阅读说明：本技术 一种阻燃涤纶面料及其制备方法 (Flame-retardant polyester fabric and preparation method thereof ) 是由 周凡雨 彭雄义 崔永明 董雄伟 李强 蔡亚君 刘仰硕 董会杰 于 2021-01-11 设计创作，主要内容包括：本发明涉及一种阻燃涤纶面料及其制备方法,其特征是该面料可由如下方法制得：将胺苯基-POSS与二氯磷酸甲酯反应,制得取代产物；然后在二甲基甲酰胺溶剂中,使取代产物附着于涤纶面料,制得阻燃涤纶面料。本发明制备的阻燃涤纶面料的初始极限氧指数达到了29%以上,属于难燃材料范围；经过5次水洗后,其极限氧指数没有明显下降,仍然达到了27%以上。(The invention relates to a flame-retardant polyester fabric and a preparation method thereof, which is characterized in that the fabric can be prepared by the following method: reacting aminophenyl-POSS with methyl dichlorophosphate to prepare a substituted product; and then in a dimethyl formamide solvent, attaching the substitution product to the polyester fabric to obtain the flame-retardant polyester fabric. The initial limit oxygen index of the flame-retardant polyester fabric prepared by the invention reaches over 29 percent, and belongs to the range of flame-retardant materials; after 5 times of water washing, the limiting oxygen index is not obviously reduced and still reaches more than 27 percent.)

1. The preparation method of the flame-retardant polyester fabric is characterized by comprising the following steps:

(1) dissolving 5-7 g of methyl dichlorophosphate and 1-2 g of triethylamine in tetrahydrofuran in a four-neck flask, stirring in ice bath, and introducing N₂Protecting, namely dissolving 5-7 g of aminophenyl-POSS in tetrahydrofuran, dropwise adding the tetrahydrofuran solution containing aminophenyl-POSS into the tetrahydrofuran solution containing methyl dichlorophosphate and triethylamine at the dropping speed of 1-3 drops/second, reacting for 8-10 hours at constant temperature in an ice bath after the dropwise adding is finished, and after the reaction is finished, carrying out reduced pressure suction filtration, rotary evaporation and drying to obtain a substitution product of aminophenyl-POSS and methyl dichlorophosphate;

dissolving the substituted product of aminophenyl-POSS and methyl dichlorophosphate prepared in the step (1) in a dimethylformamide solvent, adding a polyester fabric, heating to 120-130 ℃, and reacting for the following time: 1-2 h; after the reaction is finished, washing the polyester fabric for 3-5 times by using tap water, and finally drying to obtain the flame-retardant polyester fabric; the initial limit oxygen index of the flame-retardant polyester fabric is higher than 29%, and after 5 times of water washing, the limit oxygen index is higher than 27%.

2. The preparation method of the flame-retardant polyester fabric as claimed in claim 1, wherein the volume ratio of the tetrahydrofuran solution containing amine phenyl-POSS to the tetrahydrofuran solution containing methyl dichlorophosphate and triethylamine in the step (1) is as follows: 1: 3-5.

3. The preparation method of the flame-retardant polyester fabric according to claim 1, wherein the dosage ratio of the polyester fabric (g) in the step (2), the dimethylformamide solvent (mL) and the substitution product (g) of aminophenyl-POSS and methyl dichlorophosphate prepared in the step (1) is as follows: 1: 100 to 120: 0.1 to 0.2.

4. The flame-retardant polyester fabric is characterized by being prepared by the preparation method of the flame-retardant polyester fabric according to any one of claims 1 to 3.

Technical Field

The invention belongs to the technical field of fabric preparation, and particularly relates to a flame-retardant polyester fabric and a preparation method thereof.

Background

In recent years, the number of fires occurring in China has a tendency to rise, and it has been reported that the fires caused by textiles account for half of the total number of fires. Therefore, the prevention of fire problems caused by textiles draws attention from people of all countries in the world, and meanwhile, the research and development of the flame retardant property of the textiles are accelerated.

