Flame-retardant polyester fabric and preparation method thereof

Abstract

The present application relates to a kind of flame-retardant polyester fabric and its preparation method, its characteristics are that the fabric can be prepared by the following method: first, acryloyl chloride is reacted with bis-hydroxymethyl phosphine oxide to prepare phosphide containing double bond;Second, chloropropyl-POSS is reacted with acrylamide to prepare POSS compound containing double bond;Finally, phosphide containing double bond, POSS compound containing double bond and polyester fabric are reacted under the condition of initiator azobisisobutyronitrile to prepare flame-retardant polyester fabric.The initial limiting oxygen index of the flame-retardant polyester fabric prepared by the present application reaches more than 29%, which belongs to the range of difficult-to-burn materials;After 10 times of washing, its limiting oxygen index does not decrease significantly, still reaches more than 28%;In addition, after being washed for 10 times, the flame-retardant performance of the flame-retardant polyester fabric prepared by the present application exceeds the flame-retardant performance of the purchased flame-retardant polyester fabric.

Description

TECHNICAL FIELD

[0001] The present application belongs to the technical field of fabric preparation, and particularly relates to a flame-retardant polyester fabric and a preparation method thereof. BACKGROUND

[0002] With the development of science and technology and the progress of the textile industry, the consumption of various textiles has rapidly increased. The fire caused by the ignition of textiles or the flammability of textiles also shows an upward trend. Textiles are widely used in various fields, from clothing fabrics to interior decoration of buildings and industrial fabrics, so the use of flame-retardant fabrics in places where fires are prone to occur has been increasingly valued by people.

[0003] Polyester fabric is a fabric made of polyester fiber as raw material. It has many good properties such as high strength, good elasticity, good light and heat resistance, excellent chemical stability, good abrasion resistance, and dimensional stability, and is widely used in national defense, industrial fabrics, and various aspects of people's lives. However, polyester fiber is a flammable fiber, and its limiting oxygen index is only about 21%, which cannot meet the requirements of some fields for flame retardant properties. It is necessary to flame retardant polyester fiber, which has important practical significance and broad application prospects.

[0004] At present, the flame-retardant methods of polyester can be divided into the following three types according to the introduction method of flame-retardant additives: one is the copolymerization method, which means that the flame-retardant agent is copolymerized with the polymer monomer in the polymerization stage, or the flame-retardant group is introduced into the high molecular chain for graft modification, and then the flame-retardant polyester fiber is prepared by melt spinning; the second is the blending method, which means that the flame-retardant additive is added to the spinning melt to spin the flame-retardant polyester fiber; the third is the post-treatment method, mainly including coating method, spraying method, dipping and drying method, padding and baking method, etc., so that the flame-retardant agent is fixed on the fabric to obtain the flame-retardant effect. With the continuous deepening of the research on flame-retardant technology, some new methods have also been used to modify the flame retardant of polyester, such as composite spinning modification method and graft modification method.

[0005] According to the literature research, the flame-retardant properties of polyester fabric have been widely concerned. For example, Chinese invention patent application No. 201911188820.7 discloses a kind of flame-retardant polyester fiber and its preparation method, which is prepared by the following method: the polyester chip obtained by chemical synthesis is mixed with activated carbon and flame-retardant particles, and then added to the screw extruder for high-speed spinning, and finally the flame-retardant polyester fiber is obtained. The flame-retardant particles are prepared by uniformly mixing tricresyl phosphate, magnesium hydroxide, kaolin and zirconium oxide, heating and cooling, and grinding into powder. However, the preparation method has relatively complex raw materials and cumbersome steps, and the flame-retardant effect gradually weakens with the increase of the washing times of the polyester fabric. Therefore, it is the goal of the personnel engaged in fabric research to obtain a polyester fabric with excellent flame-retardant properties. SUMMARY

[0006] In view of the above-mentioned drawbacks in the prior art, the present application aims to provide a flame-retardant polyester fabric and a preparation method thereof.

[0007] The present application aims to provide a flame-retardant polyester fabric, which can be prepared by the following method: first, acryloyl chloride is reacted with bis-hydroxymethyl phosphine oxide to obtain a phosphine compound containing double bonds; second, chloropropyl-POSS is reacted with acrylamide to obtain a POSS compound containing double bonds; and finally, the phosphine compound containing double bonds, the POSS compound containing double bonds and a polyester fabric are reacted under the condition of an initiator azobisisobutyronitrile to obtain the flame-retardant polyester fabric.

