Flame-retardant and antibacterial curtain fabric and preparation method thereof

Abstract

The invention relates to the technical field of curtain fabrics, in particular to a flame-retardant and antibacterial curtain fabric and a preparation method thereof. The method comprises the following steps: reacting methoxy polypropylene glycol trifluoromethanesulfonate, methyltriacetoxysilane and a cotton fabric in the same system to obtain a modified cotton fabric, and preparing the curtain fabric from the modified cotton fabric. The curtain fabric is prepared from the modified cotton fabric, and the curtain fabric still has an excellent flame-retardant effect under the condition that flame retardants such as boric acid are not added.

Description

Technical Field

[0001] The invention relates to the technical field of curtain fabrics, and in particular to flame-retardant and antibacterial curtain fabrics and a preparation method thereof. Background Art

[0002] In addition to being highly sun-resistant, curtains also need to have certain flame retardancy. As an indispensable decoration in buildings, curtains have become one of the main sources of fire in urban buildings. Most of the existing ordinary curtains are flammable and combustible, often serving as a starting point for fires, and are extremely easy to spread. Burning also produces toxic gases. However, due to the difficulty in preventing fire accidents, the development of high-quality flame-retardant curtains is still very necessary.

[0003] There are two main ways to prepare flame-retardant curtain fabrics. One is to prepare flame-retardant products from flame-retardant raw materials, and the other is to make the fabric flame-retardant by flame-retardant finishing. The two methods have different focuses. Method 1 focuses on preparing fiber raw materials with flame-retardant properties, and method 2 focuses on developing an excellent flame retardant with good flame retardant properties. Summary of the invention

[0004] The purpose of the present invention is to provide a flame retardant and antibacterial curtain fabric and a preparation method thereof, and to provide an environmentally friendly flame retardant curtain that can have a good flame retardant effect and also has good antibacterial properties. The technical solution is as follows: One of the purposes of the present invention is to provide a method for preparing a flame retardant and antibacterial modified cotton fabric, comprising: (1) In an ice-salt bath at 2-8°C, methoxypolypropylene glycol and diethylamine are dissolved in dichloromethane, trifluoromethanesulfonyl chloride is added, and the mixture is reacted at room temperature to purify methoxypolypropylene glycol trifluoromethanesulfonate; (2) obtaining a treated plain cotton fabric; (3) The plain cotton fabric obtained in step (2), methyltriacetoxysilane and sodium trifluoroethoxide are placed in an ethanol solution for reflux reaction, cooled to room temperature, and a tetrahydrofuran solution containing the methoxypolypropylene glycol trifluoromethanesulfonate is added to react at room temperature. The cotton fabric after the reaction is taken out, washed with ethanol and tetrahydrofuran, and dried to obtain the modified cotton fabric.

[0005] In the above preparation method, the molecular weight of methoxypolypropylene glycol is 3000, and the input molar ratio of methoxypolypropylene glycol, diethylamine and trifluoromethanesulfonyl chloride is 1:2:2.

[0006] In the above preparation method, the plain cotton fabric is washed with ethanol and water and then dried.

[0007] In the above preparation method, the thickness of the treated plain cotton fabric is 0.1 mm.

[0008] In the above preparation method, methyltriacetoxysilane accounts for 10% of the weight of the plain cotton fabric, sodium trifluoroethoxide accounts for 15% of the weight of the plain cotton fabric, and methoxypolypropylene glycol trifluoromethanesulfonate accounts for 10% of the weight of the plain cotton fabric.

[0009] The second object of the present invention is to provide a modified cotton fabric obtained by the above preparation method.

[0010] The third object of the present invention is to provide a method for preparing curtain fabrics, comprising: preparing modified cotton fabrics by the above-mentioned preparation method; uniformly applying cold rolling stacking liquid to the grey cloth of the modified cotton fabric, then winding the grey cloth on a roller, stacking at low temperature, and washing with water until the pH value is neutral.

[0011] In the above preparation method, the cold rolling stacking liquid is 10g / L hydrogen peroxide.

[0012] In the above preparation method, the stacking time is 12-24 hours.

[0013] One of the fourth purposes of the present invention is to provide curtain cotton fabric obtained by the above preparation method.

[0014] Compared with the prior art, the present invention has at least the following technical effects: 1. The present invention allows methoxypolypropylene glycol trifluoromethanesulfonate, methyltriacetoxysilane and cotton fabric to react in the same system, so that the modified product is deeply bonded to the surface and inside of the cotton fabric. This method has a significant improvement over the method of first reacting methoxypolypropylene glycol trifluoromethanesulfonate with methyltriacetoxysilane to obtain a modified product, and then loading the modified product onto the cotton fabric through a physical step. For example, the flame retardant and antibacterial effects of the modified cotton fabric obtained by this method are improved.

