News Details
Phosphate flame retardant
2017-10-19 12:04:07
Phosphate flame retardant
A novel phosphate flame retardant was prepared with phosphoric acid and ethylene glycol, and the structural characterization was carried out. Using the synthesis of phosphate ester flame retardant flame retardant finishing of cotton fabrics, by Yang combustion agent dosage, the dosage of crosslinking agent, curing, "and the discussion of the baking temperature, between the optimized finishing technology of: flame retardant 300 g/L, crosslinking agent, 80 g/L, 170 ℃ baking 2 min. Flame retardant properties of the treated fabric and thermal analysis show that the cracking of the treated fabric significantly lower temperature, residue increased considerably, flame retardant performance is excellent, B1 level standard, can well meet the requirements of the fabric of Yang combustion.
In recent years, the fire caused by textile has increased year by year, and the world countries have issued the regulations on the burning of textiles, making the development of textile flame retardant finishing agents and finishing new technologies become hot spots. At present, the main flame retardant finishing agent for cotton fabric are four hydroxymethyl phosphonic chloride series (THPC and THPN), ten pbdes, n hydroxymethyl series, the flame retardant toxic carcinogens or formaldehyde in use process, endanger human body health.
Future flame retardants will be developed in the direction of non-formaldehyde environmental protection, and the new type of phosphate flame retardant conforms to this trend. Because of the low quality, low boiling point, poor heat resistance and easy distribution to the air middle of the air. A new type of flame retardant of phosphate ester was prepared by the preparation of phosphoric acid and ethylene glycol.
Raw materials: phosphoric acid, ethylene glycol, concentrated sulfuric acid, crosslinking agent butane tetracarboxylic acid (BTCA), sodium hypophosphite (all analyzed pure, market); Pretreated cotton plain cloth (220~272 root / 10cm).
Instruments: LCK 08 fabric flame retardant performance tester, LCK a 09 automatic oxygen index apparatus, TG7 thermogravimetric analyzer, HD026N type electronic fabrics strength tester, Bluke600MHz nuclear magnetic resonance instrument, model 2695 gel chromatography, the American type NicoletNexus670 MHz, IR spectrometer.
Synthesis process: 0. 3 moles of glycol are added to the four flask with a stirring rod and thermometer. Stir to add 0. 25 moles of phosphoric acid, a small amount of catalyst concentrated sulfuric acid. Up to 150 ℃, thermal response 4. 5h, colorless transparent microviscous liquid, reduced pressure distillation to remove excess glycol, instant flame retardant.
The structural characterization of flame retardants: FT - IR test conditions: resolution 8cm-1 scanning 64 times; Test mode: attenuated total reflection (ATR). H -- NMR test instrument: liquid nuclear magnetic resonance instrument; Solvent: deuterium chloroform, deuterium water; Sample tube: 5mm nuclear magnetic resonance tube.
Triethyl phosphate (TEP)
Triethyl phosphate(Flame retardants TEP) is mainly used as the high boiling point solvents,catalysts, plasticizers, flame retardants, ethylating agent, and organic peroxide stabilizer. And Triethyl phosphate(TEP) is widely used in medicine, pesticides, vinyl ketone, resins, hydraulic oil and other production areas. In Japan, 70% of this product is used in catalyst.
Flame retardant gel chromatography instrument: gel chromatograph; Test condition: Uhrahydrogel a 1000 + 2000 type double column in series, column temperature 30 ℃, 50 tendency for mobile phase LNaNO3, velocity of 0. 6mL/min, the sample volume is 50uL_
Flame retardant finishing process: compound finishing liquid first dip no.2 rolling (flame retardants in moderation, and crosslinking agent amount, catalyst 48 g/L sodium phosphite, rolling rate of more than 85%, dipping time is 2 min) a preliminary drying (90 ℃, 4 min) curing.
Performance testing of flame retardant fabrics. Flame-retardant performance: according to GB/T5455-1997 (vertical method of textile combustion performance test) and GB/t5454-1997 (test oxygen index method for textile combustion performance); Thermal analysis test conditions: nitrogen atmosphere, the carrier gas velocity of 20 ml/min, 15 ℃ / min heating rate, temperature range 4 o ~ 700 ℃ : strong: according to GB/T3923. 1 -- 1997 (part 1 of tensile properties of textile fabrics: test of the method of determination of breaking strength and elongation of elongation).
3320. 30cm-1 is a telescopic vibration peak of 1 0H, 2956. 29 cm - 1, 2882-1. 27cm-1 is a CH, a CH: anti-symmetric and symmetric telescopic vibration peak, 2445. 76cm-1 is P - H telescopic vibration peak, 1456. 32cm-1 is a plane shear vibration peak of a CH, 1180. 01cm-1 is a telescopic vibration peak of P - O, 1010. 84cm-1 is the telescopic vibration peak of P 1 0 1 C, 873. 39cm-1 is an external bending vibration peak of a c-h. The above characteristic peak is consistent with the target product.
With CDCL as solvent, test samples were exchanged by D2O, 9. 28, 2. At 74, two of the two ends of a 0H active hydrogen absorption peak disappeared, and in 6. The absorption peak of D2O is added at 05. The test results further illustrate that the synthetic flame retardant is the target product.
The dispersion of flame retardants is 1. 05l312, indicating that the molecular weight of flame retardants is equal to 1,250.
