阅读说明：本技术 一种阻燃抑烟功能性棉织物及其制备方法 (Flame-retardant and smoke-suppressing functional cotton fabric and preparation method thereof ) 是由 毛庆辉 罗欢 郁佳 张毓 郑琳娟 张莉 梁志结 于 2020-12-04 设计创作，主要内容包括：本发明属于纺织品技术领域,涉及一种阻燃抑烟功能性棉织物及其制备方法。包括：S1.将棉织物浸入NaOH溶液中,取出水洗至中性后烘干；S2.将环氧氯丙烷溶于助溶剂后加入NaOH溶液；S3.将经步骤S1的棉织物加入步骤S2的溶液中醚化处理；S4.将乙二胺溶于水中,并加入催化剂；S5.将醚化处理后的棉织物加入步骤S4得到的溶液中改性处理；S6.将钼酸盐溶于水中,加入五氧化二钒和硝酸,混合均匀；S7.将改性后的棉织物浸入步骤S6得到的溶液中,在70～100℃下反应1.5～6h,室温放置1～4天后取出,水洗,晾干,得阻燃抑烟功能性棉织物。该棉织物具有安全性高、抑烟、无毒、价廉等优点,且性能稳定,不易挥发。(The invention belongs to the technical field of textiles, and relates to a flame-retardant and smoke-suppressing functional cotton fabric and a preparation method thereof. The method comprises the following steps: s1, soaking a cotton fabric into a NaOH solution, taking out the cotton fabric, washing the cotton fabric to be neutral, and drying the cotton fabric; s2, dissolving epoxy chloropropane in a cosolvent, and adding a NaOH solution; s3, adding the cotton fabric obtained in the step S1 into the solution obtained in the step S2 for etherification treatment; s4, dissolving ethylenediamine in water, and adding a catalyst; s5, adding the etherified cotton fabric into the solution obtained in the step S4 for modification treatment; s6, dissolving molybdate in water, adding vanadium pentoxide and nitric acid, and uniformly mixing; and S7, soaking the modified cotton fabric into the solution obtained in the step S6, reacting for 1.5-6 h at 70-100 ℃, standing for 1-4 days at room temperature, taking out, washing with water, and airing to obtain the flame-retardant and smoke-suppression functional cotton fabric. The cotton fabric has the advantages of high safety, smoke suppression, no toxicity, low price and the like, and has stable performance and difficult volatilization.)

1. A preparation method of a flame-retardant smoke-suppressing functional cotton fabric is characterized by comprising the following steps:

s1, soaking a cotton fabric into a NaOH solution according to a bath ratio of 1 (30-100), stirring at room temperature for 1-3 h, washing with water to be neutral, and drying at 70-100 ℃;

s2, dissolving epoxy chloropropane in a cosolvent, adding a NaOH solution, and uniformly mixing to obtain a first mixed solution;

s3, adding the cotton fabric obtained by the treatment of the step S1 into the first mixed solution, etherifying for 3-8 hours at the temperature of 20-50 ℃, washing with water, and drying to obtain an etherified cotton fabric;

s4, dissolving ethylenediamine in water, adding a catalyst, and uniformly mixing to obtain a second mixed solution;

s5, adding the etherified cotton fabric into the second mixed solution, reacting for 1-5 hours at 20-50 ℃, washing with water, and drying to obtain a modified cotton fabric;

s6, dissolving molybdate in water, adding vanadium pentoxide and nitric acid, uniformly mixing, and diluting to obtain a third mixed solution;

and S7, putting the modified cotton fabric into the third mixed solution, reacting for 1.5-6 h at 70-100 ℃, standing for 1-4 days at room temperature, taking out, washing with water, and airing at room temperature to obtain the flame-retardant and smoke-suppressing functional cotton fabric.

2. The method as claimed in claim 1, wherein in step S1, the concentration of NaOH solution is 5-20 wt%.

3. The preparation method according to claim 1, wherein in step S2, the concentration of the NaOH solution is 5 to 10 wt%, and the volume ratio of the epichlorohydrin to the NaOH solution is (10 to 50): (100-500), wherein the volume ratio of the epoxy chloropropane to the cosolvent is 1: 1.