The terylene fabric is a chemical fiber garment fabric commonly used in daily life, and has higher strength and elastic recovery capability; although the moisture absorption of the polyester fabric is poor, the polyester fabric is extremely easy to dry after being washed, does not deform and has good wearability after being washed; the terylene is also the fabric with the best heat resistance in the synthetic fiber fabric, has thermoplasticity, and has very good light resistance, acid resistance, alkali resistance and other chemical properties.

The terylene fabric is widely applied to clothes and industrial fabrics, and can also be applied to outdoor articles such as various bags and tents. However, the polyester fabric has the characteristic of being very flammable due to the characteristic of synthetic materials, so that the application field of the polyester fabric is greatly limited. Therefore, the research on the flame retardant property of the polyester fabric is very important.

The research and study of the literature show that the flame retardant property of the polyester fabric is widely concerned. At present, the preparation method of the flame-retardant polyester fabric is mainly to soak the polyester fabric into a prepared flame-retardant solution, so that the fabric has high-efficiency flame-retardant performance; such as: the Chinese patent application No. 201310280126.4 discloses a preparation method of a flame-retardant polyester fabric, which is prepared by the following steps: soaking the terylene fabric in a soaking solution containing a flame retardant, wherein the flame retardant is prepared by compounding ammonium polyphosphate, tetrahydro-methyl sulfuric acid and an aluminum hydroxide solution. The flame retardant performance research of the flame retardant polyester fabric prepared by the method has many defects, because the flame retardant is attached to the surface of the fiber, absorbs heat in a combustion area under the condition of fabric combustion, dilutes and isolates air, so that combustion is prevented, the flame retardant is washed away after multiple times of washing, and the flame retardant capability of the fiber is weakened; meanwhile, the flame retardant is added on the surface of the polyester fabric, so that the fabric feels astringent and is not soft.

Therefore, it is a goal of those engaged in the fabric research field to obtain a polyester fabric with excellent flame retardant properties.

Disclosure of Invention

Aiming at the defects in the prior art, the invention aims to provide a flame-retardant polyester fabric and a preparation method thereof.

The invention aims to provide a flame-retardant polyester fabric, which can be prepared by the following method: reacting aminophenyl-POSS with methyl dichlorophosphate to prepare a substituted product; and then in a dimethyl formamide solvent, attaching the substitution product to the polyester fabric to obtain the flame-retardant polyester fabric.

The invention aims to provide a preparation method of a flame-retardant polyester fabric, which comprises the following steps:

(1) dissolving 5-7 g of methyl dichlorophosphate and 1-2 g of triethylamine in tetrahydrofuran in a four-neck flask, stirring in ice bath, and introducing N₂And (2) protection, dissolving 5-7 g of aminophenyl-POSS in tetrahydrofuran, dropwise adding the tetrahydrofuran solution containing aminophenyl-POSS into the tetrahydrofuran solution containing methyl dichlorophosphate and triethylamine at a dropping speed of 1-3 drops/second, reacting for 8-10 hours in an ice bath at constant temperature after the dropwise addition is finished, and performing reduced pressure suction filtration, rotary evaporation and drying to obtain a substitution product of aminophenyl-POSS and methyl dichlorophosphate.

Preferably, the volume ratio of the tetrahydrofuran solution containing amine phenyl-POSS to the tetrahydrofuran solution containing methyl dichlorophosphate and triethylamine is as follows: 1: 3-5.

(2) Dissolving the substituted product of aminophenyl-POSS and methyl dichlorophosphate prepared in the step (1) in a dimethylformamide solvent, adding a polyester fabric, heating to 120-130 ℃, and reacting for the following time: 1-2 h; and after the reaction is finished, washing the polyester fabric for 3-5 times by using tap water, and finally drying to obtain the flame-retardant polyester fabric.

Preferably, the dosage ratio of the terylene fabric (g), the dimethylformamide solvent (mL) and the substitution product (g) of aminophenyl-POSS and methyl dichlorophosphate prepared in the step (1) is as follows: 1: 100 to 120: 0.1 to 0.2.