Copyright: Zhang Jia Gang YaRui Chemical co.,Ltd
http://www.yaruichem.com
A novel phosphate flame retardant was prepared with phosphoric acid and ethylene glycol, and the structural characterization was carried out. Using the synthesis of phosphate ester flame retardant flame retardant finishing of cotton fabrics, by Yang combustion agent dosage, the dosage of crosslinking agent, curing, "and the discussion of the baking temperature, between the optimized finishing technology of: flame retardant 300 g/L, crosslinking agent, 80 g/L, 170 ℃ baking 2 min. Flame retardant properties of the treated fabric and thermal analysis show that the cracking of the treated fabric significantly lower temperature, residue increased considerably, flame retardant performance is excellent, B1 level standard, can well meet the requirements of the fabric of Yang combustion.
In recent years, the fire caused by textile has increased year by year, and the world countries have issued the regulations on the burning of textiles, making the development of textile flame retardant finishing agents and finishing new technologies become hot spots. At present, the main flame retardant finishing agent for cotton fabric are four hydroxymethyl phosphonic chloride series (THPC and THPN), ten pbdes, n hydroxymethyl series, the flame retardant toxic carcinogens or formaldehyde in use process, endanger human body health.
Future flame retardants will be developed in the direction of non-formaldehyde environmental protection, and the new type of phosphate flame retardant conforms to this trend. Because of the low quality, low boiling point, poor heat resistance and easy distribution to the air middle of the air. A new type of flame retardant of phosphate ester was prepared by the preparation of phosphoric acid and ethylene glycol.
Raw materials: phosphoric acid, ethylene glycol, concentrated sulfuric acid, crosslinking agent butane tetracarboxylic acid (BTCA), sodium hypophosphite (all analyzed pure, market); Pretreated cotton plain cloth (220~272 root / 10cm).
Instruments: LCK 08 fabric flame retardant performance tester, LCK a 09 automatic oxygen index apparatus, TG7 thermogravimetric analyzer, HD026N type electronic fabrics strength tester, Bluke600MHz nuclear magnetic resonance instrument, model 2695 gel chromatography, the American type NicoletNexus670 MHz, IR spectrometer.
Synthesis process: 0. 3 moles of glycol are added to the four flask with a stirring rod and thermometer. Stir to add 0. 25 moles of phosphoric acid, a small amount of catalyst concentrated sulfuric acid. Up to 150 ℃, thermal response 4. 5h, colorless transparent microviscous liquid, reduced pressure distillation to remove excess glycol, instant flame retardant.
The structural characterization of flame retardants: FT - IR test conditions: resolution 8cm-1 scanning 64 times; Test mode: attenuated total reflection (ATR). H -- NMR test instrument: liquid nuclear magnetic resonance instrument; Solvent: deuterium chloroform, deuterium water; Sample tube: 5mm nuclear magnetic resonance tube.
Triethyl phosphate (TEP)
Triethyl phosphate(Flame retardants TEP) is mainly used as the high boiling point solvents,catalysts, plasticizers, flame retardants, ethylating agent, and organic peroxide stabilizer. And Triethyl phosphate(TEP) is widely used in medicine, pesticides, vinyl ketone, resins, hydraulic oil and other production areas. In Japan, 70% of this product is used in catalyst.
Flame retardant gel chromatography instrument: gel chromatograph; Test condition: Uhrahydrogel a 1000 + 2000 type double column in series, column temperature 30 ℃, 50 tendency for mobile phase LNaNO3, velocity of 0. 6mL/min, the sample volume is 50uL_
Flame retardant finishing process: compound finishing liquid first dip no.2 rolling (flame retardants in moderation, and crosslinking agent amount, catalyst 48 g/L sodium phosphite, rolling rate of more than 85%, dipping time is 2 min) a preliminary drying (90 ℃, 4 min) curing.
Performance testing of flame retardant fabrics. Flame-retardant performance: according to GB/T5455-1997 (vertical method of textile combustion performance test) and GB/t5454-1997 (test oxygen index method for textile combustion performance); Thermal analysis test conditions: nitrogen atmosphere, the carrier gas velocity of 20 ml/min, 15 ℃ / min heating rate, temperature range 4 o ~ 700 ℃ : strong: according to GB/T3923. 1 -- 1997 (part 1 of tensile properties of textile fabrics: test of the method of determination of breaking strength and elongation of elongation).
3320. 30cm-1 is a telescopic vibration peak of 1 0H, 2956. 29 cm - 1, 2882-1. 27cm-1 is a CH, a CH: anti-symmetric and symmetric telescopic vibration peak, 2445. 76cm-1 is P - H telescopic vibration peak, 1456. 32cm-1 is a plane shear vibration peak of a CH, 1180. 01cm-1 is a telescopic vibration peak of P - O, 1010. 84cm-1 is the telescopic vibration peak of P 1 0 1 C, 873. 39cm-1 is an external bending vibration peak of a c-h. The above characteristic peak is consistent with the target product.
With CDCL as solvent, test samples were exchanged by D2O, 9. 28, 2. At 74, two of the two ends of a 0H active hydrogen absorption peak disappeared, and in 6. The absorption peak of D2O is added at 05. The test results further illustrate that the synthetic flame retardant is the target product.
The dispersion of flame retardants is 1. 05l312, indicating that the molecular weight of flame retardants is equal to 1,250.
Copyright: Zhang Jia Gang YaRui Chemical co.,Ltd
http://www.yaruichem.com
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