CN101876143A - A method for modifying nylon fabric by using butyl titanate - Google Patents

Abstract

The invention discloses a method for modifying nylon fabric by using butyl titanate. The nylon fabric to be modified is respectively treated with deionized water and 95% absolute ethanol at a temperature of 60-90°C. Repeated ultrasonic vibration cleaning, drying and standby; weigh nylon fabric and butyl titanate according to the mass ratio of 1 to 3:1, dissolve butyl titanate in deionized water at a volume ratio of 1:20 to 100, and then dissolve the nylon fabric The fabric is immersed in the butyl titanate solution for 5-10 minutes, then the butyl titanate solution impregnated with the nylon fabric is added to the high-temperature and high-pressure reaction kettle, sealed, and treated at a constant temperature of 110-140°C for 3-6 hours, and the reaction The finished nylon fabric is washed with washing liquid at 70-90°C for 10-20 minutes at a bath ratio of 1:30-50, washed repeatedly with hot and cold water, dried or naturally dried to obtain the modified nylon fabric. fabric. The method of the invention saves raw materials, is easy to operate, and the prepared modified nylon fabric has good washing resistance.

Description

A method for modifying nylon fabric by using butyl titanate

technical field

The invention belongs to the technical field of functional textile materials, and relates to a method for modifying nylon fabric, in particular to a method for modifying nylon fabric by using butyl titanate.

Background technique

Anatase phase nano-titanium dioxide powder is an oxide wide-bandgap semiconductor material that has attracted much attention today. It has excellent anti-ultraviolet and antibacterial functions. Combining it with ordinary textile materials can protect people from ultraviolet rays and reduce disease transmission. , so it has very important practical application value and development prospect. At present, the methods for preparing nano-titanium dioxide mainly include sol-gel method, uniform precipitation method, microemulsion method and hydrothermal method, etc. Among them, the hydrothermal method is environmentally friendly and high in purity, and the prepared nanoparticles are uniform and well dispersed without high temperature. Burning, easy to achieve industrial production of high-quality products and other advantages. Nylon fabric has excellent strength and wear resistance, not only can be used as clothing fabrics such as down jackets and mountaineering suits, but also widely used in decorative and industrial fabrics, but its heat resistance and light resistance are poor.

At present, there are two main methods for surface modification of nylon fabrics: one is to prepare functional fibers containing nanoparticles, that is, to disperse nanoparticles in chemical fiber raw materials during the spinning process, and then spin them into fibers. Long-lasting, the disadvantage is that the affinity between nanoparticles and polymer materials is poor, the dispersion of nanoparticles is uneven, and the agglomeration phenomenon is serious. Most of the nanoparticles are embedded in the fiber matrix, and there are few nanoparticles on the surface of the fiber, so the functionality is greatly reduced. The second is to use the post-finishing process to arrange the nanoparticles to the surface of the fabric, usually using raw materials such as adhesives and auxiliary agents, so it also faces the problem of nanoparticle agglomeration, and the fabric after finishing has poor washing fastness. The taking performance is affected, and the hand feeling is obviously deteriorated.

Contents of the invention

The purpose of the present invention is to provide a method for modifying nylon fabric by using butyl titanate, which solves the problem that the nylon fabric prepared by the existing modification method has low anti-ultraviolet and antibacterial properties, and the washing resistance is not durable. The problem of poor ventilation performance.

The technical scheme adopted in the present invention is, a kind of method that adopts butyl titanate to modify nylon fabric, concretely implement according to the following steps:

Step 1: Wash the nylon fabric to be modified with deionized water and 95% absolute ethanol with repeated ultrasonic oscillation at a temperature of 60-90°C, and dry it for later use;

Step 2: Weigh the treated nylon fabric and butyl titanate obtained in step 1 according to the mass ratio of 1-3:1, and dissolve the weighed butyl titanate in deionized water at a volume ratio of 1:20-100 , to obtain a butyl titanate solution, and then dip the weighed nylon fabric in the butyl titanate solution for 5 to 10 minutes, then add the butyl titanate solution impregnated with the nylon fabric into a high-temperature and high-pressure reactor, and use a deionized Fill the reactor with water to 60-80% of its volume, seal it, and treat the sealed reactor at a constant temperature of 110-140°C for 3-6 hours, and take out the nylon fabric after the reaction is completed;

Step 3: Wash the reacted nylon fabric obtained in the previous step with washing liquid at 70-90°C for 10-20 minutes at a bath ratio of 1:30-50, then repeatedly wash with hot and cold water, dry or Dry naturally to obtain the modified nylon fabric.