[0008] Another object of the present application is to provide a preparation method of the flame-retardant polyester fabric, which comprises the following steps:

[0009] (1) Reaction of acryloyl chloride and bis-hydroxymethyl phosphine oxide: 5-7 g of bis-hydroxymethyl phosphine oxide and 1-2 g of triethylamine are dissolved in tetrahydrofuran in a four-necked flask, and ice-bath stirring and N2 protection are performed; 4-6 g of acryloyl chloride is dissolved in tetrahydrofuran, and the tetrahydrofuran solution of acryloyl chloride is added dropwise to the tetrahydrofuran solution of bis-hydroxymethyl phosphine oxide and triethylamine at a dropwise addition speed of 1-3 drops / s; after the dropwise addition is completed, ice-bath constant temperature reaction is performed; after the reaction is completed, vacuum filtration is performed, rotary evaporation is performed, and drying is performed to obtain the phosphine compound containing double bonds.

[0010] Preferably, the use amount ratio of the tetrahydrofuran (mL) solution of acryloyl chloride to the tetrahydrofuran (mL) solution of bis-hydroxymethyl phosphine oxide and triethylamine is 1:3-5.

[0011] Preferably, the reaction time is 4-6 h.

[0012] (2) Reaction of chloropropyl-POSS and acrylamide: 5-7 g of chloropropyl-POSS and 1-2 g of triethylamine are dissolved in 150 mL of tetrahydrofuran in a four-necked flask, and ice-bath stirring and N2 protection are performed; 4-6 g of acrylamide is dissolved in 100 mL of tetrahydrofuran, and the tetrahydrofuran solution of acrylamide is added dropwise to the tetrahydrofuran solution of chloropropyl-POSS and triethylamine at a dropwise addition speed of 1-3 drops / s; after the dropwise addition is completed, ice-bath constant temperature reaction is performed; after the reaction is completed, vacuum filtration is performed, rotary evaporation is performed, and drying is performed to obtain the POSS compound containing double bonds.

[0013] Preferably, the reaction time is 5-9 h.

[0014] (3) Preparation of the flame-retardant polyester fabric: the double-bond-containing phosphide prepared in step (1), the double-bond-containing POSS compound prepared in step (2) and azobisisobutyronitrile are dissolved in an organic solvent to prepare a finishing solution; the finishing solution is heated to 90-100°C, and the polyester fabric is immersed in the finishing solution for 1-2 hours; the immersed polyester fabric is taken out and washed with a large amount of tap water, and dried to obtain the flame-retardant polyester fabric.

[0015] Preferably, the organic solvent is dimethylformamide.

[0016] Preferably, the use amount ratio of the double-bond-containing phosphide (g) prepared in step (1), the double-bond-containing POSS compound (g) prepared in step (2) and azobisisobutyronitrile (g) to the organic solvent (mL) is 1:1-2:0.1-0.2:100-200.

[0017] Compared with the prior art, the present application has the following advantages:

[0018] (1) The present application realizes the grafting of the compound containing silicon and phosphorus on the surface of the polyester fabric, and significantly improves the flame-retardant property of the polyester fabric.

[0019] (2) The present inventors have unexpectedly found that the initial limiting oxygen index of the flame-retardant polyester fabric prepared by the present application is above 29%, which belongs to the range of difficult-to-burn materials; after 10 times of washing, the limiting oxygen index does not decrease obviously and is still above 28%; in addition, after 10 times of washing, the flame-retardant property of the flame-retardant polyester fabric prepared by the present application is better than that of the purchased flame-retardant polyester fabric.

[0020] (3) The present application prepares the compound containing silicon and phosphorus, which is reacted with the polyester fabric through a chemical reaction; the compound containing silicon and phosphorus is an excellent flame-retardant material, so that the prepared polyester fabric also has excellent flame-retardant property.

[0021] (4) The present inventors have unexpectedly found that the chemical reaction of the compound containing silicon and phosphorus with the polyester fabric can realize the firm combination of the two; it is further found that the flame-retardant property of the polyester fabric is not weakened after multiple times of washing.

