A tris(ethylene glycol) ammonium phosphate flame retardant, a flame retardant finishing solution, and their preparation methods and applications

By using triethylene glycol amine phosphate salt flame retardant and green flame retardant finishing solution, the problem of insufficient flame retardant performance of suede fabrics is solved, and an efficient and environmentally friendly flame retardant effect is achieved, generating non-toxic gases and improving the high temperature resistance of the fabric.

CN119708047BActive Publication Date: 2025-05-30ZHEJIANG MEISHENG NEW MATERIALS CO LTD +1
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Patent Information

Application Number
CN202510220815.9
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2025-02-27
Publication Date
2025-05-30
Estimated Expiration
2045-02-27

AI Technical Summary

Technical Problem

The flame retardant properties of echoed suede fabrics are insufficient. Traditional halogen-containing flame retardants release toxic gases when burning, which cannot meet the requirements of modern society for green and environmental protection.

Method used

A flame retardant containing nitrogen and phosphorus elements is used to form a flame retardant containing nitrogen and phosphorus through the condensation reaction principle, and is compounded with 3-aminopropyltriethoxysilane to form a green flame retardant finish. Through impregnation and high-temperature curing treatment, the flame retardant performance of the fabric is enhanced.

Benefits of technology

It realizes the efficient flame retardant properties of the suede fabric, produces non-toxic or low-toxic gases, reduces oxygen concentration, forms a dense carbon layer, isolates combustion heat and flammable gases, improves the high-temperature resistance and anti-aging properties of the fabric, and meets environmental protection requirements.

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Abstract

The present invention belongs to the technical field of textile fabrics, and provides a triethylene glycol phosphoric acid amine salt flame retardant, a green flame retardant finishing solution, and a preparation method and application thereof. The method of the present invention comprises the following steps: reacting triethylene glycol and phosphoric acid to obtain a viscous solution; dropping a urea solution into the viscous solution for reaction to obtain triethylene glycol phosphoric acid amine salt. An aqueous solution of triethylene glycol phosphoric acid amine salt is dropped into a colloidal solution of 3-aminopropyltriethoxysilane to obtain a flame retardant finishing solution. In the present invention, triethylene glycol, phosphoric acid and urea form a triethylene glycol phosphoric acid amine salt flame retardant. The structure of the flame retardant contains rich nitrogen and phosphorus elements at the same time, enabling the flame retardant to quickly form carbon during combustion, forming a dense carbon layer to isolate the interior of the material from contact with air; 3-aminopropyltriethoxysilane is added to the flame retardant finishing solution, and compounded with triethylene glycol phosphoric acid amine salt, which has good flame retardant synergistic effect and can improve the carbon formation property of fiber materials.
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Description

Technical Field

[0001] The present invention relates to the technical field of textile fabrics, and particularly to a triethylene glycol phosphate amine salt flame retardant, a green flame retardant finishing solution, and their preparation methods and applications. Background Art

[0002] Suede-like fabrics occupy an important position in many fields due to their unique texture and properties. It has a soft and delicate touch similar to natural suede, and at the same time has good warmth retention and moisture absorption properties, which makes it very popular in industries such as clothing, home decoration, and automotive interiors. In terms of production process, suede-like fabrics usually use polyester microfibers as raw materials and are made into base fabrics through needling, hydroentangling, or weaving. Subsequently, through a series of complex post-treatment processes such as dyeing, sanding, and shaping, the final product that meets market requirements can be presented. However, although suede-like fabrics perform well in appearance and some properties, they have a key problem - serious lack of flame retardancy. In actual application scenarios, the lack of flame retardancy may cause a series of safety hazards.

[0003] To solve the problem of insufficient flame retardancy, the traditional method is to add halogen-containing flame retardants. Halogen-containing flame retardants can improve the flame retardancy of materials to a certain extent. However, this method brings more serious negative impacts. During the combustion process, halogen-containing flame retardants will release a large amount of toxic gases, among which hydrogen halide is one of the main components, and the harm of these toxic gases to human health is multi-faceted.