The present invention is also characterized in that,

Wherein the washing liquid in the step 3 is made up of the solid soap flakes of 2g/L, the soda ash of 2g/L dissolved in water.

The beneficial effect of the present invention is that, while preparing the nano-titanium dioxide powder by adopting the hydrothermal synthesis technology, the nano-titanium dioxide film is directly loaded on the surface of the nylon fabric fiber, endowing the nylon fabric with anti-ultraviolet and antibacterial properties, and by controlling the reaction temperature and time, the titanium dioxide The process parameters such as the amount of butyl ester and deionized water were used to optimize the finishing process. This method saves raw materials, is easy to operate, and has good washing resistance. The test results show that the nylon fabric modified by butyl titanate hydrothermally still has excellent anti-ultraviolet and antibacterial properties after 30 times of washing.

Description of drawings

Fig. 1 is the scanning electron microscope photo of nylon fabric butyl titanate before hydrothermal modification;

Fig. 2 is the scanning electron microscope photo after adopting the inventive method to nylon fabric butyl titanate hydrothermal modification;

Fig. 3 is the X-ray diffraction spectrogram after adopting the inventive method to nylon fabric butyl titanate hydrothermal modification;

Fig. 4 is the ultraviolet reflectance spectrum curve before and after hydrothermal modification of nylon fabric butyl titanate in Example 1 of the present invention;

Fig. 5 is the ultraviolet reflection spectrum curve before and after hydrothermal modification of nylon fabric butyl titanate in Example 2 of the present invention;

Fig. 6 is the ultraviolet reflectance spectrum curves before and after hydrothermal modification of nylon fabric butyl titanate in Example 3 of the present invention.

Detailed ways

The present invention will be described in detail below in conjunction with the accompanying drawings and specific embodiments.

The present invention adopts butyl titanate to carry out the method for modifying nylon fabric, specifically implements according to the following steps:

Step 1: Wash the nylon fabric to be modified with deionized water and 95% absolute ethanol with repeated ultrasonic oscillation at a temperature of 60-90°C, and then dry it for later use.

Step 2: Weigh the treated nylon fabric and butyl titanate obtained in step 1 according to the mass ratio of 1-3:1, and dissolve the weighed butyl titanate in deionized water at a volume ratio of 1:20-100 , to obtain a butyl titanate solution, and then dip the weighed nylon fabric in the butyl titanate solution for 5 to 10 minutes, then add the butyl titanate solution impregnated with the nylon fabric into a high-temperature and high-pressure reactor, and use a deionized Fill the reactor with water to 60-80% of its volume, seal it, and treat the sealed reactor at a constant temperature of 110-140°C for 3-6 hours, and take out the nylon fabric after the reaction is completed.

Step 3: Wash the reacted nylon fabric obtained in the previous step with washing liquid at 70-90°C for 10-20 minutes at a bath ratio of 1:30-50, then repeatedly wash with hot and cold water, dry or Dry naturally to obtain the modified nylon fabric. The washing solution is composed of 2g/L solid soap flakes and 2g/L soda ash dissolved in water.

Figure 1 and Figure 2 are scanning electron micrographs of nylon fabric before and after hydrothermal modification with butyl titanate. It can be seen that after the nylon fabric is hydrothermally modified by butyl titanate, the surface of the fiber is covered with a layer of nano-titanium dioxide film. Fig. 3 is the X-ray diffraction spectrum of butyl titanate hydrothermally modified nylon fabric. It can be seen that the nano titanium dioxide film is anatase type. The bandgap width of the anatase nano-titanium dioxide crystal structure is larger than that of the rutile crystal structure, so that the hole-electron pairs generated by the anatase crystal form have more positive and negative potentials, so for most photocatalytic As far as the reaction system is concerned, the anatase-type nano-titanium dioxide film has higher catalytic activity.