[0022] (5) The flame-retardant polyester fabric prepared by the method of the present application has strong flame-retardant property, the whole production process is simple, the price is low, and the production process has little environmental pollution. DETAILED DESCRIPTION

[0023] The following examples and comparative examples illustrate the present application in detail.

[0024] Main raw material source: The purchased flame-retardant polyester fabric was purchased from Xinxiang Zhuocheng Special Textile Co., Ltd. The chloropropyl-POSS was purchased from Shanghai Maikelin Biochemical Technology Co., Ltd., and its molecular structure is as follows:

[0025]

[0026] Example 1

[0027] The preparation method of the flame-retardant polyester fabric of the present embodiment comprises the following steps:

[0028] (1) Reaction of acryloyl chloride and bis-hydroxymethyl phosphine oxide: 6 g of bis-hydroxymethyl phosphine oxide and 1.5 g of triethylamine were dissolved in 200 mL of tetrahydrofuran in a four-necked flask, and stirred in an ice bath and protected by N2. 5 g of acryloyl chloride was dissolved in 50 mL of tetrahydrofuran, and the tetrahydrofuran solution of acryloyl chloride was added dropwise to the tetrahydrofuran solution of bis-hydroxymethyl phosphine oxide and triethylamine at a rate of 2 drops per second. After the dropwise addition was completed, the reaction was carried out in an ice bath. The reaction time was 5 h. After the reaction was completed, vacuum filtration, rotary evaporation and drying were carried out to obtain a phosphine compound containing a double bond.

[0029] (2) Reaction of chloropropyl-POSS and acrylamide: 6 g of chloropropyl-POSS and 1.5 g of triethylamine were dissolved in 150 mL of tetrahydrofuran in a four-necked flask, and stirred in an ice bath and protected by N2. 5 g of acrylamide was dissolved in 100 mL of tetrahydrofuran, and the tetrahydrofuran solution of acrylamide was added dropwise to the tetrahydrofuran solution of chloropropyl-POSS and triethylamine at a rate of 2 drops per second. After the dropwise addition was completed, the reaction was carried out in an ice bath. The reaction time was 7 h. After the reaction was completed, vacuum filtration, rotary evaporation and drying were carried out to obtain a POSS compound containing a double bond.

[0030] (3) Preparation of flame-retardant polyester fabric: 1 g of the phosphine compound containing a double bond prepared in step (1), 1.5 g of the POSS compound containing a double bond prepared in step (2), and 0.15 g of azobisisobutyronitrile were dissolved in 150 mL of dimethylformamide to prepare a finishing solution. The finishing solution was heated to 95°C, and the polyester fabric was immersed in the finishing solution for 1.5 hours. The immersed polyester fabric was washed with a large amount of tap water, and dried to obtain a flame-retardant polyester fabric.

[0031] Example 2

[0032] The preparation method of the flame-retardant polyester fabric of the present embodiment comprises the following steps:

[0033] (1) Acryloyl chloride and bis-hydroxymethyl phosphine oxide reaction: In a four-necked flask, 5 g of bis-hydroxymethyl phosphine oxide and 1.5 g of triethylamine were dissolved in 150 mL of tetrahydrofuran, stirred in an ice bath and protected by N2, 5 g of acryloyl chloride was dissolved in 50 mL of tetrahydrofuran, the tetrahydrofuran solution of acryloyl chloride was added dropwise to the tetrahydrofuran solution of bis-hydroxymethyl phosphine oxide and triethylamine, the dropwise addition rate was 1 drop / s, after the dropwise addition was completed, the reaction was kept in an ice bath, the reaction time was 4 h, after the reaction was completed, vacuum filtration, rotary evaporation and drying were performed to obtain a double bond-containing phosphine compound.

[0034] (2) Chloropropyl-POSS and acrylamide reaction: In a four-necked flask, 5 g of chloropropyl-POSS and 1 g of triethylamine were dissolved in 150 mL of tetrahydrofuran, stirred in an ice bath and protected by N2, 4 g of acrylamide was dissolved in 100 mL of tetrahydrofuran, the tetrahydrofuran solution of acrylamide was added dropwise to the tetrahydrofuran solution of chloropropyl-POSS and triethylamine, the dropwise addition rate was 1 drop / s, after the dropwise addition was completed, the reaction was kept in an ice bath, the reaction time was 5 h, after the reaction was completed, vacuum filtration, rotary evaporation and drying were performed to obtain a double bond-containing POSS compound.