[0004] With the development of society and the increasing awareness of environmental protection among people, the environmental protection requirements for products are getting higher and higher. Traditional halogen-containing flame retardants obviously cannot meet the requirements of modern society for green environmental protection. Consumers are more inclined to choose products that have good performance and are friendly to the environment and human health. Therefore, in the field of suede-like fabrics, there is an urgent need to develop a new type of flame retardant with high flame retardancy, non-toxic, and environmental protection characteristics. Summary of the Invention

[0005] The purpose of the present invention is to provide a triethylene glycol phosphate amine salt flame retardant, a green flame retardant finishing solution, and their preparation methods and applications in order to overcome the deficiencies of the prior art.

[0006] In order to achieve the above-mentioned invention purpose, the present invention provides the following technical solutions:

[0007] The present invention provides a preparation method of a triethylene glycol phosphate amine salt flame retardant, which comprises the following steps:

[0008] 1) Mix triethylene glycol and phosphoric acid and then react to obtain a viscous solution;

[0009] 2) Drop the urea solution into the viscous solution for reaction to obtain the triethylene glycol ammonium phosphate flame retardant.

[0010] Preferably, the molar ratio of triethylene glycol, phosphoric acid and urea in the urea solution is 1:1.8 - 2.2:3 - 5; in the urea solution, the molar volume ratio of urea to water is 1.5×10 -2 ~2.5×10 -2 mol:1 mL.

[0011] Preferably, the temperature of the reaction in step 1) is 135 - 145 °C and the reaction time is 2.5 - 3.5 h; the temperature of the reaction in step 2) is 165 - 175 °C and the reaction time is 1.8 - 2.2 h.

[0012] The present invention also provides the triethylene glycol ammonium phosphate flame retardant prepared by the preparation method of the triethylene glycol ammonium phosphate flame retardant.

[0013] The present invention also provides a method for preparing a green flame retardant finishing solution from the triethylene glycol ammonium phosphate flame retardant, comprising the following steps:

[0014] Mix 3-aminopropyltriethoxysilane and water to obtain a colloidal solution; drop the aqueous solution of triethylene glycol ammonium phosphate into the colloidal solution to obtain a green flame retardant finishing solution.

[0015] Preferably, in the colloidal solution, the molar volume ratio of 3-aminopropyltriethoxysilane to water is 4×10 -4 ~5×10 -4 mol:1 mL; in the aqueous solution of triethylene glycol ammonium phosphate, the molar volume ratio of triethylene glycol ammonium phosphate to water is 9×10 -4 ~1.5×10 -3 mol:1 mL.

[0016] Preferably, the volume ratio of the aqueous solution of triethylene glycol ammonium phosphate to the colloidal solution is 2.5 - 3.5:1; the mixing time is ≥12 h.

[0017] The present invention also provides the green flame retardant finishing solution prepared by the method for preparing a green flame retardant finishing solution from the triethylene glycol ammonium phosphate flame retardant.

[0018] The present invention also provides the application of the green flame retardant finishing solution in suede-like fabrics. Immerse the suede-like fabric in the green flame retardant finishing solution and then sequentially carry out curing, washing and drying to obtain a flame retardant suede-like fabric;

[0019] The immersion time is 5 - 8 min, the curing temperature is 145 - 155 °C, the curing time is 10 - 15 min, the drying temperature is 75 - 85 °C, and the drying time is 3 - 4 h.

[0020] Preferably, before impregnation, the green flame retardant finishing solution is stirred at 75-85 °C for a stirring time of ≥3 h; after impregnation, the fabric liquor pickup is controlled to be 125-135% and then cured.

[0021] The beneficial effects of the present invention include the following points:

[0022] 1) In the present invention, triethylene glycol, phosphoric acid and urea form a triethylene glycol phosphoamine salt flame retardant by using the principle of condensation reaction. The structure of the flame retardant contains rich nitrogen and phosphorus elements at the same time, enabling the flame retardant to quickly form carbon during combustion, forming a dense carbon layer to achieve the purpose of isolating the interior of the material from contact with air; during high-temperature combustion degradation, it can generate non-toxic and hardly flammable gases or smoke, reducing the oxygen concentration. The carbon residue containing phosphorus elements generates an expanded carbon layer due to the release of gases, isolating the heat and flammable gases generated during combustion. The simultaneous introduction of nitrogen and phosphorus can exert a good synergistic flame retardant effect.

[0023] 2) In the present invention, 3-aminopropyltriethoxysilane is added to the flame retardant finishing solution and has good flame retardant synergistic effect when compounded with triethylene glycol phosphoamine salt, which can improve the charring property of fiber materials. First, the siloxane structure is not easily thermally decomposed at high temperature and can form a physical crosslinking network with polyester fibers during the melting process, which is beneficial to increasing the thermal decomposition temperature of the fibers and enhancing the high-temperature resistance performance; second, the siloxane structure thermally decomposes at high temperature to generate inorganic silicon, which forms a continuous and dense covering layer on the material surface in combination with the carbon layer, achieving the effect of heat and oxygen insulation, inhibiting the combustion process of polyester fibers, and at the same time, the covering layer can inhibit the volatilization of flue gas, improving the smoke suppression property and anti-melting drop property.

[0024] 3) The impregnation method of the present invention is an effective process for finishing the green flame retardant finishing solution on the suede-like fabric. During the impregnation process, the flame retardant finishing solution is in full contact with the fibers and enters the interior of the fibers through osmosis. At the same time, the flame retardant molecules adsorb on the surface and inside of the fibers and can firmly adhere to the fibers. After impregnation and drying, the fibers are subjected to high-temperature treatment to thermally cure the flame retardant on the fibers. This step not only enhances the binding force between the flame retardant and the fibers but also makes it more stable; at the same time, the high-temperature treatment can also cause further chemical reactions of the flame retardant molecules on the fibers to form a more stable structure, thereby improving the durability and anti-aging performance of the flame retardant.

[0025] 4) The nitrogen-phosphorus-silicon flame retardant in the green flame retardant finishing liquid of the present invention conforms to the environmental protection concept. On the one hand, it does not contain toxic halogens, mainly produces non-toxic or low-toxic gases during combustion, and the decomposition products are relatively safe. Moreover, formaldehyde is not generated during the application process, avoiding the direct harm of formaldehyde to the human body and ensuring human health and environmental safety. On the other hand, nitrogen, phosphorus, and silicon elements are abundant in nature, the raw materials are widely sourced and relatively low in price, the production process is more environmentally friendly, and the generated three wastes are less, having significant practical value and broad market prospects. Brief Description of the Drawings

[0026] Figure 1 It is a schematic diagram of the effect of the green flame retardant finishing liquid of the present invention on suede fabric;

[0027] Figure 2 It is the Fourier transform infrared spectrum of the triethylene glycol ammonium phosphate flame retardant in Example 1;

[0028] Figure 3 It is the limiting oxygen index test results of the flame-retardant suede fabrics prepared in Examples 1 to 3 and Comparative Examples 1 to 3;

[0029] Figure 4 It is the peak heat release and total heat release of the flame-retardant suede fabrics prepared in Examples 1 to 3 and Comparative Examples 1 to 3. Detailed Embodiments

[0030] The present invention provides a preparation method of a triethylene glycol ammonium phosphate flame retardant, which comprises the following steps:

[0031] 1) React triethylene glycol and phosphoric acid after mixing to obtain a viscous solution;

[0032] 2) Drop the urea solution into the viscous solution for reaction to obtain the triethylene glycol ammonium phosphate flame retardant.

[0033] In the present invention, the molar ratio of triethylene glycol, phosphoric acid, and urea in the urea solution is preferably 1:1.8 - 2.2:3 - 5, more preferably 1:1.9 - 2.1:3.5 - 4.5, and still more preferably 1:2:4; in the urea solution, the molar volume ratio of urea to water is preferably 1.5×10 -2 ~2.5×10 -2 mol:1 mL, more preferably 1.7×10 -2 ~2.3×10 -2 mol:1 mL, and still more preferably 2×10 -2 mol:1 mL.

