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Polyhydroxy cage-shaped P-N synergistic flame retardant and synthesis method thereof

A polyhydroxyl cage-like, synergistic flame retardant technology, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc. , The effect of improving mechanical properties and high flame retardant efficiency

Inactive Publication Date: 2022-01-14
KUNMING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, because it only contains a single flame-retardant P element, it often cannot meet high application requirements, so it is particularly necessary to add other flame-retardant elements.

Method used

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  • Polyhydroxy cage-shaped P-N synergistic flame retardant and synthesis method thereof
  • Polyhydroxy cage-shaped P-N synergistic flame retardant and synthesis method thereof
  • Polyhydroxy cage-shaped P-N synergistic flame retardant and synthesis method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] A kind of synthetic method of polyhydroxyl cage-like P-N synergistic flame retardant, the steps that it comprises are as follows:

[0032] a. Accurately weigh 0.05 mol of TGIC and 0.15 mol of PEPA and dissolve them in 150 mL and 100 mL of N,N-dimethylformamide (DMF), respectively;

[0033] b. After adding the PEPA solution into the reactor, add 0.15g of benzyltriethylammonium chloride;

[0034] c. Adjust the temperature of the oil bath to the condensation reaction temperature of 100°C, and drip the TGIC solution into the reaction kettle, and the dripping time is 20 hours;

[0035] d. Continue to raise the temperature to 100° C., feed nitrogen gas at a rate of 10 mL / min, avoid the influence of moisture in the air on the reaction, and react at a constant temperature for 8 hours.

[0036] e. After the reaction is completed, use a rotary evaporator to spin dry the DMF, extract the reaction product with methanol, and then filter it to leave the part soluble in methanol, and...

Embodiment 2

[0038] A kind of synthetic method of polyhydroxyl cage-like P-N synergistic flame retardant, the steps that it comprises are as follows:

[0039] a. Accurately weigh 0.1mol of TGIC and 0.36mol of PEPA and dissolve them in 300mL and 200mL of DMF respectively;

[0040] B, the PEPA solution is added in the reactor, then add 1g of benzyltriethylammonium chloride;

[0041] c. Adjust the temperature of the oil bath to the condensation reaction temperature of 110°C, and drip the TGIC solution into the reaction kettle with a dripping time of 15 hours;

[0042] d. Continue to raise the temperature to 110° C., feed nitrogen gas at a rate of 15 mL / min, avoid the influence of moisture in the air on the reaction, and react at a constant temperature for 8 hours.

[0043] e. After the reaction is completed, use a rotary evaporator to spin dry the DMF, extract the reaction product with methanol, filter the part soluble in methanol, and spin dry again; use ethanol to extract, take the part so...

Embodiment 3

[0045] A kind of synthetic method of polyhydroxyl cage-like P-N synergistic flame retardant, the steps that it comprises are as follows:

[0046] a. Accurately weigh 0.25mol of TGIC and 1mol of PEPA and dissolve them in 750mL and 500mL of DMF respectively;

[0047] B, the benzyltriethylammonium chloride of 7.4g is added after the PEPA solution is joined in the reactor;

[0048] c. Adjust the temperature of the oil bath to the condensation reaction temperature of 120°C, and drip the TGIC solution into the reaction kettle for 16 hours;

[0049]d. Continue to raise the temperature to 120° C., feed nitrogen gas at a rate of 20 mL / min, avoid the influence of moisture in the air on the reaction, and react at a constant temperature for 11 hours.

[0050] e. After the reaction is completed, use a rotary evaporator to spin dry the DMF, extract the sample with methanol, and then filter with suction to leave the part soluble in methanol, and spin dry again; use ethanol to extract the pa...

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PUM

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Abstract

The invention discloses a polyhydroxy cage-shaped P-N synergistic flame retardant obtained by reacting triglycidyl isocyanurate with 1-oxo phospha-4-hydroxymethyl-2,6,7-trioxabicyclo[2.2.2] octane under the action of a catalyst. The invention further discloses a contract method of the polyhydroxy cage-shaped P-N synergistic flame retardant. The flame retardant has the advantages of being good in symmetry, high in decomposition temperature, good in material compatibility, capable of adapting to processing of most materials, easy in raw material obtaining, halogen-free, environment-friendly and the like, is easy to form carbon, free of molten drops, low in toxicity and low in smoke in the combustion process, is good in flame retardant effect, and has quite good application and development prospects.

Description

technical field [0001] The invention relates to the technical field of organic compound synthesis, in particular to a ring-opening synthesized polyhydroxyl cage-like P-N synergistic flame retardant and a synthesis method thereof. Background technique [0002] Due to its excellent performance, polymer materials have become the basic raw materials and important materials on which scientific and technological progress and economic development depend. However, due to its flammability, droplet behavior, and a large amount of smoke and toxic gases produced during the combustion process, it has brought huge losses to people's lives and property; therefore, it is necessary to improve the flame retardancy, smoke suppression properties of polymer materials Drip resistance is very necessary. Halogenated flame retardants generally use the gas phase flame retardant mechanism to achieve high-efficiency flame retardant by terminating the chain branching reaction. The high-energy O and H ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574
CPCC07F9/65748
Inventor 谢德龙赵依文谢于辉吴枫冯东何艳萍梅毅
Owner KUNMING UNIV OF SCI & TECH
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