[0035] (3) Preparation of flame-retardant polyester fabric: 1 g of the double bond-containing phosphine compound prepared in step (1), 1 g of the double bond-containing POSS compound prepared in step (2) and 0.1 g of azobisisobutyronitrile were dissolved in 100 mL of an organic solvent to prepare a finishing liquid; the finishing liquid was heated to 90°C, and the polyester fabric was immersed in the finishing liquid for 1 h; the immersed polyester fabric was washed with a large amount of tap water, dried and obtained as a flame-retardant polyester fabric.

[0036] Example 3

[0037] The preparation method of the flame-retardant polyester fabric of the present embodiment comprises the following steps:

[0038] (1) Acryloyl chloride and bis-hydroxymethyl phosphine oxide reaction: In a four-necked flask, 5 g of bis-hydroxymethyl phosphine oxide and 1.5 g of triethylamine were dissolved in 150 mL of tetrahydrofuran, stirred in an ice bath and protected by N2, 5 g of acryloyl chloride was dissolved in 50 mL of tetrahydrofuran, the tetrahydrofuran solution of acryloyl chloride was added dropwise to the tetrahydrofuran solution of bis-hydroxymethyl phosphine oxide and triethylamine, the dropwise addition rate was 1 drop / s, after the dropwise addition was completed, the reaction was kept in an ice bath, the reaction time was 4 h, after the reaction was completed, vacuum filtration, rotary evaporation and drying were performed to obtain a double bond-containing phosphine compound.

[0039] (2) Chloropropyl-POSS reacted with acrylamide: 7 g of chloropropyl-POSS and 2 g of triethylamine were dissolved in 150 mL of tetrahydrofuran in a four-necked flask, stirred in an ice bath and protected by N2, 6 g of acrylamide was dissolved in 100 mL of tetrahydrofuran, the tetrahydrofuran solution of acrylamide was added dropwise into the tetrahydrofuran solution of chloropropyl-POSS and triethylamine, the dropping speed was 3 drops per second, after the dropping was completed, the reaction was kept in an ice bath, the reaction time was 9 h, after the reaction was completed, filtration was performed under reduced pressure, rotary evaporation was performed, and drying was performed to obtain a double-bond-containing POSS compound.

[0040] (3) Preparation of flame-retardant polyester fabric: 1 g of the double-bond-containing phosphide prepared in step (1), 2 g of the double-bond-containing POSS compound prepared in step (2) and 0.2 g of azobisisobutyronitrile were dissolved in 200 mL of dimethylformamide to prepare a finishing solution; the finishing solution was heated to 100°C, and the polyester fabric was immersed in the finishing solution for 2 h; the immersed polyester fabric was washed with a large amount of tap water, and dried to obtain the flame-retardant polyester fabric.

[0041] Comparative Example A

[0042] In comparison with Example 1, in the present comparative example, step "(1) acryloyl chloride reacted with bis-hydroxymethyl phosphine oxide" was not implemented, that is, "1 g of the double-bond-containing phosphide prepared in step (1)" was deleted in step (3), and the other preparation methods were implemented according to the preparation method of Example 1.

[0043] Comparative Example B

[0044] In comparison with Example 1, in the present comparative example, step "(2) chloropropyl-POSS reacted with acrylamide" was not implemented, that is, "1.5 g of the double-bond-containing POSS compound prepared in step (2)" was deleted in step (3), and the other preparation methods were implemented according to the preparation method of Example 1.

[0045] Comparative Example C

[0046] In comparison with Example 1, in the present comparative example, the amount of "azobisisobutyronitrile" was reduced from 0.15 g to 0.015 g in step (3), and the other preparation methods were implemented according to the preparation method of Example 1.

[0047] Comparative Example D

[0048] In comparison with Example 1, in the present comparative example, the amount of "azobisisobutyronitrile" was increased from 0.15 g to 1.5 g in step (3), and the other preparation methods were implemented according to the preparation method of Example 1.