[0034] In the present invention, the temperature of the reaction in step 1) is preferably 135 - 145 °C, more preferably 137 - 142 °C, and even more preferably 140 °C. The reaction time is preferably 2.5 - 3.5 h, more preferably 2.8 - 3.2 h, and even more preferably 3 h. The temperature of the reaction in step 2) is preferably 165 - 175 °C, more preferably 168 - 172 °C, and even more preferably 170 °C. The reaction time is preferably 1.8 - 2.2 h, and more preferably 2 h.

[0035] In the present invention, the mixing in step 1) is preferably adding phosphoric acid dropwise to triethylene glycol. Magnetic stirring is carried out during the mixing and reaction processes, and the viscous solution is a brown viscous solution.

[0036] In the present invention, the synthetic route for preparing triethylene glycol phosphoamine salt from triethylene glycol, phosphoric acid, and urea is as follows:

[0037]

[0038] The present invention also provides a triethylene glycol phosphoamine salt flame retardant prepared by the preparation method of the triethylene glycol phosphoamine salt flame retardant.

[0039] The present invention also provides a method for preparing a green flame retardant finishing solution using the triethylene glycol phosphoamine salt flame retardant, which comprises the following steps:

[0040] Mix 3 - aminopropyltriethoxysilane and water to obtain a colloidal solution; drop an aqueous solution of triethylene glycol phosphoamine salt into the colloidal solution to obtain a green flame retardant finishing solution.

[0041] In the present invention, in the colloidal solution, the molar volume ratio of 3 - aminopropyltriethoxysilane to water is preferably 4×10 -4 ~5×10 -4 mol: 1 mL, more preferably 4.3×10 -4 ~4.7×10 -4 mol: 1 mL, and even more preferably 4.5×10 -4 mol: 1 mL; in the aqueous solution of triethylene glycol phosphoamine salt, the molar volume ratio of triethylene glycol phosphoamine salt to water is preferably 9×10 -4 ~1.5×10 -3 mol: 1 mL, more preferably 1×10 -3 ~1.3×10 -3 mol: 1 mL, and even more preferably 1.1×10 -3 ~1.2×10 -3 mol: 1 mL.

[0042] In the present invention, the volume ratio of the aqueous solution of triethylene glycol ammonium phosphate to the colloidal solution is preferably 2.5 to 3.5:1, more preferably 2.8 to 3.2:1, and still more preferably 3:1; the mixing time is preferably ≥12 h, more preferably ≥14 h.

[0043] The present invention also provides a green flame retardant finishing solution prepared by the method for preparing a green flame retardant finishing solution using the triethylene glycol ammonium phosphate flame retardant.

[0044] The present invention also provides the application of the green flame retardant finishing solution in suede-like fabrics. After impregnating the suede-like fabric in the green flame retardant finishing solution, it is successively cured, washed, and dried to obtain a flame retardant suede-like fabric.

[0045] In the present invention, the impregnation time is preferably 5 to 8 min, more preferably 6 to 7 min; the curing temperature is preferably 145 to 155 °C, more preferably 147 to 152 °C, and still more preferably 149 to 150 °C; the curing time is preferably 10 to 15 min, more preferably 11 to 14 min, and still more preferably 12 to 13 min; the drying temperature is preferably 75 to 85 °C, more preferably 78 to 82 °C, and still more preferably 80 °C; the drying time is preferably 3 to 4 h, more preferably 3.2 to 3.7 h, and still more preferably 3.5 h.

[0046] In the present invention, before impregnation, the green flame retardant finishing solution is preferably stirred at 75 to 85 °C, more preferably 78 to 82 °C, and still more preferably 80 °C; the stirring time is preferably ≥3 h, more preferably ≥4 h; after impregnation, the fabric liquor pickup rate is controlled to be 125 to 135% and then cured, more preferably 128 to 132%, and still more preferably 130%.

[0047] The schematic diagram of the effect of the green flame retardant finishing solution of the present invention on the suede-like fabric is as Figure 1 shown.

[0048] The technical solutions provided by the present invention will be described in detail below in conjunction with the embodiments, but they should not be construed as limiting the protection scope of the present invention.