[0015] 2. The present invention makes the modified cotton fabric into curtain fabric, which still has excellent flame retardant effect without adding flame retardants such as boric acid.

[0016] 3. The modified product and curtain fabric provided by the present invention not only have excellent flame retardant and antibacterial effects, but also have extremely high thermal stability.

[0017] 4. The modified material and curtain fabric provided by the present invention can absorb ammonia and have a deodorizing function.

[0018] 5. The modified material and curtain fabric provided by the present invention have a higher ultraviolet reflectivity and a lower ultraviolet transmittance in the range of 280-400nm, have the ability to protect against ultraviolet radiation, and provide a layer of protection for ultraviolet protection of household curtains. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 The ammonia adsorption amount of the plain cotton fabric, the modified cotton fabric provided in Example 1, the modified cotton fabric provided in Comparative Example 1, the curtain cotton fabric provided in Example 2, and the curtain cotton fabric provided in Comparative Example 2.

[0020] Figure 2 The ultraviolet transmittance curves of the modified cotton fabric (red) provided in Example 1, the modified cotton fabric (green) provided in Comparative Example 1, the curtain cotton fabric (blue) provided in Example 2, and the curtain cotton fabric (purple) provided in Comparative Example 2 are shown.

[0021] Figure 3 The ultraviolet reflectance curves are the modified cotton fabric (red) provided in Example 1, the modified cotton fabric (green) provided in Comparative Example 1, the curtain cotton fabric (blue) provided in Example 2, and the curtain cotton fabric (purple) provided in Comparative Example 2. DETAILED DESCRIPTION

[0022] In order to make the purpose, technical scheme and advantages of the present invention more clearly understood, the present invention is further described in detail below in conjunction with the examples. It should be understood that the specific embodiments described herein are only used to explain the present invention and are not intended to limit the present invention. The reagents not described separately in detail in the present invention are all conventional reagents and can be obtained from commercial channels; the methods not described in detail are all conventional experimental methods and can be obtained from the prior art.

[0023] Example 1: Preparation of modified cotton fabric In Example 1 of the present invention, the modified cotton fabric is prepared by the following steps. The specific steps are as follows: (1) In a 4°C ice-salt bath, methoxypolypropylene glycol (Cas: 37286-64-9, molecular weight of about 3000) and diethylamine were dissolved in dichloromethane, trifluoromethanesulfonyl chloride (Cas: 1939-99-7) was added, and the mixture was reacted at room temperature for 30 hours. The molar ratio of methoxypolypropylene glycol, diethylamine, and trifluoromethanesulfonyl chloride (Cas: 421-83-0) was 1:2:2. The insoluble matter in the obtained reactant was removed, and the obtained mixture was concentrated and separated by silica gel column chromatography using petroleum ether: ethyl acetate = 1:1 as the eluent to obtain methoxypolypropylene glycol trifluoromethanesulfonate.

[0024] (2) The plain cotton fabric was thoroughly washed with ethanol and water and then dried to obtain a plain cotton fabric with a thickness of 0.1 mm.

[0025] (3) The cotton fabric obtained in step (2), 10% of the weight of the fabric obtained in step (2) in methyltriacetoxysilane (Cas: 4253-34-3), and 15% of the weight of the fabric obtained in step (2) in sodium trifluoroethoxide in a mass volume ratio of 1 g:100 mL are placed in an ethanol solution for reflux reaction for 3 hours, cooled to room temperature, and 10% of the weight of the fabric obtained in step (2) in methoxypolypropylene glycol trifluoromethanesulfonate obtained in step 1) is dissolved in tetrahydrofuran, added to the reaction system, and reacted at room temperature for 48 hours; the cotton fabric after the reaction is taken out, washed with ethanol 3 times and then with tetrahydrofuran 3 times, the unreacted raw materials are removed from the surface of the cotton fabric after the reaction, and dried at 40°C for 48 hours.

