Reactive phosphorus triazine flame retardant for dyeing, and preparation method and application thereof

A reactive, triazine-based technology, applied in the field of flame retardants, can solve problems such as toxic gases, secondary hazards, and limited application range, and achieve the effects of good carbon formation, high thermal stability, and simple preparation methods

Inactive Publication Date: 2012-08-15
ZHONGBEI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Halogenated flame retardants were mostly used in the early days, which have the characteristics of less addition, obvious flame retardant effect, and high cost performance, but they will release toxic and corrosive gases when burning, causing "secondary hazards" while flame retardant. Applications are limited

Method used

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  • Reactive phosphorus triazine flame retardant for dyeing, and preparation method and application thereof
  • Reactive phosphorus triazine flame retardant for dyeing, and preparation method and application thereof
  • Reactive phosphorus triazine flame retardant for dyeing, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] The preparation method of the reactive phosphorus-containing triazine flame retardant used in the dyeing process comprises the following steps:

[0041] (1) Synthesis of PEPA: Add 67.2g (0.50mol) of pentaerythritol and 200mL of 1,4-dioxane to a 500mL four-necked flask equipped with a nitrogen conduit, a thermometer, a constant pressure dropping funnel, a stirrer, and a reflux condenser Ring, start stirring, pass nitrogen protection, heat up to 80°C, add 76.6g (0.50mol) phosphorus oxychloride quickly and then slowly within 2h, after dropping, add 2~3 drops of triethylamine, and reflux for 10h , let it cool down to room temperature, and filtered to obtain a white solid, which was washed once with 100mL 1,4-dioxane, once with 100mL n-hexane, once with 100mL absolute ethanol, once with 50mL diethyl ether, and then placed in a vacuum at 60°C After drying in an oven for 5 hours, 83.7 g of a white solid was obtained, with a yield of 92.3%;

[0042] (2) In a 250mL four-necked ...

Embodiment 2

[0054] The preparation method of the reactive phosphorus-containing triazine flame retardant used in the dyeing process comprises the following steps:

[0055] (1) Synthesis of PEPA: Add 67.2g (0.50mol) of pentaerythritol and 200mL of 1,4-dioxane to a 500mL four-necked flask equipped with a nitrogen conduit, a thermometer, a constant pressure dropping funnel, a stirrer, and a reflux condenser ring, start stirring, pass nitrogen protection, heat up to 80°C, add 107.2g (0.70mol) phosphorus oxychloride quickly and then slowly within 2h, after dropping, add 2~3 drops of triethylamine, and reflux for 8h , let stand to cool to room temperature, filtered to obtain a white solid, washed four times with 100mL 1,4-dioxane, and then dried in a vacuum oven at 60°C for 5h to obtain a white solid with a yield of 91.6%;

[0056] (2) In a 250mL four-necked flask equipped with a condenser, a thermometer and a stirring device, add 0.025mol of cyanuric chloride powder, then add 30mL of dichlorom...

Embodiment 3

[0061] The preparation method of the reactive phosphorus-containing triazine flame retardant used in the dyeing process comprises the following steps:

[0062] (1) