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Ionic liquid-type phosphate fire retardant and preparation method thereof

A technology of phosphate esters and ionic liquids, which is applied in chemical instruments and methods, bulk chemical production, organic chemistry, etc., and can solve problems such as poor compatibility with polymer matrix, degradation of mechanical properties of materials, poor thermal stability, etc. problems, to achieve good application prospects, superior charcoal performance, and good compatibility

Active Publication Date: 2013-02-13
HEFEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when the IFR system is applied to flame retardant polymer materials, there are also problems such as relatively low flame retardant efficiency, poor compatibility with the polymer matrix, and poor thermal stability.
In order to make the flame retardant performance of the material pass the UL-94 V-0 test, its addition amount is usually more than 30wt%, which will lead to the deterioration of the mechanical properties of the material

Method used

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  • Ionic liquid-type phosphate fire retardant and preparation method thereof
  • Ionic liquid-type phosphate fire retardant and preparation method thereof
  • Ionic liquid-type phosphate fire retardant and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] 1. Equipped with magnetic stirring, reflux condenser, dropping funnel and N 2 Add 27.01g (0.15mol) of PEPA and 100mL of acetonitrile to a 500mL three-necked flask with a ball, start stirring, and the reaction temperature rises to 40°C, then slowly add 33.89g (0.30mol) of chloroacetyl chloride dropwise within 1h, and wait After the addition of chloroacetyl chloride, the temperature was raised to 80°C to continue the reaction for 24h. After the reaction, the solvent was evaporated under reduced pressure, and then washed with deionized water and dried in a vacuum oven at 70°C for 12h to obtain intermediate I. The yield 79%.

[0042] 2. Equipped with magnetic stirring, reflux condenser and N 2 Add 25.66g (0.15mol) of intermediate I, 9.85g (0.12mol) of 1-methylimidazole, and 100mL of acetonitrile into a 500mL three-neck flask with a ball, start stirring, heat up to 80°C for 24 hours, and filter after the reaction. The cake was washed with acetonitrile and dried in a vacuum...

Embodiment 2

[0046] 1. When equipped with N 2 In the 500mL flask of the ball, add 16.94g (0.05mol) anion as Cl - Ionic liquid phosphate flame retardant ([PCMIM]Cl), 6.59g (0.06mol) NaBF 4 and 100mL of acetonitrile, stirring and reacting at room temperature for 24h, filtering and concentrating the filtrate after the completion of the reaction, and drying in vacuum at 70°C for 12h to obtain the anion as BF 4 - The ionic liquid phosphate flame retardant (abbreviated as [PCMIM] BF 4 ), the structural formula is as follows:

[0047]

[0048] 2. Using ethanol as a solvent, the flame retardant [PCMIM]BF synthesized in step 1 4 Carry out wet compounding with APP at a mass ratio of 1:5, evaporate the solvent under reduced pressure, and dry in vacuum to obtain a composite flame retardant. Then the composite flame retardant is mixed with polypropylene (S1003) in an addition amount of 30wt% in a 175°C Huck torque rheometer at a speed of 30rpm for 10min to obtain a flame-retardant polypropylene...

Embodiment 3

[0050] 1. When equipped with N 2 In the 500mL flask of the ball, add 16.94g (0.05mol) anion as Cl - Ionic liquid phosphate flame retardant ([PCMIM]Cl), 11.04g (0.06mol) KPF 6 and 100mL of acetonitrile, stirring and reacting at room temperature for 24h, filtering and concentrating the filtrate after the reaction, drying in a vacuum oven at 70°C for 12h, and obtaining anion as PF 6 - The ionic liquid phosphate flame retardant (abbreviated as [PCMIM]PF 6 ), the structural formula is as follows:

[0051]

[0052] 2. Using ethanol as a solvent, the flame retardant [PCMIM]PF synthesized above was 6 Carry out wet compounding with APP at a mass ratio of 1:5, evaporate the solvent under reduced pressure, and dry in vacuum to obtain a composite flame retardant. Then the composite flame retardant is mixed with polypropylene (S1003) in an addition amount of 30wt% in a Hack torque rheometer at 175°C at a speed of 30rpm for 10min to obtain a flame-retardant polypropylene whose oxyge...

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Abstract

The invention discloses an ionic liquid-type phosphate fire retardant and a preparation method thereof. The formula of the ionic liquid-type phosphate fire retardant is shown in the description. The R in the formula is equal to CnH2n+1, wherein n may be 1, 3 or any even number between 2 and 18; and X may be Cl, Br, BF4, PF6 or N(CF3SO2)2. As the module of the fire retardant disclosed by the invention contains a 1-oxo-4-hydroxymethyl-2,6,7-trioxa-1-phabicyclo[2.2.2]octane(PEPA) framework, the fire retardant combines the acid source and the carbon source of an intumescent flame retardant (IFR). The fire retardant has the characteristics of high thermostability and high charring performance. The fire retardant can combine external gas sources such as ammonium polyphosphate to form a new IFR, which has high fire retarding efficiency and high compatibility with polymeric substrates.

Description

1. Technical field [0001] The invention relates to a flame retardant and a preparation method thereof, in particular to a preparation method of an ionic liquid type phosphate flame retardant. 2. Background technology [0002] In recent years, with the continuous development of science and technology, polymer materials have been widely used in the fields of national defense, construction, transportation, aviation, electrical appliances, and household furniture. However, most polymer materials are easy to burn and release a large amount of toxic smoke, which brings huge threats and losses to the safety of people's lives and properties. Therefore, it is of great significance to carry out flame retardant treatment on polymer materials. [0003] Since the 1990s, intumescent flame retardant (IFR) has been considered as a promising flame retardant method due to its low smoke, low toxicity and superior anti-dripping properties, and has gradually become a polymer The focus of mater...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K5/527C08L23/12C07F9/6574
CPCY02P20/54
Inventor 丁运生杨雪峰何飞陈守雨
Owner HEFEI UNIV OF TECH
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