[0026] Comparative Example 1: Preparation of modified cotton fabric Comparative Example 1 of the present invention is to prepare the modified cotton fabric by the following steps. The specific steps are as follows: 10g of methyltriacetoxysilane (Cas: 4253-34-3) and 15g of sodium trifluoroethoxide were placed in an ethanol solution at a mass volume ratio of 1g:100mL and refluxed for 3h. The mixture was cooled to room temperature, and the methoxypolypropylene glycol trifluoromethanesulfonate prepared in step (1) above was dissolved in tetrahydrofuran and added to the reaction system. The mixture was reacted at room temperature for 48h. The filtrate was concentrated by rotary evaporation, and separated by silica gel column chromatography using petroleum ether:ethyl acetate = 1:1 as the eluent to obtain the modified product. The plain cotton fabric was thoroughly washed with ethanol and water and then dried in an oven to obtain a plain cotton fabric with a thickness of about 0.1 mm. 10g of the modified product was collected into a solution of petroleum ether:ethyl acetate = 1:1 containing 100g of plain cotton fabric at a mass volume ratio of 1g:100mL. After 10 min, the modified product was taken out and dried at 80°C for 10 min and 160°C for 3 min. Finally, the modified product was thoroughly washed and dried to remove the unreacted modified product.

[0027] Test Example 1: Loading rate test on cotton fabric The weight of the modified cotton fabrics prepared in Example 1 and Comparative Example 1 was accurately weighed respectively, and the weight difference between the modified cotton fabrics and the plain cotton fabrics before modification was calculated, and the weight difference was calculated as the weight percentage of the plain cotton fabrics before modification, which was the loading rate of the modified substance on the plain cotton fabrics. The loading rates of the modified substance in Example 1 and Comparative Example 1 were 15.9% and 9.8% respectively, which indicated that the loading rate of the modified substance prepared in Example 1 was higher.

[0028] Example 2: Preparation of curtain fabric In Example 2 of the present invention, a curtain fabric is obtained by using the modified cotton fabric described above through the following steps. The details are as follows: The cold rolling stacking liquid (10g / L hydrogen peroxide) is evenly applied to the grey fabric of the modified cotton fabric, and then the grey fabric is wound on a roller and stacked at low temperature for 18 hours to allow the fabric to undergo a chemical reaction during the stacking process to remove impurities, improve whiteness and glossiness, etc. After stacking, the grey fabric is placed in a washing machine for thorough washing to remove residual chemicals and impurities on the fabric until the pH value of the washing liquid is neutral.

[0029] Comparative Example 2: Preparation of curtain fabric Comparative Example 2 of the present invention prepared a curtain fabric. The details are as follows: The pure cotton plain fabric is finished with 400g / L flame retardant (boric acid content 40g / L) finishing liquid, adjusted to pH 2~9, impregnated and rolled (two impregnations and two rollings, 60℃, 20min, rolling rate of about 80%), pre-dried (80℃, 3min), and baked (140~200℃, 2min) to obtain the curtain fabric of the control group.

[0030] Test Example 2: Flame retardant performance test The flame retardant properties of modified cotton fabrics and curtain fabrics were tested with reference to GB / T 5455-1997 “Vertical method for testing the burning performance of textiles”.

[0031] Table 1

[0032] As can be seen from Table 1, when the plain cotton fabric is subjected to a vertical combustion test, it burns until it is completely burned out, indicating that it does not have flame retardant properties. The afterburning time, smoldering time, and damaged length of Example 1 are all smaller than those of Comparative Example 1. It does not immediately generate flames when approaching the fire source, and the afterburning time and smoldering time are short after leaving, and combustion does not form immediately. The afterburning time, smoldering time, and damaged length of Example 2 are all smaller than those of Comparative Example 2, indicating that the modified cotton fabric provided by the present invention is made into a curtain fabric, which has a better flame retardant effect than the conventional flame retardant of Comparative Example 2, especially has a smaller damaged length, provides protection for the integrity of the curtain, and effectively prevents the spread of smoke and fire during a fire.

[0033] Test Example 3: Thermal Stability Test The thermal stability of the modified cotton fabric prepared in Example 1, the curtain fabric prepared in Example 2, the modified cotton fabric prepared in Comparative Example 1, and the curtain fabric prepared in Comparative Example 2 were tested by a thermogravimetric / differential thermal comprehensive analyzer in air atmosphere. Plain cotton fabric was used as a control. The heating rate was 15°C / min.

[0034] Table 2 shows the decomposition temperature (T5% (°C)) at 5% weight loss, the decomposition temperature (T10% (°C)) at 10% weight loss, the maximum decomposition temperature (Tmax (°C)), the average decomposition rate (Rmax (% / min)) and the final carbon residue rate (%) of the plain cotton fabric, the modified cotton fabric prepared in Example 1, the curtain fabric prepared in Example 2, the modified cotton fabric prepared in Comparative Example 1 and the curtain fabric prepared in Comparative Example 2 in air atmosphere.

