction of oxygen-containing polar groups. So it can be summarized that plasma treatment can enhance the quality of pigment ink jet printing technology. And also a new way was opened up for the promotion and application of pigment inkjet printing technology.
目前聚酯织物喷墨印花工艺主要有三种,一种是分散染料直接喷墨印花,另一种是分散染料转移印花,第三种是颜料墨水喷墨印花。分散染料直接喷墨印花生产工艺复杂,织物需要预处理,印花后需要汽蒸、水洗等后处理,存在一定程度的环境污染。分散染料转移印花是将印花图案直接打印在转移纸上,再通过加热使染料从纸上转移到织物上。不需要预处理,也不需要汽蒸、水洗等后处理,没有污水排放,工艺简单。但是染料利用率不高,印制深浓色图案困难。大量使用的转移印花纸同样会对环境产生污染。颜料墨水喷墨印花原则上不需要预处理,但是聚酯分子结构紧密,对称性高,结晶度高,吸湿性低,在进行喷墨印花时图案容易模糊,表面颜色深度差,为了提高喷墨印花效果需要进行预处理。
聚酯织物颜料墨水喷墨印花的预处理一般采用传统印花糊料(如海藻酸钠、羧甲基纤维素等)或阳离子助剂(如十二烷基三甲基氯化铵、甲基苄基氯化铵、苄基三乙基氯化铵等)进行化学湿加工,存在污染。低温等离子体技术用于织物喷墨印花的预处理加工,不使用水和化学品,仅对纤维材料极浅表面产生作用,纤维整体性能不受影响,是环境友好加工方法。采用不同的等离子体处理方法对聚酯织物进行表面改性,可以提高颜料墨水喷墨印花效果。
射频辉光放电低温O2等离子体处理能改变聚酯织物的表面性能,作用强度和等离子体操作参数有关,较适处理条件是40Pa、80W、7min。改性后织物润湿性能提高,和未处理织物相比,润湿时间下降到52s左右。ATR FT-IR和XPS结果表明,织物表面元素含量发生变化,含C量由75.9%下降到59.3%,含O量由24.1%增加到40.7%,极性含氧官能团增加。SEM和AFM研究揭示纤维表面发生明显刻蚀,光滑表面变得粗糙,有利吸附更多水分子,改善润湿性能。处理后的织物喷墨印花图案边缘线条界面精细度发生变化,经向和纬向喷墨打印直线宽度分别下降35.3%和43.9%;图案表面颜色深度K/S值则增加约54%;实际喷墨印花图案轮廓清晰,表面颜色较深,质量提高。但射频辉光放电是低气压放电,需要真空设备,能耗和成本高,无法连续化加工,实用性受到一定限制。
聚酯织物进行常压介质阻挡放电低温等离子体表面改性,通过在空气中进行放电处理可以降低织物表面的疏水性。改变等离子体处理时间及功率,研究相关参数的变化对织物颜料墨水喷墨印花性能的影响。常压介质阻挡放电低温等离子体处理可以对织物产生刻蚀,使之失重,润湿性能提高。在试验范围内较适处理条件是200W、3min,可以使织物失重约0.86%,润湿时间下降到148s左右。SEM和AFM分析显示,低温等离子体处理可以使织物表面形貌发生变化,粗糙度增加;ATR FT-IR和XPS研究表明处理后织物表面C元素含量下降11.7%,O元素含量上升7.4%。处理后织物喷墨印花图案边缘线条清晰,经、纬向喷墨打印直线宽度分别下降34.8%和40.7%,表面颜色深度提高39.5%,打印效果明显提高,其改性效果接近射频辉光放电低温O2等离子体,但由于该放电使用自然状态的空气产生气体放电等离子体,工艺简单方便,成本低。
等离子体改性后织物表面性能的变化随放置时间延长会逐渐衰退,即具有经时效应。因而织物进行等离子体处理后必须立即喷墨印花,给加工带来很大不便。可以使用等离子体引发亲水性单体表面接枝加以解决。对聚酯织物进行RFGDP表面接枝改性,较适条件为:丙烯酸和丙烯酰胺单体浓度35%,温度30°C,浸渍3h;马来酸酐单体浓度15%,温度70°C,浸渍3h。接枝后的织物表面引入极性羧基或酰胺基,润湿性能提高。经不同单体丙烯酸、丙烯酰胺和马来酸酐接枝后,润湿时间由未处理的大约20min,分别下降到6.44分钟、4.39分钟和2.81分钟;接触角也明显下降。同时对聚酯织物进行APDBDP引发表面接枝改性,改性条件为:丙烯酸和丙烯酰胺单体浓度35%,温度30°C,浸渍3h;马来酸酐单体浓度15%,温度70°C,浸渍3h。改性后织物的润湿性能提高且不随放置时间延长而衰退,效果持久。等离子体表面接枝改性后织物表面形貌发生变化,光滑的表面变得粗糙,喷墨印花时能快速均匀地吸收墨水,使喷墨打印经、纬向直线的宽度减小,表面颜色深度增加,印花图案轮廓鲜明、清晰,喷墨印花质量改善。更为重要的是没有经时效应,可以根据实际使用需要进行后续喷墨印花加工,操作更加方便。
对聚酯织物等离子体改性的经时效应进行了探讨。结果表明,单独的等离子体表面改性具有明显的经时效应,主要是由于织物表面引入的极性基团从表面向本体反转,反转的难易程度受织物放置环境影响很大。温度和湿度是影响等离子体表面处理效果经时效应的重要因素。放置在温度较高、相对湿度较大的环境中,经时效应较明显。而等离子体表面接枝改性所获得的效果则较稳定,不随放置时间的延长而衰减。
经等离子体表面及亲水性单体接枝改性后聚酯织物表面性能发生较大变化,光滑的纤维表面由于等离子体的刻蚀作用变得凹凸不平,含氧极性基团的引入使润湿性能提高,从而有利于改善喷墨印花质量,为颜料墨水喷墨印花技术的推广和应用开辟了新途径。