[0049] Example 1

[0050] 15 g (0.1 mol) of triethylene glycol was added dropwise to a 250 mL round-bottom flask, and then 19.6 g (0.2 mol) of phosphoric acid crystals were added. The flask was placed in a constant-temperature oil bath and heated with stirring at 140 °C for 3 h to obtain a brown viscous solution. 24 g (0.4 mol) of urea was dissolved in 20 mL of deionized water and added dropwise to the brown viscous solution at a rate of 10 mL / min. The temperature was raised to 170 °C and stirred at a speed of 500 r / min in a constant-temperature oil bath for 2 h. After the reaction was completed, it was cooled to room temperature to obtain a brown viscous product (triethylene glycol phosphate amine salt flame retardant).

[0051] 3-Aminopropyltriethoxysilane was added to deionized water (the molar volume ratio of 3-aminopropyltriethoxysilane to deionized water was 4.5×10 -4 mol: 1 mL), and magnetically stirred for 12 h to obtain 60 mL of a colorless transparent colloidal solution; triethylene glycol phosphate amine salt was dissolved in deionized water (the molar volume ratio of triethylene glycol phosphate amine salt to deionized water was 1.1×10 -3 mol: 1 mL) to obtain 200 mL of a triethylene glycol phosphate amine salt solution. The colloidal solution was dropped into the triethylene glycol phosphate amine salt solution to obtain a green flame retardant finishing solution.

[0052] The green flame retardant finishing solution was heated to 80 °C and stirred at a speed of 500 r / min for 3 h. A 10 cm×10 cm suede-like fabric was placed into the finishing solution, fully impregnated for 5 min, and the suede-like fabric was taken out, controlling the liquor pick-up rate to be 130%; then it was placed in an oven and cured at 150 °C for 10 min. Then the suede-like fabric was washed in clean water and dried on a dryer at 80 °C for 3.5 h to obtain a flame retardant suede-like fabric.

[0053] The Fourier transform infrared spectrum of the triethylene glycol phosphate amine salt flame retardant in Example 1 is as Figure 2 shown. It can be seen from Figure 2 that the absorption peaks of triethylene glycol phosphate amine salt are located at 3214 cm -1 and 2893 cm -1 , which are respectively attributed to the chemical vibration absorption peaks of NH 4 + ions and CH 2 bonds in the structure; an additional absorption peak was detected at 1178 cm -1 , which is attributed to the P=O bond; meanwhile, the stretching vibration of the P-O bond was observed at 1093 cm -1 . All these prove the accuracy of the chemical structure of the triethylene glycol phosphate amine salt flame retardant, and further prove the successful synthesis of the flame retardant.

[0054] Example 2

[0055] 30 g (0.2 mol) of triethylene glycol was added dropwise to a 250 mL round-bottom flask, and then 39.2 g (0.4 mol) of phosphoric acid crystals were added. The flask was placed in a constant-temperature oil bath and heated with stirring at 140 °C for 3 h to obtain a brown viscous solution. 48 g (0.8 mol) of urea was dissolved in 40 mL of deionized water and added dropwise to the brown viscous solution at a rate of 10 mL / min. The temperature was raised to 170 °C, and it was stirred at a speed of 500 r / min in the constant-temperature oil bath for 2 h. After the reaction was completed, it was cooled to room temperature to obtain a brown viscous product (triethylene glycol phosphate amine salt flame retardant).

[0056] 3-aminopropyltriethoxysilane was added to deionized water (the molar volume ratio of 3-aminopropyltriethoxysilane to deionized water was 4.7×10 -4 mol: 1 mL), and magnetically stirred for 13 h to obtain a 120 mL colorless transparent colloidal solution; triethylene glycol phosphate amine salt was dissolved in deionized water (the molar volume ratio of triethylene glycol phosphate amine salt to deionized water was 1×10 -3 mol: 1 mL) to obtain a 400 mL triethylene glycol phosphate amine salt solution. The colloidal solution was dropped into the triethylene glycol phosphate amine salt solution to obtain a green flame retardant finishing solution.

[0057] The green flame retardant finishing solution was heated to 80 °C and stirred at a speed of 500 r / min for 3 h. A 10 cm×10 cm suede-like fabric was placed into the finishing solution, fully impregnated for 5 min, and the suede-like fabric was taken out, controlling the liquor pickup rate to be 130%; then it was placed in a vacuum oven and cured at 150 °C for 10 min. Then the suede-like fabric was washed in clean water and dried on a dryer at 80 °C for 3 h to obtain a flame retardant suede-like fabric.