Compared with the prior art, the invention has the following beneficial effects:

(1) the invention realizes that the compound containing organic silicon and organic phosphorus is grafted on the surface of the terylene fabric, and the method obviously improves the flame retardant property of the terylene fabric.

(2) The initial limit oxygen index of the flame-retardant polyester fabric prepared by the invention reaches over 29 percent, and belongs to the range of flame-retardant materials; after 5 times of water washing, the limiting oxygen index is not obviously reduced and still reaches more than 27 percent.

(3) The compound containing organic silicon and organic phosphorus is prepared through polymerization reaction, and the compound containing organic silicon and organic phosphorus is an excellent flame retardant, so that the prepared polyester fabric also has excellent flame retardant property.

(4) According to the invention, the compound containing organic silicon and organic phosphorus and the polyester fabric are subjected to chemical reaction to realize the combination of the organic silicon and organic phosphorus, so that the flame retardant property of the polyester fabric is not weakened after the polyester fabric is washed for many times.

(5) The flame-retardant polyester fabric prepared by the method has strong flame retardance, simple whole production process, low price and small environmental pollution in the production process.

Detailed Description

The examples described below illustrate the invention in detail.

The main raw material sources are as follows: the purchased flame-retardant polyester fabric is purchased from Zhuocheng specialty textiles GmbH in New county; aminophenylsilsesquioxane (aminophenyl-POSS) is available from Shanghai Michelin Biotechnology Ltd and has the following molecular structure:

example 1

The preparation method of the flame-retardant polyester fabric comprises the following steps:

(1) 6g of methyl dichlorophosphate and 1.5g of triethylamine were dissolved in 100mL of tetrahydrofuran in a four-necked flask, stirred in an ice bath and charged with N₂And (2) protection, namely dissolving 6g of aminophenyl-POSS in 400mL of tetrahydrofuran, dropwise adding the tetrahydrofuran solution containing the aminophenyl-POSS into the tetrahydrofuran solution containing methyl dichlorophosphate and triethylamine at a dropping speed of 2 drops/second, after the dropwise addition is finished, carrying out ice-bath constant-temperature reaction for 9 hours, after the reaction is finished, carrying out reduced pressure suction filtration, rotary evaporation and drying to obtain a substitution product of the aminophenyl-POSS and methyl dichlorophosphate.

(2) Dissolving 1.5g of substituted product of aminophenyl-POSS and methyl dichlorophosphate prepared in the step (1) in 1100mL of dimethylformamide solvent, adding 10g of polyester fabric, heating to 125 ℃, and reacting for the following time: 1.5 h; and after the reaction is finished, washing the polyester fabric for 4 times by using tap water, and finally drying to obtain the flame-retardant polyester fabric.

Example 2

The preparation method of the flame-retardant polyester fabric comprises the following steps:

(1) in a four-necked flask, 5g of methyl dichlorophosphate and 1g of triethylamine were dissolved in 100mL of tetrahydrofuran, stirred in an ice bath and charged with N₂And (2) protection, dissolving 5g of aminophenyl-POSS in 300mL of tetrahydrofuran, dropwise adding the tetrahydrofuran solution containing aminophenyl-POSS into the tetrahydrofuran solution containing methyl dichlorophosphate and triethylamine at a dropping speed of 1 drop/second, reacting for 8 hours at constant temperature in an ice bath after the dropwise addition is finished, and performing reduced pressure suction filtration, rotary evaporation and drying to obtain a substitution product of aminophenyl-POSS and methyl dichlorophosphate.

(2) Dissolving 1g of the substituted product of aminophenyl-POSS and methyl dichlorophosphate prepared in the step (1) in 1000mL of dimethylformamide solvent, adding 10g of polyester fabric, heating to 120 ℃, and reacting for the following time: 1 h; and after the reaction is finished, washing the polyester fabric for 3 times by using tap water, and finally drying to obtain the flame-retardant polyester fabric.