After half a century of development, polyester fiber has become an important raw material of textile industry. Polyester fiber is not only widely used in civilian areas, and industrial applications are increasingly important. In the conventional textile printing of polyester fabric, the disperse dye is applied with other additional chemicals in the form of a print paste. The print is then normally steamed to fix the dye onto the fabric and then washed thoroughly to remove any unfixed dye, chemicals and thickener. It was high consumption of dye, chemicals, water, steam and energy. And also it is ease to produce taking colour and bleeding, and so on. Polyester fabric inkjet printing technology is a clean printing method and it can reduce waste emissions and energy consumption. This technology can also promote the development of the whole textile printing. The prospects are broad.
The technology of polyester fabric inkjet printing is usually classified into three categories: disperse dye inkjet printing, disperse dye transfer printing and pigment inkjet printing. It is necessary for disperse dye inkjet printing to undertake special pretreatment on the fabric before printing, and the final products must be achieved by steaming and washing. Disperse dye transfer printing is to print directly in the transfer paper, and then the dye transferred from paper to polyester fabric by heat sublimation. The technology has no pretreatment, steam washing and other post-treatment. There is no sewage disposal, and it is a simple process. But the dye utilization is not high and there are some difficulties in printing deep color patterns. A large amount of transfer printing paper will produce the pollution. Pigment-based inks printing undertake no special pretreatment on the fabric before printing. But the molecular structure of the poly(ethylene terephthalate) lacks polar groups, which causes it to have low surface free energy and poor wettability. When polyester fabric is printed with pigment-based inks, the printed patterns have poor color yield and easily bleeding, especially for thin fabric. As a result, the pretreatment process is necessary for the polyester fabric inkjet printing.
Traditional pretreatment method was to use printing paste(such as sodium alginate, carboxymethyl cellulose, and so on) or cationic auxiliary (dodecyl trimethyl ammonium chloride, methyl benzyl ammonium chloride, benzyl triethyl ammonium chloride, and so forth). Although chemical modification of the fibers has been somewhat successful, there are environmental concerns related to the disposal of chemicals after treatment. Plasma treatment of polymeric fibers only affects their surface layer, and does not decrease intrinsic mechanical properties of textile materials. Plasma treatment is a clean, dry and environmental friendly physical technique.