[0049] Performance evaluation example:

[0050] In order to better detect the flame retardancy of the terylene fabric prepared in the application, the flame retardant properties of the terylene fabrics prepared in the above specific examples 1-3 and comparative examples A-D and the purchased flame-retardant terylene fabric in the application were tested, and the test method was the oxygen index test method, that is, according to GB / T 5454-1997 "Textile Burning Property Test Oxygen Index Method", the terylene fabric was standard washed according to GB / T 20944.1-2007 washing method for color fastness. The test results are shown in Table 1.

[0051] Table 1 Flame retardant test results of terylene fabrics prepared in examples 1-3 and comparative examples A-D and purchased terylene fabric after no washing and washing 10 times

[0052]

[0053] The limiting oxygen index LOI is one of the important indicators of flame-retardant materials. Generally, materials with a limiting oxygen index greater than 28% are difficult to burn. As can be seen from Table 1, the initial limiting oxygen index of the flame-retardant terylene fabric prepared in the application is more than 29%, which belongs to the range of difficult-to-burn materials. After 10 times of washing, the limiting oxygen index does not decrease significantly, and is still more than 28%. In addition, after 10 times of washing, the flame retardant performance of the flame-retardant terylene fabric prepared in the application exceeds that of the purchased flame-retardant terylene fabric. In addition, the inventors of the present application further found that the limiting oxygen index of the terylene fabric prepared in comparative examples A-D is relatively small, which indicates that the selection of phosphide containing double bonds, the selection of POSS compound containing double bonds and the amount of azobisisobutyronitrile all have important influence on the flame retardant performance of terylene fabric. The flame retardant performance test shows that the flame-retardant terylene fabric prepared in the application has good flame retardant effect and is a qualified flame-retardant terylene fabric.

Claims

1. A process for the preparation of flame retardant polyester fabric, characterized by, The method comprises the following steps: The phosphide containing double bond, the POSS compound containing double bond and the azobisisobutyronitrile are dissolved in the organic solvent to prepare a finishing liquor; the finishing liquor is heated to 90-100 DEG C, and the polyester fabric is immersed in the finishing liquor for 1-2 hours; the immersed polyester fabric is taken out and washed with a large amount of tap water, and dried to obtain the flame-retardant polyester fabric; wherein the initial limiting oxygen index of the flame-retardant polyester fabric is higher than 29%, and the limiting oxygen index is higher than 28% after 10 times of washing; The organic solvent is dimethylformamide; the use amount ratio of the phosphide containing double bond, the POSS compound containing double bond, the azobisisobutyronitrile and the organic solvent is 1g: (1-2) g: (0.1-0.2) g: (100-200) mL; The preparation method of the phosphide containing double bond comprises the following steps: 5-7g of bis-hydroxymethyl phosphine oxide and 1-2g of triethylamine are dissolved in tetrahydrofuran in a four-necked flask, ice-bath stirring is carried out and N2 protection is carried out, 4-6g of acryloyl chloride is dissolved in tetrahydrofuran, the tetrahydrofuran containing the acryloyl chloride is added dropwise into the tetrahydrofuran containing the bis-hydroxymethyl phosphine oxide and the triethylamine, the dropwise adding speed is 1-3 drops / s, after the dropwise adding is completed, ice-bath constant temperature reaction is carried out, after the reaction is completed, vacuum filtration is carried out, rotary evaporation is carried out, and drying is carried out to obtain the phosphide containing double bond. The preparation method of the POSS compound containing double bond comprises the following steps: 5-7g of chloropropyl-POSS and 1-2g of triethylamine are dissolved in 150mL of tetrahydrofuran in a four-necked flask, ice-bath stirring is carried out and N2 protection is carried out, 4-6g of acrylamide is dissolved in 100mL of tetrahydrofuran, the tetrahydrofuran containing the acrylamide is added dropwise into the tetrahydrofuran containing the chloropropyl-POSS and the triethylamine, the dropwise adding speed is 1-3 drops / s, after the dropwise adding is completed, ice-bath constant temperature reaction is carried out, after the reaction is completed, vacuum filtration is carried out, rotary evaporation is carried out, and drying is carried out to obtain the POSS compound containing double bond.

2. A process for the preparation of flame retardant polyester fabric as claimed in claim 1, wherein, The ice-bath constant temperature reaction time in the preparation method of the POSS compound containing double bond is 5-9h.

3. A flame retardant polyester fabric, characterized in that, The flame-retardant polyester fabric is prepared by the preparation method of the flame-retardant polyester fabric according to any one of claims 1-2.

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