According to the national standard GB/T8629-2001 "Household Washing and Drying Procedures for Textile Tests", the hydrothermally modified nylon fabric of butyl titanate was washed and dried (type A washing machine, 4A washing procedure, and type A drying procedure were selected), and According to the national standard GB/T18830-2009 "Evaluation of UV protection performance of textiles", the UV protection performance of butyl titanate hydrothermally modified nylon fabric was determined. After 30 times of standard washing, the spectral transmittance T of the modified nylon fabric in the UVB and UVA bands is <3.5%, and the ultraviolet protection factor UPF>50, which can be used as an anti-ultraviolet product.

According to the national standard GB/T20944.1-2007 "Evaluation of antibacterial performance of textiles Part 1: Agar plate diffusion method", the antibacterial effect of nylon fabric after hydrothermal modification of butyl titanate was determined. The butyl titanate hydrothermally modified nylon fabric has an antibacterial effect on Staphylococcus aureus (ATCC6538) and Escherichia coli (8099) within 1mm, no reproduction, and good antibacterial effect.

The present invention adopts the hydrothermal method to prepare the nano-titanium dioxide powder while directly loading the nano-titanium dioxide film on the surface of the nylon fabric fiber. By optimizing the reaction temperature and time, the dosage ratio of the fabric, butyl titanate and deionized water, the optimum Good finishing process. The proportion of nylon fabric, butyl titanate and deionized water, the filling amount, the temperature and time of hydrothermal reaction all affect the crystal phase, degree of crystallization, morphology and particle size of the product. When the mass ratio of nylon fabric to butyl titanate is 1 to 3:1, the surface of the fiber can be coated with a film of a certain thickness, and the nanoparticles and nylon fiber are firmly combined without agglomeration and excessive deposition in the solution. Titanium dioxide particles; when it is less than 1:1, the amount of butyl titanate is too large, which is easy to cause waste, and the film coated on the surface of the fiber is too thick, which is not conducive to the formation of nanoparticles, affecting the fabric feel and wearing performance; when it is greater than 3:1 When the amount of butyl titanate is too small, no continuous film is formed on the surface of the fiber, and the anti-ultraviolet and antibacterial properties are affected. When the ratio of butyl titanate to deionized water is controlled at 1:20-100, the surface of the fiber is coated with a certain thickness of nano-titanium dioxide film, and the particles will not agglomerate, and at the same time, too many nanoparticles will not be deposited in the solution, and It is firmly combined with the fiber; when it is less than 1:20, the amount of butyl titanate is too large and it will easily cause waste, the titanium dioxide adhered to the surface of the fiber is too thick, the adhesion fastness is not good, and the nanoparticles are easy to fall off during use; when it is greater than 1: When 100, the titanium dioxide adhered to the surface of the fiber is too little, and no continuous film is formed, which affects the anti-ultraviolet and antibacterial properties. When the filling amount of the solution is 60-80%, it can generate anatase nano-titanium dioxide particles; when it is less than 60%, the pressure in the reactor is low, which will affect the formation of nano-titanium dioxide; when it is greater than 80%, it is also unfavorable for nano-titanium dioxide The generation of reactors will also affect the safety of the reactor. The reaction temperature and time mainly affect the degree of crystallization of the product and the morphology and size of the crystal, and also have some influence on the generated crystal phase. The hydrothermal reaction temperature is controlled between 110 and 140°C, and anatase nano-titanium dioxide particles can be generated; when it is lower than 110°C, the crystal structure of nano-titanium dioxide will be affected, and the purpose of UV protection and antibacterial cannot be achieved; when it is higher than When the temperature is 140°C, the hand of the treated fabric is obviously hard, the strength of the fabric is greatly damaged, and the usability is lost. The hydrothermal reaction time is controlled between 3 and 6 hours, and anatase nano-titanium dioxide film can be formed on the fiber surface; when it is lower than 3 hours, it will affect the crystallization degree of nano-titanium dioxide, and the anti-ultraviolet performance is not good; when it is higher than 6 hours At this time, the generated titanium dioxide particles will be agglomerated, the particle size will increase significantly, and the increase in surface roughness will easily cause shedding.