4. The method according to claim 1, wherein in step S2, the cosolvent is ethanol, acetone or a mixture of both.

5. The method according to claim 1, wherein in step S4, the catalyst is Na₂CO₃Or NaHCO₃The dosage ratio of the ethylenediamine to the water to the catalyst is (10-50) mL, (100-500) mL and (1-5) g.

6. The preparation method according to claim 1, wherein in the step S6, the molybdate is sodium molybdate or ammonium molybdate, the mass ratio of the molybdate to the vanadium pentoxide is (1-5) - (1-3), and the concentration of the molybdate in the third mixed solution is 0.5-50 g/L.

7. The flame-retardant smoke-suppression functional cotton fabric prepared by the preparation method of any one of claims 1 to 6.

Technical Field

The invention belongs to the technical field of textiles, and particularly relates to a flame-retardant and smoke-suppressing functional cotton fabric and a preparation method thereof.

Background

With the increase of urban areas, high-rise and super high-rise buildings are gradually increased, people working and living in the buildings are more and more, the demand of indoor textiles is greatly increased, and the fire problem of the high-rise buildings caused by the increase of the demand is more and more noticed by the world. Therefore, the research on the flame-retardant fabric becomes necessary, and the flame-retardant fabric can well play the roles of preventing fire, delaying fire and striving for rescue time by utilizing the textile with flame retardance. Cotton is a main material in the textile industry, and occupies a very critical position in textile products, and cotton textiles are widely applied by virtue of excellent hygroscopicity, air permeability, softness and heat preservation characteristics, but cotton fabrics generally need to achieve a certain flame retardant effect through flame retardant finishing due to poor flame retardant performance. The traditional flame retardant finishing generally adopts organic flame retardants, the organic flame retardants are gradually limited along with the continuous improvement of the environmental protection requirements, and the inorganic flame retardants are more and more concerned by the market. Therefore, the development of the flame-retardant smoke-inhibiting functional cotton fabric which is high in safety, smoke-inhibiting and non-toxic has important significance.

Disclosure of Invention

In view of the above, the invention aims to provide a flame-retardant and smoke-suppressing functional cotton fabric and a preparation method thereof.

In order to solve the technical problems, the invention provides a preparation method of a flame-retardant and smoke-suppressing functional cotton fabric, which comprises the following steps:

s1, soaking a cotton fabric into a NaOH solution according to a bath ratio of 1 (30-100), stirring at room temperature for 1-3 h, washing with water to be neutral, and drying at 70-100 ℃;

s2, dissolving epoxy chloropropane in a cosolvent, adding a NaOH solution, and uniformly mixing to obtain a first mixed solution;

s3, adding the cotton fabric obtained by the treatment of the step S1 into the first mixed solution, etherifying for 3-8 hours at the temperature of 20-50 ℃, washing with water, and drying to obtain an etherified cotton fabric;

s4, dissolving ethylenediamine in water, adding a catalyst, and uniformly mixing to obtain a second mixed solution;

s5, adding the etherified cotton fabric into the second mixed solution, reacting for 1-5 hours at 20-50 ℃, washing with water, and drying to obtain a modified cotton fabric;

s6, dissolving molybdate in water, adding vanadium pentoxide and nitric acid, uniformly mixing, and diluting to obtain a third mixed solution;

and S7, putting the modified cotton fabric into the third mixed solution, reacting for 1.5-6 h at 70-100 ℃, standing for 1-4 days at room temperature, taking out, washing with water, and airing at room temperature to obtain the flame-retardant and smoke-suppressing functional cotton fabric.

Further, in the step S1, the concentration of the NaOH solution is 5-20 wt%,

further, in the step S2, the concentration of the NaOH solution is 5 to 10 wt%, and the volume ratio of the epichlorohydrin to the NaOH solution is (10 to 50): (100-500), wherein the volume ratio of the epoxy chloropropane to the cosolvent is 1: 1.

Further, in step S2, the cosolvent is ethanol, acetone or a mixture of both.

Further, in the step S4, the catalyst is Na₂CO₃Or NaHCO₃The dosage ratio of the ethylenediamine to the water to the catalyst is (10-50) mL, (100-500) mL and (1-5) g.

