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Hyperbranched ionic liquid based on HCCP and application of hyperbranched ionic liquid as fire retardant

A technology of hexachlorocyclotriphosphazene and ionic liquid, which is applied in the field of hyperbranched ionic liquid flame retardants, can solve problems such as no research reports on HCCP grafted ionic liquid, and achieves simple process, easy control, and low equipment requirements. Effect

Active Publication Date: 2015-04-29
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there have been no research reports on the use of HCCP grafted ionic liquids in the field of flame retardancy.

Method used

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  • Hyperbranched ionic liquid based on HCCP and application of hyperbranched ionic liquid as fire retardant
  • Hyperbranched ionic liquid based on HCCP and application of hyperbranched ionic liquid as fire retardant
  • Hyperbranched ionic liquid based on HCCP and application of hyperbranched ionic liquid as fire retardant

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Dissolve 3.47 g of HCCP in 50 ml of acetonitrile, then add 9.93 g of N-butylimidazole (nBuMI) and 0.3 g of potassium iodide (KI), stir the reaction at 40°C for 2 hours, filter and dry the filter cake to obtain 10.09 g of N 3 P 3 (C 7 H 12 N 2 ) 6 Cl 6 , Abbreviated as HCCP-[nBuMI]Cl, the yield is 92.3%.

[0053] Dissolve 5 g of HCCP-[nBuMI]Cl in 20 ml of deionized water, and add 6.73 g of potassium hexafluorophosphate (KPF 6 ) And react at 20-30°C for 24 hours. After the reaction, the reactants are poured into 80 ml methanol to precipitate the product. The resulting mixture is suction filtered and the filter cake is vacuum dried to obtain 6.82 g of HCCP-based hyperbranched ionic liquid. N 3 P 3 (C 7 H 12 N 2 ) 6 (PF 6 ) 6 , Marked as HCCP-[nBuMI]PF 6， The yield was 85.2%.

[0054] HCCP-[nBuMI]PF prepared 6 of 1 H NMR see attached figure 1 As shown, see the attached infrared spectrum figure 2 Shown.

[0055] Take 2.5 grams of HCCP-[nBuMI]PF 6 And 47.5 grams of GPPS were prep...

Embodiment 2

[0058] Dissolve 3.47 g of HCCP in 50 ml of acetonitrile, then add 6.57 g of N-methylimidazole (nMeMI) and 0.2 g of sodium iodide (NaI), stir the reaction at 40°C for 2 hours, filter and dry the filter cake to obtain 7.99 g of N 3 P 3 (C 4 H 6 N 2 ) 6 Cl 6 , Abbreviated as HCCP-[nMeMI]Cl, the yield is 95.1%.

[0059] Dissolve 5 grams of HCCP-[nMeMI]Cl in 20ml of deionized water, then add 6.73 grams of potassium hexafluorophosphate (KPF 6 ) And react at 20-30°C for 24 hours. After the reaction, the reactants are poured into 80 ml methanol to precipitate the product. The resulting mixture is suction filtered and the filter cake is vacuum dried to obtain 7.55 g of HCCP-based hyperbranched ionic liquid. N 3 P 3 (C 4 H 6 N 2 ) 6 (PF 6 ) 6 , Marked as HCCP-[nMeMI]PF 6， The yield was 84.7%.

[0060] Take 2.5 grams of HCCP-[nMeMI]PF 6 And 47.5 grams of GPPS were prepared with a micro extruder and a micro injection machine at 200°C, and the limiting oxygen index was tested to be 27.9%.

[0061...

Embodiment 3

[0063] Dissolve 3.47 g of HCCP in 50 ml of acetonitrile, then add 8.10 g of triethylamine (TEA) and 0.3 g of potassium iodide (KI), stir the reaction at 40°C for 2 hours, filter and dry the filter cake to obtain 8.52 g of N 3 P 3 (C 6 H 15 N) 6 Cl 6 , Abbreviated as HCCP-[TEA]Cl, the yield is 89.2%.

[0064] Take 6 grams of HCCP-[TEA]Cl dissolved in 20ml of deionized water, and then add 10.82 grams of lithium bis(trifluoromethanesulfonyl)imide (LiNTF 2 ) And react at 20~30℃ for 24 hours. After the reaction, the reactants are poured into 80 ml of ethanol to precipitate the product. The resulting mixture is suction filtered and the filter cake is vacuum dried to obtain 5.8 g of HCCP-based hyperbranched ionic liquid. N 3 P 3 (C 6 H 15 N) 6 (N(SO 2 CF 3 ) 2 ) 6 , Abbreviated as HCCP-[TEA][NTF 2 ], the yield is 51.2%.

[0065] Take 2.5 grams of HCCP-[TEA][NTF 2 ] And 47.5 grams of GPPS were prepared with a micro extruder and a micro injection machine at 200°C, and the limiting oxygen ind...

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Abstract

The invention provides a method for synthesizing a hyperbranched ionic liquid fire retardant based on HCCP. According to the method, HCCP reacts with trialkylamin, trialkyl phosphorus, and N-alkyl imidazole to realize ionization, salts such as sodium tetrafluoroborate, potassium hexafluorophosphate and bistrifluoromethanesulfonimide lithium, which contain different anions, are used for ion exchange, so that a hyperbranched ionic liquid fire retardant containing different anions is obtained, and synergistic flame retardance of HCCP and the ionic liquid is realized. The synthesized hyperbranched ionic liquid based on HCCP can be used as the fire retardant in various polymers.

Description

(1) Technical field [0001] The invention relates to a hyperbranched ionic liquid flame retardant based on hexachlorocyclotriphosphazene and a preparation method and application thereof. (2) Background technology [0002] With the rapid development of modern society, polymer materials have become more and more widely used in human life. However, most polymer materials have the disadvantages of being flammable and easy to produce toxic gases, which poses a huge threat and harm to people's lives. At present, the effective method to improve the flame retardant performance of polymer materials is to add flame retardants. Commonly used flame retardants mainly include halogen and non-halogen flame retardants. The addition amount of halogen flame retardants is small, the flame retardant effect is remarkable, and the cost performance High, has little effect on the performance of polymer substrates. However, it generates a large amount of smoke and corrosive toxic gas when it burns, posi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6593C08K5/5399C08L23/12C08L23/06C08L25/06
Inventor 杨晋涛何志才郑炯洲羊银钟明强
Owner ZHEJIANG UNIV OF TECH
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