Example 1

Weigh 5g each of nylon fabric and butyl titanate, wherein the nylon fabric is washed with deionized water and 95% absolute ethanol solution with a volume ratio of 1:1 at a temperature of 80°C for 30min under the condition of 50KHz power 100W, 60°C Drying; butyl titanate was dissolved in deionized water at a ratio of 1:20; then the nylon fabric was immersed in the butyl titanate aqueous solution for 5 minutes, and the nylon fabric and the butyl titanate solution were added to 200ml high temperature and high pressure reaction The reactor was filled with deionized water to 80% of the volume of the reactor, and the sealed reactor was treated at a constant temperature of 110°C for 3 hours; after the reaction was completed, 2g/L soap flakes and 2g/L soda Wash at 90°C for 15 minutes at a bath ratio of 1:30, then repeatedly wash with 80°C hot water and cold water, and dry at 60°C. Fig. 4 is the ultraviolet reflection spectrum curve of the nylon fabric before and after the modification by the above-mentioned finishing process. It can be seen that after 30 times of washing of the modified nylon fabric, the average reflectance of ultraviolet rays in the UVB band (280-315nm) dropped from 19.9% to 7.6%, that is, the absorption capacity of ultraviolet rays increased by 12.3%, while the UVA band (315 ~ 400nm) average absorption capacity of ultraviolet rays increased by 16.2%.

According to the national standard GB/T8629-2001, the nylon fabric after hydrothermal modification of butyl titanate is washed and dried (select A-type washing machine, 4A washing procedure, A-type drying procedure), and according to the national standard GB/T18830-2009 Determination of the anti-ultraviolet properties of nylon fabrics after hydrothermal modification of butyl titanate. After 30 times of washing, the spectral transmittance of the modified nylon fabric in the UVB and UVA bands is T=3.4%, and the ultraviolet protection factor UPF=53. According to the national standard GB/T20944.1-2007, the antibacterial effect of nylon fabric after hydrothermal modification of butyl titanate was determined. The antibacterial zone of the modified nylon fabric against Staphylococcus aureus and Escherichia coli is within 1mm, without reproduction, and the antibacterial effect is good.

Example 2

Weigh 15g of nylon fabric and 5g of butyl titanate respectively, wherein the nylon fabric is washed with deionized water and 95% absolute ethanol solution with a volume ratio of 1:1 at a temperature of 80°C for 30 minutes under ultrasonic vibration at 50KHz and 100W. Dry at 60°C; dissolve butyl titanate with deionized water at a ratio of 1:100; then immerse the nylon fabric in the aqueous solution of butyl titanate for 10 minutes, and add the nylon fabric together with the butyl titanate solution to 200ml high temperature In a high-pressure reactor, fill it with deionized water to 60% of the volume of the reactor, and treat the sealed reactor at a constant temperature of 140°C for 6 hours; after the reaction is completed, use 2g/L soap flakes, 2g/L soda ash solution , washed at 90°C for 15 minutes with a bath ratio of 1:30, then repeatedly washed with 80°C hot water and cold water, and dried at 60°C. Fig. 5 is the ultraviolet reflection spectrum curve of the nylon fabric before and after the modification by the above-mentioned finishing process. It can be seen that after the modified nylon fabric has been washed 30 times, the average ultraviolet absorption capacity of the UVB band (280-315nm) has increased by 12.2%, while the average absorption capacity of the UVA band (315-400nm) has increased by 13.5%. .