[0058] Example 3

[0059] 45 g (0.3 mol) of triethylene glycol was added dropwise to a 250 mL round-bottom flask, and then 58.8 g (0.6 mol) of phosphoric acid crystals were added. The flask was placed in a constant-temperature oil bath and heated with stirring at 140 °C for 3 h to obtain a brown viscous solution. 72 g (1.2 mol) of urea was dissolved in 60 mL of deionized water and added dropwise to the brown viscous solution at a rate of 10 mL / min. The temperature was raised to 170 °C, and it was stirred at a speed of 500 r / min in the constant-temperature oil bath for 2 h. After the reaction was completed, it was cooled to room temperature to obtain a brown viscous product (triethylene glycol phosphate amine salt flame retardant).

[0060] 3-aminopropyltriethoxysilane was added to deionized water (the molar volume ratio of 3-aminopropyltriethoxysilane to deionized water was 4.3×10 -4mol: 1 mL), stir magnetically for 14 h to obtain a 120 mL colorless and transparent colloidal solution; Triethylene glycol phosphonium amine salt is dissolved in deionized water (the molar volume ratio of triethylene glycol phosphonium amine salt to deionized water is 1.4×10 -3 mol: 1 mL) to obtain a 400 mL triethylene glycol phosphonium amine salt solution. The colloidal solution is dropped into the triethylene glycol phosphonium amine salt solution to obtain a green flame retardant finishing solution.

[0061] The green flame retardant finishing solution is heated to 80 °C and stirred at a speed of 500 r / min for 3 h. A 10 cm×10 cm suede-like fabric is placed into the finishing solution, fully impregnated for 5 min, and the suede-like fabric is taken out, controlling the liquor pickup rate to be 130%; then it is placed in a vacuum oven and cured at 150 °C for 10 min, and then the suede-like fabric is washed in clean water and dried on a dryer at 80 °C for 4 h to obtain a flame retardant suede-like fabric.

[0062] Comparative Example 1

[0063] Change the molar volume ratio of triethylene glycol phosphonium amine salt to deionized water in Example 1 to 1.4×10 -4 mol: 1 mL, and other conditions are the same as those in Example 1.

[0064] Comparative Example 2

[0065] Change the molar volume ratio of triethylene glycol phosphonium amine salt to deionized water in Example 1 to 3.2×10 -4 mol: 1 mL, and other conditions are the same as those in Example 1.

[0066] Comparative Example 3

[0067] Change the molar volume ratio of triethylene glycol phosphonium amine salt to deionized water in Example 1 to 6.6×10 -4 mol: 1 mL, and other conditions are the same as those in Example 1.

[0068] Perform performance tests on the flame retardant suede-like fabrics of Examples 1 to 3 and Comparative Examples 1 to 3. Use a limiting oxygen index tester and a cone calorimeter to test the flame retardant suede-like fabrics prepared in Examples 1 to 3 and Comparative Examples 1 to 3, and observe the changes in the limiting oxygen index value, heat release rate, and total heat release of the fabrics.

[0069] The test results of the limiting oxygen index of the flame retardant suede-like fabrics prepared in Examples 1 to 3 and Comparative Examples 1 to 3 are as Figure 3 shown. The results show that the limiting oxygen index value of the suede-like fabric finished with the flame retardant finishing solution of the present invention is about 35, indicating that the flame retardant finishing solution has a good flame retardant effect on the fabric. With the increase in the number of washing times, the flame retardancy of the fabric gradually decreases.