Further, in the step S6, the molybdate is sodium molybdate or ammonium molybdate, the mass ratio of the molybdate to the vanadium pentoxide is (1-5) - (3-5), and the concentration of the molybdate in the third mixed solution is 0.5-50 g/L.

The invention also provides the flame-retardant smoke-suppressing functional cotton fabric prepared by the preparation method.

Compared with the prior art, the invention controls the content of hydroxyl in the modified cotton fiber macromolecules by controlling the modification conditions, thereby controlling the number of active binding points, finally realizing the controllable growth of the POM flaky crystal with flame-retardant and smoke-eliminating functions and obtaining the flame-retardant and smoke-suppressing functional cotton fabric. The POM with flame retardance and smoke abatement is bonded with cotton fabric, the modified cotton fiber macromolecules contain a large number of organic electron donors of active groups such as hydroxyl (-OH) and the like, charge transfer donating and accepting compounds can be formed by the modified cotton fiber macromolecules and the POM, the POM can be decomposed at high temperature to release substances capable of absorbing certain amount of heat to play a role in cooling and diluting, and polyacid covers the surface of the cotton fiber to form a carbon layer to block external oxygen and volatile combustible substances, so that the purposes of flame retardance and smoke abatement are achieved.

Drawings

FIG. 1 is an electron microscope image of a flame-retardant smoke-suppressing functional cotton fabric provided by embodiment 1 of the invention.

Detailed Description

The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Furthermore, it should be understood that various changes or modifications can be made by those skilled in the art after reading the teaching of the present invention, and equivalents also fall within the scope of the claims of the present application.

Example 1

Step 1, soaking 10g of cotton fabric into NaOH solution with the mass fraction of 20%, stirring for 3h at room temperature according to the bath ratio of 1: 100, washing to be neutral, and drying at 80 ℃.

And 2, dissolving 50mL of epoxy chloropropane in 50mL of ethanol, adding 500mL of NaOH solution with the mass fraction of 10%, and uniformly mixing to obtain a first mixed solution.

And 3, adding the cotton fabric processed in the step 1 into the first mixed solution in the step 2, etherifying for 5 hours at 50 ℃, washing with water, and drying at 70 ℃ to obtain the etherified cotton fabric.

Step 4, 50mL of ethylenediamine was dissolved in 500mL of water and 5g of Na was added₂CO₃And uniformly mixing to obtain a second mixed solution.

And 5, adding the etherified cotton fabric obtained in the step 3 into the solution obtained in the step 4, reacting for 5 hours at 50 ℃, washing with water, and drying at 70 ℃ to obtain the modified cotton fabric.

And step 6, dissolving 5g of sodium molybdate in 50mL of water, adding 3g of vanadium pentoxide and 10mL of nitric acid, and diluting to 300mL to obtain a third mixed solution.

And 7, putting the modified cotton fabric obtained in the step 5 into the third mixed solution obtained in the step 6, reacting for 2 hours at 100 ℃, standing for 4 days at room temperature, taking out, washing with water, and airing at room temperature to obtain the flame-retardant and smoke-suppressing functional cotton fabric. The electron microscope image of the cotton fabric is shown in figure 1.

Example 2

Step 1, soaking 5g of cotton fabric into NaOH solution with the mass fraction of 20%, stirring for 1h at room temperature according to the bath ratio of 1: 30, washing to be neutral, and drying at 70 ℃.

And 2, dissolving 10mL of epoxy chloropropane in 10mL of acetone, adding 500mL of NaOH solution with the mass fraction of 5%, and uniformly mixing to obtain a first mixed solution.

And 3, adding the cotton fabric processed in the step 1 into the first mixed solution in the step 2, etherifying for 8 hours at the temperature of 20 ℃, washing with water, and drying at the temperature of 70 ℃ to obtain the etherified cotton fabric.

Step 4, 10mL of ethylenediamine was dissolved in 500mL of water, and 1g of Na was added₂CO₃And uniformly mixing to obtain a second mixed solution.