According to the national standard GB/T8629-2001, the nylon fabric after hydrothermal modification of butyl titanate is washed and dried (select A-type washing machine, 4A washing procedure, A-type drying procedure), and according to the national standard GB/T18830-2009 Determination of the anti-ultraviolet properties of nylon fabrics after hydrothermal modification of butyl titanate. After 30 times of washing, the spectral transmittance of the modified nylon fabric in the UVB and UVA bands is T=3.5%, and the ultraviolet protection factor UPF=51. According to the national standard GB/T20944.1-2007, the antibacterial effect of nylon fabric after hydrothermal modification of butyl titanate was determined. The antibacterial zone of the modified nylon fabric against Staphylococcus aureus and Escherichia coli is within 1mm, without reproduction, and the antibacterial effect is good.

Example 3

Weigh 10g of nylon fabric and 5g of butyl titanate respectively, wherein the nylon fabric is washed with deionized water and 95% absolute ethanol solution at a temperature of 80°C with a volume ratio of 1:1 and ultrasonic vibration washing at 50KHz and 100W for 30min. Dry at 60°C; dissolve butyl titanate with deionized water at a ratio of 1:80; then immerse the nylon fabric in the butyl titanate aqueous solution for 8 minutes, and add the nylon fabric together with the butyl titanate solution to 200ml high temperature In a high-pressure reactor, fill it with deionized water to 70% of the volume of the reactor, and treat the sealed reactor at a constant temperature of 120°C for 5 hours; after the reaction is completed, use 2g/L soap flakes, 2g/L soda ash solution , washed at 90°C for 15 minutes with a bath ratio of 1:30, then repeatedly washed with 80°C hot water and cold water, and dried at 60°C. Fig. 6 is the ultraviolet reflection spectrum curve of the nylon fabric before and after the modification by the above-mentioned finishing process. It can be seen that after the modified nylon fabric has been washed 30 times, the average ultraviolet absorption capacity of the UVB band (280-315nm) has increased by 15.1%, and the average ultraviolet absorption capacity of the UVA band (315-400nm) has increased by 18.6%. .

According to the national standard GB/T8629-2001, the nylon fabric after hydrothermal modification of butyl titanate is washed and dried (select A-type washing machine, 4A washing procedure, A-type drying procedure), and according to the national standard GB/T18830-2009 Determination of the anti-ultraviolet properties of nylon fabrics after hydrothermal modification of butyl titanate. After 30 times of washing, the spectral transmittance of the modified nylon fabric in the UVB and UVA bands is T=3.2%, and the ultraviolet protection factor UPF=56. According to the national standard GB/T20944.1-2007, the antibacterial effect of nylon fabric after hydrothermal modification of butyl titanate was determined. The antibacterial zone of the modified nylon fabric against Staphylococcus aureus and Escherichia coli is within 1mm, without reproduction, and the antibacterial effect is good.

Claims (2)

1. a method that adopts butyl titanate to modify nylon fabric, is characterized in that, specifically implements according to the following steps: Step 1: Wash the nylon fabric to be modified with deionized water and 95% absolute ethanol with repeated ultrasonic oscillation at a temperature of 60-90°C, and dry it for later use; Step 2: Weigh the treated nylon fabric and butyl titanate obtained in step 1 according to the mass ratio of 1-3:1, and dissolve the weighed butyl titanate in deionized water at a volume ratio of 1:20-100 , to obtain a butyl titanate solution, and then dip the weighed nylon fabric in the butyl titanate solution for 5 to 10 minutes, then add the butyl titanate solution impregnated with the nylon fabric into a high-temperature and high-pressure reactor, and use a deionized Fill the reactor with water to 60-80% of its volume, seal it, and treat the sealed reactor at a constant temperature of 110-140°C for 3-6 hours, and take out the nylon fabric after the reaction is completed; Step 3: Wash the reacted nylon fabric obtained in the previous step with washing liquid at 70-90°C for 10-20 minutes at a bath ratio of 1:30-50, then repeatedly wash with hot and cold water, dry or Dry naturally to obtain the modified nylon fabric. 2. the method that adopts butyl titanate to modify nylon fabric according to claim 1, is characterized in that, the washing liquid in the described step 3 is made of solid soap flakes of 2g/L, soda ash of 2g/L Soluble in water composition.

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