The radio frequency glow discharge low-temperature oxygen plasma treatment can change the surface properties of polyester fabric and the effect of plasma is related to the operating parameters. The optimum treatment condition was as follows: the power 80W, the processing time 7 min, and the pressure 40Pa. Compared to the untreated fabric, the wettability of the modified fabric was improved, and the wetting time was declined to 52s. Attenuated total reflection Fourier infrared spectroscopy (ATR FT-IR) and X-ray photoelectron spectroscopy (XPS) analyses revealed that the element content of the fabric surface was changed. The C element content was decreased from the 75.9% to 59.3%, and the O element content was increased from 24.1% to 40.7%. The polar oxygen group was also increased. These polar groups will incorporate with moisture through hydrogen bonding and help moisture penetration and binding on the fabric surface, which enhances the wettability. Scanning electron microscopy (SEM) and atomic force microscopy (AFM) photographs showed that the surface of fiber was etched and the smooth surface became rough. The warp and weft line width was decreased 35.3% and 43.9%, and the K/S values were increased by approximately 54%. So the pattern effect of ink jet printing was markedly improved. However, the radio frequency glow discharge is low pressure discharge, and it requires vacuum equipment. The energy consumption and costs are high. It is not a continuous process, and the practical applicability is limited.
The atmospheric pressure dielectric barrier discharge plasma treatment can improve the hydrophilicity of the fabric surface by discharge treatment in air. The plasma treatment time and power was changed, and the performance of the pigment-based ink jet printing fabric was researched. In the experimental range, the optimum processing condition was as follows: the power 200W and the processing time l min. After plasma treatment, the weight loss of fabric was about 0.86%, and the wetting time was about 148s. The wettability of polyester fabric was increased. SEM and AFM photographs showed that plasma treatment caused the increase of surface roughness. XPS analyses revealed that plasma treatment introduced an amount of the oxygen containing polar groups on the fabric surface. At the same time, the warp line width was decreased 34.8%, and the weft line width was decreased 40.7%. Therefore, the inkjet printing performance of the fabric was improved. The surface modification effect and quality of ink jet printing was the same as of radio frequency discharge plasma treatment. The discharge was produced using ambient air and the process is simple and convenient, but also the cost is low.
Plasma surface modification has obviously aging effect. It is necessary for the fabric to be inkjet printed after treatment. The inkjet printing effect of polyester fabric can be increased after plasma grafting treatment and also there is no aging effect. It is a convenient and simple pretreatment method. The optimum processing condition of RFGEP surface grafting was as follows: The concentration of acrylic acid and acrylamide was 35%, temperature of 30℃, and dipping 3h. The concentration of maleic anhydride was 15%, temperature of 70℃, and dipping 3h. The enhanced wettability was mainly contributed by some polar groups such as carboxyl and hydroxyl groups induced onto fabric surface through plasma grafting treatment. After grafting, the wetting time was decreased from about 20min to 6.44min, 4.39min and 2.81min respectively, and the contact angle was also decreased. The morphology of fiber and the surface chemical composition was changed, respectively. The warp and the weft line width were greatly decreased and the K/S values were enhanced. The inkjet printing performance was improved. APDBDP surface grafting has the same effect as of RFGEP surface grafting.
In this paper,we also investigate the aging behavior of the plasma treated polyester fabric. The results showed that the surface modification of plasma treatment show the aging process. The fabric surface show a gradual hydrophobicity recovery over the time and the surface properties simultaneously decreases to the original value after plasma treatment. This is due to that the polar groups of the fabric surface were inversed to the body from the surface. The temperature and humidity that the fabric is stored play an important role in the aging process. As the temperature and the humidity are high,the sample exhibits a significant aging process. There is no obviously aging behavior for plasma grafting treated surface. This result indicates that the effect of plasma grafting is more stable than that of plasma surface processing.
The surface performance of the polyester fabric was changed greatly after the plasma modification and plasma grafting. Due to the plasma etching smooth fiber surface became uneven. The wetting properties of the fabric were improved owing to the introduction of oxygen-containing polar groups. So it can be summarized that plasma treatment can enhance the quality of pigment ink jet printing technology. And also a new way was opened up for the promotion and application of pigment inkjet printing technology.
引文
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