Example 3

The preparation method of the flame-retardant polyester fabric comprises the following steps:

(1) in a four-necked flask, 7g of methyl dichlorophosphate and 2g of triethylamine were dissolved in 100mL of tetrahydrofuran, stirred in an ice bath and charged with N₂And (2) protection, dissolving 7g of aminophenyl-POSS in 500mL of tetrahydrofuran, dropwise adding the tetrahydrofuran solution containing aminophenyl-POSS into the tetrahydrofuran solution containing methyl dichlorophosphate and triethylamine at the dropping speed of 3 drops/second, reacting for 10 hours at constant temperature in an ice bath after the dropwise addition is finished, and performing reduced pressure suction filtration, rotary evaporation and drying to obtain a substitution product of aminophenyl-POSS and methyl dichlorophosphate.

(2) Dissolving 2g of the substitution product of aminophenyl-POSS and methyl dichlorophosphate prepared in the step (1) in 1200mL of dimethylformamide solvent, adding 10g of terylene fabric, heating to 130 ℃, and reacting for the following time: 2 h; and after the reaction is finished, washing the polyester fabric for 5 times by using tap water, and finally drying to obtain the flame-retardant polyester fabric.

Comparative example A

In this comparative example, "6 g of aminophenyl-POSS" in the step (1) was reduced to "0.6 g of aminophenyl-POSS" by way of comparison with example 1, and the other production process was carried out in accordance with the production process of example 1.

Comparative example B

In this comparative example, "6 g of aminophenyl-POSS" in the step (1) was increased to "30 g of aminophenyl-POSS" by way of comparison with example 1, and other production methods were carried out in accordance with the production method of example 1.

Comparative example C

In this comparative example, "1.5 g of the substitution product of aminophenyl-POSS with methyl dichlorophosphate obtained in step (1)" was reduced to "0.15 g of the substitution product of aminophenyl-POSS with methyl dichlorophosphate obtained in step (1)" in step (2), by way of comparison with example 1, and the other preparation methods were carried out in accordance with the preparation method of example 1.

Comparative example D

In this comparative example, "1.5 g of the substitution product of aminophenyl-POSS with methyl dichlorophosphate obtained in step (1)" was added to "15 g of the substitution product of aminophenyl-POSS with methyl dichlorophosphate obtained in step (1)" in step (2), by way of comparison with example 1, and the other preparation method was carried out in accordance with the preparation method of example 1.

Comparative example E

In this comparative example, "1100 mL of dimethylformamide" was changed to "110 mL of dimethylformamide" in step (2) by way of comparison with example 1, and the other preparation method was carried out in the same manner as in example 1.

Comparative example F

In this comparative example, "1100 mL of dimethylformamide" was changed to "11000 mL of dimethylformamide" in step (2) by way of comparison with example 1, and the other preparation method was carried out in accordance with the preparation method of example 1.

Performance evaluation examples:

in order to better detect the flame retardance of the polyester fabric prepared in the invention, the flame retardance of the polyester fabric prepared in the specific embodiments 1-3 and the comparative examples A-F in the invention and the flame retardant performance of the purchased flame retardant polyester fabric are tested, and the test method adopts an oxygen index test method, namely, the polyester fabric is subjected to standard washing according to GB/T5454 1997 textile combustion performance test oxygen index method, and reference GB/T20944.1-2007 washing fastness tester washing method. The test results are shown in table 1.

TABLE 1 flame retardancy test results of the polyester fabrics prepared in examples 1-3 and comparative examples A-F and the purchased polyester fabrics after 5 times of water washing and water washing

The limiting oxygen index LOI is one of important indexes of flame-retardant materials, and materials with the limiting oxygen index of more than 28 percent are flame-retardant materials generally. As can be seen from Table 1, the initial limit oxygen index of the flame-retardant polyester fabric prepared by the invention reaches over 29 percent, and the flame-retardant polyester fabric belongs to the range of flame-retardant materials; after 5 times of water washing, the limiting oxygen index is not obviously reduced and still reaches more than 27 percent. After 5 times of washing, the flame retardant performance of the flame retardant polyester fabric prepared by the invention is slightly higher than that of the purchased flame retardant polyester fabric. The flame retardant property test shows that: the flame-retardant polyester fabric prepared by the invention has a good flame-retardant effect, and is a qualified flame-retardant polyester fabric.