Journal of Textile Research ›› 2025, Vol. 46 ›› Issue (02): 180-187.doi: 10.13475/j.fzxb.20240902401

• Dyeing and Finishing Engineering • Previous Articles     Next Articles

Modification of cotton fabric by in-situ deposition of phosphorus/nitrogen flame retardants for durable flame retardancy

ZHANG Jie1,2, GUO Xinyuan1,2, GUAN Jinping1,2(), CHENG Xianwei1,2, CHEN Guoqiang1,2   

  1. 1. College of Textile and Clothing Engineering, Soochow University, Suzhou, Jiangsu 215021, China
    2. Key Laboratory of Flame Retardancy Finishing of Textile Materials (CNTAC), Soochow University, Suzhou, Jiangsu 215021, China
  • Received:2024-09-29 Revised:2024-10-31 Online:2025-02-15 Published:2025-03-04
  • Contact: GUAN Jinping E-mail:guanjinping@suda.edu.cn

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Abstract:

Objective Cotton fabrics are known for their softness, wearing comfort, moisture absorption and breathability, and are widely used in clothing, decoration, construction and other fields. However, cotton fabrics would burn rapidly and the burning is accompanied by obvious phenomena of secondary ignition and shadow ignition, which needs improving for the fire safety of cotton fabrics. Proban technology is known to offer flame retardant durability, low cost and minimal impact on mechanical properties to cotton fabrics, but it is limited by the complex ammonia fumigation process, which largely restricts its application.

Method Different concentrations of tetrakis(hydroxymethyl)phosphonium sulfate (THPS), dicyandiamide (DCD), and cyclic phosphate ester flame-retardant FRC-1 were used to prepare the solution at 80 ℃ oscillation for 10 min. The cotton fabrics were immersed in the solution for impregnation for 10 min, followed by two further immersion and two rolling processes. The rolling rate was 100%, and the fabric was then dried at 80 ℃ for 3 min, then baked at 150 ℃ for 3 min. THPS was used to form amine macromolecules with anionic FRC-1 electrostatic interaction, aiming to form more complex condensation products within the fibers. The complex condensation products were formed within the fiber to enable the cotton fabrics with efficient and durable flame-retardant properties.

Results Experiment showed that the cotton fabric burned fiercely with obvious continuation of combustion and the phenomenon of negative combustion. The length of damage was 30 cm, and the LOI value was only 18.6%. After the flame-retardant finishing, the flame retardancy of the modified cotton fabric was improved, and the flame was self-extinguished within 6 s, and the length of damage was reduced to 7.5 cm, and the LOI reached 29.7%, when the concentration of FRC-1 was 80 g/L and the concentration of THPS was 100 g/L. The modified cotton fabric exhibited good self-extinguishing performance after 50 times of home washing, when the destruction length was 11.0 cm, and the LOI was 26.4%. These still satisfy the performance requirements for grade B1 according to GB/T 17591—2006 Flame-retardant Fabrics. The heat release rate and total heat release of the modified cotton fabrics were greatly reduced, indicating that the flame-retardant coating obviously inhibited the heat release performance of cotton fabrics, and the fire hazard of modified cotton fabrics was reduced. The early decomposition of phosphorus-containing compound in the heating process promoted dehydration and charring of cotton fabrics. The modified fabrics showed high thermal stability with the formation of more residual carbon under high-temperature conditions, leaving a char layer with high degree of graphitization, effectively isolating oxygen and heat. In the combustion process, a large number of non-combustible volatile substances were produced, diluting the concentration of flammable gases, and the quenching effect of the phosphorus radical was also beneficial for improving flame retardancy. It is evident that the phosphorus-containing flame-retardant groups in the polycondensation products played a flame-retardant role in the solid phase and gas phase. The physical properties of the modified cotton fabrics did not change significantly and did not affect their subsequent use.

Conclusion The condensation product of tetrakis(hydroxymethyl)phosphine sulphate, dicyandiamide and the cyclic phosphate ester FRC-1 shows a high level of flame retardancy on cotton fabrics. Even after 50 home washing cycles, the modified cotton fabrics were able to pass the vertical flame test and meet the requirements of Class B1. Thermal analysis, thermogravimetric infrared analysis, cone calorimetry, carbon residue analysis and physical property analysis showed that the phosphorus-containing polycondensates effectively improved the flame retardancy of the modified cotton fabrics through the mechanism of solid-phase and gas-phase flame retardancy. In conclusion, phosphorus-containing polycondensates have a great potential to be used as a sustainable and effective flame-retardant method for modified cotton fabrics.

Key words: cotton fabric, flame retardancy, washing durability, nitrogen/phosphorus flame retardant, flame reardamts fabric, functional textile

CLC Number: 

  • TS156

Fig.1

Photograph of insoluble white precipitate"

Fig.2

FT-IR spectra of cotton fabrics"

Fig.3

Flame retardant durability of modified cotton fabrics. (a) Combustion process of cotton fabrics and modified cotton fabrics in vertical combustion tests; (b) Flame retardant properties of modified cotton fabrics at different THPS concentrations; (c) Flame retardant properties of modified cotton fabrics under different washing times"

Fig.4

Thermal stability performance of modified cotton fabrics. (a) HRR curves; (b) THR curves"

Fig.5

TG and DTG curves of cotton fabrics under nitrogen and air atmospheres. (a) TG curve under nitrogen; (b) DTG curve under nitrogen; (c) TG curve in air; (d) DTG curve in air"

Tab.1

Thermal degradation data of coated cotton"

气体
氛围		 织物 T5% /
℃		 Tmax1/
℃		 Tmax2/
℃		 700 ℃时的
残炭量/%
氮气 棉织物 234 360 — 7.80
改性棉织物 223 305 — 39.00
空气 棉织物 229 350 451 0.15
改性棉织物 222 299 500 15.80

Fig.6

TG-IR spectra of cotton fabrics(a)and modified cotton fabrics(b)in a nitrogen environment"

Fig.7

Digital photos of cotton fabrics calcined at different calcination temperatures. (a) Cotton fabrics; (b) Modified cotton fabrics"

Fig.8

FT-IR spectra of char residues of cotton fabrics(a)and modified cotton fabrics(b)calcined at various temperatures"

Fig.9

Raman spectra of char residues of cotton fabrics (a) and modified cotton fabrics(b) calcined at 500 ℃"

Tab.2

Physical and mechanical properties of cotton fabrics"

织物 断裂强力/N 断裂伸长率/% 白度/%
原棉织物 256.9±6.6 4.60±0.17 88.8±0.3
改性棉织物 254.7±9.6 4.46±0.20 88.4±1.5
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