And 5, adding the etherified cotton fabric obtained in the step 3 into the solution obtained in the step 4, reacting for 1 hour at 20 ℃, washing with water, and drying at 70 ℃ to obtain the modified cotton fabric.

And step 6, dissolving 0.5g of sodium molybdate in 50mL of water, adding 1g of vanadium pentoxide and 2mL of nitric acid, and diluting to 1000mL to obtain a third mixed solution.

And 7, putting the modified cotton fabric obtained in the step 5 into the third mixed solution obtained in the step 6, reacting for 6 hours at 100 ℃, standing for 1 day at room temperature, taking out, washing with water, and airing at room temperature.

Example 3

Step 1, soaking 10g of cotton fabric into NaOH solution with the mass fraction of 5%, the bath ratio is 1: 50, stirring for 2h at room temperature, washing with water to neutrality, and drying at 100 ℃.

And 2, dissolving 50mL of epoxy chloropropane in 50mL of ethanol, adding 100mL of NaOH solution with the mass fraction of 10%, and uniformly mixing to obtain a first mixed solution.

And 3, adding the cotton fabric processed in the step 1 into the first mixed solution in the step 2, etherifying for 3 hours at 50 ℃, washing with water, and drying at 70 ℃ to obtain the etherified cotton fabric.

Step 4, 50mL of ethylenediamine was dissolved in 100mL of water and 5g of Na was added₂CO₃And uniformly mixing to obtain a second mixed solution.

And 5, adding the etherified cotton fabric obtained in the step 3 into the solution obtained in the step 4, reacting for 5 hours at 50 ℃, washing with water, and drying at 70 ℃ to obtain the modified cotton fabric.

And step 6, dissolving 5g of ammonium molybdate in 50mL of water, adding 3g of vanadium pentoxide and 1mL of nitric acid, and diluting to 100mL to obtain a third mixed solution.

And 7, putting the modified cotton fabric obtained in the step 5 into the third mixed solution obtained in the step 6, reacting for 1.5h at 70 ℃, standing for 2 days at room temperature, taking out, washing with water, and airing at room temperature.

Comparative example 1

Step 1, soaking 10g of cotton fabric into NaOH solution with the mass fraction of 20%, stirring for 3h at room temperature according to the bath ratio of 1: 100, washing to be neutral, and drying at 80 ℃.

And 2, dissolving 50mL of epoxy chloropropane in 50mL of ethanol, adding 500mL of NaOH solution with the mass fraction of 10%, and uniformly mixing to obtain a first mixed solution.

And 3, adding the cotton fabric processed in the step 1 into the first mixed solution in the step 2, etherifying for 5 hours at 50 ℃, washing with water, and drying at 70 ℃ to obtain the etherified cotton fabric.

Step 4, 50mL of ethanediThe amine was dissolved in 500mL of water and 5g of Na was added₂CO₃And uniformly mixing to obtain a second mixed solution.

And 5, adding the etherified cotton fabric obtained in the step 3 into the solution obtained in the step 4, reacting for 5 hours at 50 ℃, washing with water, and drying at 70 ℃ to obtain the modified cotton fabric.

And step 6, dissolving 5g of sodium tungstate in 50mL of water, adding 3g of vanadium pentoxide and 10mL of nitric acid, and diluting to 300mL to obtain a third mixed solution.

And 7, putting the modified cotton fabric obtained in the step 5 into the third mixed solution obtained in the step 6, reacting for 2 hours at 100 ℃, standing for 4 days at room temperature, taking out, washing with water, and airing at room temperature to obtain the polyoxometallate cotton fabric.

The raw cotton fabric, the flame-retardant and smoke-suppressing functional cotton fabric prepared in examples 1 to 3 and the cotton fabric prepared in comparative example 1 were subjected to a vertical combustion method flame-retardant performance test, respectively, and the results are shown in table 1.

TABLE 1 Cotton Fabric vertical Combustion test data

From table 1, it can be seen that the polymetallic molybdate cotton fabric prepared from sodium molybdate and ammonium molybdate has better flame retardant and smoke suppression effects, while the polymetallic tungstate cotton fabric prepared from sodium tungstate has poorer flame retardant and smoke suppression effects.

It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.