N-P flameresistant material and preparation method thereof and application in textiles

A flame retardant material and reaction technology, which is applied in the field of flame retardant material preparation, can solve the problems of low carbon formation rate and poor thermal stability, and achieve the effects of high carbon formation rate, controllable reaction and high limiting oxygen index

Active Publication Date: 2016-02-24
HUNAN INSTITUTE OF ENGINEERING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Most of the currently developed N-P flame retardants are complex. The P in this type of system mainly comes from ammonium phosphate, ammonium polyphosphate, phosphate, etc., and the N comes from various nitrogen or amine compounds, such as urea. , dicy

Method used

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  • N-P flameresistant material and preparation method thereof and application in textiles
  • N-P flameresistant material and preparation method thereof and application in textiles
  • N-P flameresistant material and preparation method thereof and application in textiles

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Synthesis of Hexachlorocyclotriphosphazene (HCPP)

[0048]In a 250mL three-neck flask with a constant pressure dropping funnel and a magnetic stirring device, add 16.0g of finely ground ammonium chloride and 120mL of chlorobenzene in sequence; then weigh 34.0g of phosphorus pentachloride in a 100mL beaker, and add 80mL Chlorobenzene, heating, stirring evenly, after phosphorus pentachloride is completely dissolved in chlorobenzene, quickly transfer to a constant pressure funnel, and take insulation measures to prevent phosphorus pentachloride from chlorobenzene solution precipitation. Turn on the heating device under the protection of nitrogen, and when the temperature of the solution in the three-necked flask reaches 120-130°C, start to add the chlorobenzene solution of phosphorus pentachloride dropwise at a uniform speed, and the dropping time should be controlled at about 2.5 hours. , reacted for about 2-3h, stopped heating, cooled, suction filtered, and rotary evapor...

Embodiment 2

[0050] Synthesis of 1-Oxyphospha-4-hydroxymethyl-2,6,7-trioxabicyclo[2.2.2]octane (PEPA)

[0051] Add 44.8g of pentaerythritol and 130mL of 1,4-dioxane into a three-necked flask with a constant pressure dropping funnel and a tail gas receiving device, and then measure 33.6mL of POCl 3 Add 40mL of 1,4 dioxane to the constant pressure funnel and heat it. When the temperature reaches 85°C, start to add phosphorus oxychloride dropwise. It takes about 2.5 hours for the dropwise addition to be completed. React for 2-3h, then heat up to reflux state, react for about 2-4h, filter with suction, recrystallize to get white needle-like crystal PEPA, the yield is 88%, M.P.209.5-212.3°C, IR (KBr, cm-1 ): 869, 987, 1226, 1299, 2959, 3391; 1 HNMR (400MHZ, CDCl3, TMS, δppm): 5.09 (d, 1H), 4.58 (m, 6H), 3.28 (d, 1H).

Embodiment 3

[0053] Synthesis of N-P Flame Retardant Material (HCPPA)

[0054] Weigh 10.8g of PEPA and an appropriate amount of NaH in a three-necked flask, measure 60mL of acetonitrile solution into the three-necked flask, and add an equimolar amount of pyridine to the three-necked flask, heat to 60°C, and mechanically stir Pour 3.3g of hexachlorocyclotriphosphazene into a three-necked flask, react at reflux temperature for 1-3 hours, wash twice with water, then wash once with absolute ethanol, and dry in a constant temperature oven at 60-80°C. A white powdery solid HCPPA was obtained with a yield of 66.2%. M.P. 265-268°C. Its infrared spectrum is as Figure 4 As shown, the H NMR spectrum is shown as Figure 5 Shown; IR(KBr,cm -1 ): 853, 1033, 1191, 1261, 1317, 1480, 2971, 2911; 1 HNMR (400MHZ, DMSO, TMS, δppm): 3.42 (d, 6H), 4.65 (m, 36H).

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Abstract

The invention discloses an N-P flameresistant material and a preparation method thereof and application in textiles. The chemical name of a flame retardant of the material is hexa(1-oxo-phospha-2,6,7-trioxabicyclo[2,2,2]octane-4-methylenedioxy)cyclotriphosphazene (HCPPA); the preparation method of the material comprises the steps of synthesizing hexachlorocyclotriphosphazene (HCPP) by reacting ammonium chloride with phosphorus pentachloride, wherein a catalyst is pyridine and ZnO; then synthesizing 1-oxo-phospha-4-hydroxymethyl-2,6,7-trioxabicyclo[2,2,2]octane (PEPA) by reacting pentaerythritol with phosphorus oxychloride; finally synthesizing the HCPPA by reacting the HCPP with the PEPA. According to the preparation method, NaH is used as a catalyst, so that the synthesis reactions can be performed quickly, the reaction time is greatly shortened, and the product yield is improved. When the N-P flame retardant is used for retarding a flame of a cotton fabric, high limit oxygen index and char yield are achieved, and the wash durability is good.

Description

technical field [0001] The invention relates to the technical field of preparation of flame retardant materials, in particular to the preparation of a class of novel N-P flame retardant materials based on phosphazene rings and double cage structures and their application in the field of textiles, especially cotton textiles. Background technique [0002] The fire caused by the flammability of textile fiber products has become one of the major social disasters, seriously threatening people's lives, property and safety. Therefore, countries all over the world attach great importance to the flame retardant research of fibers and textiles. Today, although the research on flame retardants has made great progress, with the deepening of environmental protection and the continuous improvement of people's ideology, the textile industry has higher and higher requirements for flame retardants, which are highly efficient, green and environmentally friendly. , Environmental protection ha...

Claims

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Application Information

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IPC IPC(8): C07F9/6593D06M13/44
CPCC07F9/65815D06M13/44D06M2101/06D06M2200/30
Inventor 邓继勇董新理
Owner HUNAN INSTITUTE OF ENGINEERING
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