[0070] The peak heat release and total heat release of the flame-retardant suede-like fabrics prepared in Examples 1 to 3 and Comparative Examples 1 to 3 are as follows Figure 4 shown. The peak heat release and total heat release are important indicators for judging the flame retardancy of fabrics. The peak heat release reflects the severity of the fire development and the rapidity of energy release during combustion. For fabrics with good flame retardancy, the combustion reaction is inhibited, and the peak heat release is low; otherwise, it is high. The total heat release reflects the total amount of energy released during the entire combustion process. For flame-retardant fabrics, due to flame retardants or their own structures, the decomposition and combustion of combustible substances are restricted, and the total heat release is reduced. Fabrics without flame retardant properties have a high total heat release. From Figure 4 it can be seen that there is a basically positive correlation trend between the peak heat release and the total heat release in both the examples and the comparative examples. The peak heat release and total heat release of the flame-retardant suede-like fabrics prepared in Examples 1 to 3 prove that the fabrics have good flame retardancy. It can be seen from the bar chart that as the concentration of triethylene glycol phosphate amine salt increases, the peak heat release and total heat release of the fabric gradually decrease, indicating that the concentration of the flame retardant has a significant impact on the flame retardancy. When the concentration increases, the peak heat release decreases because the flame retardant decomposes to produce non-combustible gases and forms a barrier layer to slow down combustion; the total heat release decreases by taking away heat and promoting carbonization to reduce the consumption of combustible components. In addition, the peak heat release and total heat release of the fabrics in the comparative examples are higher than those of the fabrics in Examples 1 to 3, indicating that the flame retardancy of the fabrics in the examples is better than that of the fabrics in the comparative examples.

[0071] The above is only the preferred embodiment of the present invention. It should be noted that for those of ordinary skill in the art, without departing from the principle of the present invention, several improvements and refinements can be made, and these improvements and refinements should also be regarded as the protection scope of the present invention.

Claims

1. A method for preparing a flame retardant finishing liquid using a triethylene glycol amine phosphate flame retardant, characterized in that: The following steps are included: 3-aminopropyltriethoxysilane and water are mixed to obtain a colloidal solution; an aqueous solution of triethylene glycol amine phosphate is dripped into the colloidal solution to obtain a flame retardant finishing solution; The preparation method of triethylene glycol amine phosphate flame retardant comprises the following steps: 1) Triethylene glycol and phosphoric acid are mixed and reacted to obtain a viscous solution; 2) dropping the urea solution into the viscous solution to react and obtain a triethylene glycol amine phosphate flame retardant; The molar ratio of urea in triethylene glycol, phosphoric acid and urea solution is 1:1.8~2.2:3~5; in urea solution, the molar volume ratio of urea to water is 1.5×10 -2 ~2.5×10 -2 mol: 1mL; The reaction temperature of step 1) is 135-145°C, and the reaction time is 2.5-3.5h; the reaction temperature of step 2) is 165-175°C, and the reaction time is 1.8-2.2h.

2. The method for preparing a flame retardant finishing liquid using the triethylene glycol amine phosphate flame retardant according to claim 1, characterized in that: In the colloidal solution, the molar volume ratio of 3-aminopropyltriethoxysilane to water is 4×10 -4 ~5×10 -4 mol: 1mL; in the aqueous solution of triethylene glycol amine phosphate, the molar volume ratio of triethylene glycol amine phosphate and water is 9×10 -4 ~1.5×10 -3 mol:1mL.

3. The method for preparing a flame retardant finishing liquid using the triethylene glycol amine phosphate flame retardant according to claim 1 or 2, characterized in that: The volume ratio of the aqueous solution of triethylene glycol amine phosphate to the colloidal solution is 2.5-3.5:1; and the mixing time is ≥12h.

4. The flame retardant finishing liquid prepared by the method for preparing a flame retardant finishing liquid using the triethylene glycol amine phosphate flame retardant according to any one of claims 1 to 3.

5. The use of the flame retardant finishing liquid according to claim 4 in suede-like fabrics, characterized in that: The suede-like fabric is immersed in a flame retardant finishing liquid, and then cured, washed, and dried in sequence to obtain a flame retardant suede-like fabric; The dipping time is 5-8 minutes, the curing temperature is 145-155°C, the curing time is 10-15 minutes, the drying temperature is 75-85°C, and the drying time is 3-4 hours; Before impregnation, the flame retardant finishing liquid is stirred at 75~85℃ for ≥3h; After impregnation, the liquid loading rate of the fabric is controlled to be 125~135% before curing.

Citation Information

Patent Citations

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