[0035] As shown in Table 2, the weight loss of plain cotton fabric is 5% at 288°C, 10% at 323°C, the maximum decomposition temperature is 361°C, the average decomposition rate is 24.9% / min, and the residual carbon rate is 1.6%. After modification, the decomposition temperature of 5% weight loss, the decomposition temperature of 10% weight loss, the maximum decomposition temperature and the final residual carbon rate of the modified cotton fabric obtained in Example 1 and Comparative Example 1 are significantly increased, while the average decomposition rate is significantly decreased. It can be seen that Example 1 and Comparative Example 1 improve the thermal stability of the plain cotton fabric by modifying it. In addition, the thermal stability of Example 1 is higher than that of Comparative Example 1. Similarly, the decomposition temperature of 5% weight loss, the decomposition temperature of 10% weight loss, the maximum decomposition temperature and the final residual carbon rate of the curtain fabric obtained in Example 2 and Comparative Example 2 are significantly increased, while the average decomposition rate is significantly decreased. It can be seen that the curtain fabric obtained in Example 2 and Comparative Example 2 is modified to improve its thermal stability. In addition, the thermal stability of Example 2 is higher than that of Comparative Example 2.

[0036] Table 2

[0037] Test Example 4: Antibacterial Performance Test According to AATCC TM 100-2019 "Evaluation of Antimicrobial Finishes for Textile Materials", Staphylococcus aureus and Escherichia coli were used as target bacteria, with initial inoculation concentrations of 10 7 (7 log) CFU / mL and 10 7 (7 log) CFU / mL of live bacterial solution, the fabric was in contact with the bacteria for 30 min, and the antibacterial test was performed. The number of live bacteria in the bacterial solution after inoculation was tested, and the logarithm was taken. The percentage of the logarithm difference before and after treatment to the initial logarithm of live bacteria was used as the sterilization rate. As shown in Table 3.

[0038] Table 3

[0039] It can be seen from Table 3 that the plain cotton fabric was treated with 10 7 After the live bacterial solution of Staphylococcus aureus with a concentration of (7 log) CFU / mL was added, the logarithmic reduction value was 0.05 and the bactericidal rate was 0.71%.7 After the active bacterial solution of Escherichia coli (7 log) CFU / mL was added, the logarithmic reduction value was 0.12 and the bactericidal rate was 1.71%, indicating that the plain cotton fabric had almost no bactericidal activity. 7 (7 log) CFU / mL of Staphylococcus aureus live bacterial solution and 10 7 After the active bacterial solution of Escherichia coli (7 log) CFU / mL was added, the logarithmic reduction value and the sterilization rate were significantly increased. It can be seen that Example 1 and Comparative Example 1 obtained antibacterial activity by modifying the plain cotton fabric. In addition, the antibacterial activity of Example 1 was higher than that of Comparative Example 1. Similarly, the curtain fabrics obtained in Example 2 and Comparative Example 2 were treated with 10 7 (7 log) CFU / mL of Staphylococcus aureus live bacterial solution and 10 7 After the live bacterial liquid of Escherichia coli with (7 log) CFU / mL was added, the logarithmic reduction value and the sterilization rate were significantly increased. It can be seen that the curtain fabrics prepared in Example 2 and Comparative Example 2 were modified and obtained to obtain antibacterial activity. In addition, the antibacterial activity of Example 2 is higher than that of Comparative Example 2.

[0040] Test Example 5: Ammonia absorption performance Refer to GBT 14668-1993 "Determination of Ammonia in Air Quality - Nessler's Reagent Colorimetric Method" for testing. The results are as follows Figure 1 As shown, the ammonia adsorption amount of the modified cotton fabrics obtained in Example 1 and Comparative Example 1 is significantly higher than that of the plain cotton fabric, and the ammonia adsorption amount of Example 1 is higher than that of Comparative Example 1. The ammonia adsorption amount of the modified cotton fabrics obtained in Example 2 and Comparative Example 2 is significantly higher than that of the plain cotton fabric, and the ammonia adsorption amount of Example 2 is higher than that of Comparative Example 2. This shows that the modified cotton fabric and curtain fabric prepared by the present invention can absorb ammonia and have a deodorizing function.

