Oligomer type high phosphorus content polyphosphonate halogen-free flame retardant and preparation method thereof

A polyphosphonate and oligomer technology, applied in chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., can solve the problem of reducing the physical properties of polymer materials and the compatibility of polymer materials Poor performance, human and environmental hazards, etc., to achieve the effect of easy large-scale transformation and production, small physical properties, and low cost

Active Publication Date: 2020-09-25
TIANJIN UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, a large number of flame retardants used in polymer materials mainly include halogenated flame retardants and inorganic flame retardants, but halogenated flame retardants will release toxic gases and corrosive hydrogen halide gases during combustion. Harmful to people and the environment; Inorganic flame retardants are used in polymer materials, the addition amount is large, and the compatibility with polymer materials is poor, which will reduce the physical properties of polymer materials

Method used

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  • Oligomer type high phosphorus content polyphosphonate halogen-free flame retardant and preparation method thereof
  • Oligomer type high phosphorus content polyphosphonate halogen-free flame retardant and preparation method thereof
  • Oligomer type high phosphorus content polyphosphonate halogen-free flame retardant and preparation method thereof

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Effect test

Embodiment 1

[0028] A preparation method of oligomer type high phosphorus content polyphosphonate halogen-free flame retardant, the steps are as follows:

[0029] In a 250ml four-neck flask equipped with a thermometer, a stirrer, and a high-efficiency splitter, the air in the flask was driven out with nitrogen, and 12.40g (0.1mol) of dimethylolphosphine oxide and 0.11g of butyl titanate catalyst were added. Under stirring, heat under normal pressure and continue to feed nitrogen, raise the temperature to 120°C, slowly add 9.93g (0.08mol) dimethyl methylphosphonate dropwise, keep the reaction at constant temperature for 4 hours, control the column top temperature not higher than 65°C, when fractional distillation When the methanol produced reaches the theoretical amount, stop nitrogen flow, continue to heat up to 150°C for 0.5h under reduced pressure, and cool to room temperature to obtain light yellow viscous oligomer type high phosphorus content polyphosphonate halogen-free flame retardant...

Embodiment 2

[0036] A preparation method of oligomer type high phosphorus content polyphosphonate halogen-free flame retardant, the steps are as follows:

[0037] In a 250ml four-neck flask equipped with a thermometer, a stirrer, and a high-efficiency splitter, the air in the flask was driven out with nitrogen, and 18.60g (0.15mol) of dimethylolphosphine oxide and 0.17g of sodium methylate catalyst were added. Under stirring, heat under normal pressure and continue to feed nitrogen, raise the temperature to 110°C, slowly add 11.16g (0.09mol) dimethyl methylphosphonate dropwise, and react at constant temperature for 5 hours, and control the column top temperature not higher than 65°C. When the amount of methanol produced reached the theoretical amount, the nitrogen flow was stopped, and the temperature was raised to 140°C for 1 hour of decompression reaction, and cooled to room temperature to obtain a light yellow viscous oligomer-type polyphosphonate halogen-free flame retardant with high p...

Embodiment 3

[0044] A preparation method of oligomer type high phosphorus content polyphosphonate halogen-free flame retardant, the steps are as follows:

[0045] In a 250ml four-neck flask equipped with a thermometer, a stirrer, and a high-efficiency splitter, the air in the flask was driven away with nitrogen, and 16.12g (0.13mol) of dimethylolphosphine oxide and 0.19g of p-toluenesulfonic acid catalyst were added. Under stirring, heat under normal pressure and continue to feed nitrogen gas, raise the temperature to 90°C, slowly add 8.68g (0.07mol) dimethyl methylphosphonate dropwise, keep the reaction at constant temperature for 6h, control the column top temperature not higher than 65°C, when fractional distillation When the methanol produced reaches the theoretical amount, stop nitrogen flow, continue to raise the temperature to 130°C for 1.5h under reduced pressure, and cool to room temperature to obtain light yellow viscous oligomer-type polyphosphate halogen-free flame retardant wit...

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Abstract

The invention relates to an oligomer type high-phosphorous-content polyphosphonate halogen-free flame retardant and a preparation method thereof. The preparation method includes: allowing a certain mole proportion of dihydroxymethyl methyl phosphine oxide and dimethyl methylphosphonate to have reaction for 4-7 hours under nitrogen protection, the effect of a catalyst and the temperature of 90-120DEG C, and performing pressure-reducing reaction for 0.5-2 hours under 120-150 DEG C to obtain the oligomer type high-phosphorous-content polyphosphonate halogen-free flame retardant. The oligomer type high-phosphorous-content polyphosphonate halogen-free flame retardant has the advantages that high-phosphorous-content polyphosphonate is oligomer, active hydroxyl functional groups in the structurecan well compatible with polymer materials, and migration cannot occur easily; the active hydroxyl functional groups can be combined with the polymer materials to form the flame-retardant material, and product stability and high decomposing temperature are achieved; the flame retardant is wide in application range and suitable for being used as the flame retardant of polyolefin, polyurethane, epoxy resin, unsaturated resin and leather. The preparation method is simple in process, low in equipment investment and easy to achieve industrial production.

Description

technical field [0001] The invention relates to the field of organic chemistry, more specifically, an oligomer-type polyphosphonate halogen-free flame retardant with high phosphorus content and a preparation method thereof. Background technique [0002] Polymer materials are widely used in industrial production and people's life. High-rise buildings, interior decoration, electrical appliances, automobiles, and conveyor belts in underground coal mines all have polymer materials. The consumption of polymer materials has become a symbol of the advanced level of science and technology in a country or region. While they are widely used, most polymer materials have a fatal shortcoming, that is, they are easy to decompose and burn at high temperatures. Most of their oxygen index is less than 21, and the oxygen content in the air is 21%, so, as long as they encounter a fire source, most polymer materials will be ignited in the air, and then burn, and their molten droplets can also i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/53C14C9/00C08K5/5397
CPCC07F9/5304C08K5/5397C08L101/00C08L2201/02C14C9/00
Inventor 唐旭东陈晓婷汪俊超
Owner TIANJIN UNIV OF SCI & TECH
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