[0041] Test Example 6: In this paper, the most widely used and relatively accurate spectrophotometer method is used in the study of the optical properties of window screen fabrics to obtain the characteristic spectrum of the optical properties (transmittance and reflectance) of the samples. Lambda 900 UV / visible spectrophotometer is used to cut 5cm×6cm samples from each sample fabric without cutting the edge of the fabric. The instrument is tested after 30 minutes of preheating. The test band is selected as 280~400nm. Before the test, the sample is placed in an environment with a temperature of (20±1)℃ and a relative humidity of (65±2)% for 24 hours. The selected sample is cut and then the transmittance curve and reflectance curve are obtained.

[0042] like Figure 2As shown, in the range of 280-400nm, Example 1 (red line) has only a small amount of transmittance between 310-338nm, and no transmission in other ultraviolet wavelength ranges, indicating that it has a lower transmittance to ultraviolet rays and has the highest protection against ultraviolet radiation. However, Comparative Example 1 (green line) has a small amount of transmitted ultraviolet rays between 310-380nm, and its protection against ultraviolet radiation is not as good as that of Example 1. Example 2 (blue line) is made from the modified cotton fabric provided by Example 1, and its ultraviolet transmittance between 310-338nm is further reduced, indicating that its protection against ultraviolet radiation is further enhanced. Comparative Example 2 (purple line) has a higher ultraviolet transmittance between 310-400nm, and its protection against ultraviolet radiation is weak.

[0043] like Figure 3 As shown, in the range of 280-400nm, Example 1 (red line) has a higher reflectivity between 280-400nm, indicating that its protection against ultraviolet radiation is mainly achieved through reflection. However, the amount of ultraviolet rays reflected by Comparative Example 1 (green line) is significantly reduced between 310-380nm, indicating that its reflectivity against ultraviolet radiation is not as good as that of Example 1. Example 2 (blue line) is made from the modified cotton fabric provided by Example 1, which not only has a higher reflectivity between 280-400nm, but also further increases its ultraviolet reflectivity between 310-338nm, indicating that its reflectivity against ultraviolet radiation is further enhanced. Comparative Example 2 (purple line) has a lower ultraviolet reflectivity between 310-400nm, and its ultraviolet reflectivity is weak.

[0044] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any changes or substitutions that can be easily conceived by any technician familiar with the technical field within the technical scope disclosed by the present invention should be covered within the protection scope of the present invention.

Claims

1. A method for preparing flame retardant and antibacterial modified cotton fabric, characterized in that: include: (1) In an ice-salt bath at 2-8°C, methoxypolypropylene glycol and diethylamine are dissolved in dichloromethane, trifluoromethanesulfonyl chloride is added, and the mixture is reacted at room temperature to purify methoxypolypropylene glycol trifluoromethanesulfonate; (2) obtaining a treated plain cotton fabric; (3) The obtained plain cotton fabric, methyltriacetoxysilane and sodium trifluoroethoxide are placed in an ethanol solution for reflux reaction, cooled to room temperature, and a tetrahydrofuran solution containing the methoxypolypropylene glycol trifluoromethanesulfonate is added to react at room temperature. The cotton fabric after the reaction is taken out, washed with ethanol and tetrahydrofuran, and dried to obtain the modified cotton fabric.

2. The preparation method according to claim 1, characterized in that: The molecular weight of methoxypolypropylene glycol is 3000, and the input molar ratio of methoxypolypropylene glycol, diethylamine and trifluoromethanesulfonyl chloride is 1:2:

2.

3. The preparation method according to claim 1, characterized in that: The plain cotton fabric was washed with ethanol and water and then dried.

4. The preparation method according to claim 1, characterized in that: The thickness of the treated plain cotton fabric was 0.1 mm.

5. The preparation method according to claim 1, characterized in that: The weight of the plain cotton fabric contains 10% methyltriacetoxysilane, the weight of the plain cotton fabric contains 15% sodium trifluoroethoxide, and the weight of the plain cotton fabric contains 10% methoxypolypropylene glycol trifluoromethanesulfonate.

6. The modified cotton fabric obtained by the preparation method according to any one of claims 1 to 5.

7. A method for preparing curtain fabric, characterized in that: include: The modified cotton fabric is prepared by the preparation method according to any one of claims 1 to 5; The cold rolling stacking liquid is evenly applied to the grey cloth of the modified cotton fabric, and then the grey cloth is wound on a roller, stacked at a low temperature, and then washed with water until the pH value is neutral.

8. The preparation method according to claim 7, characterized in that: The cold rolling stacking liquid is 10g / L hydrogen peroxide.

9. The preparation method according to claim 7, characterized in that: The stacking time is 12-24h.

10. Curtain fabric obtained by the preparation method according to any one of claims 7 to 9.

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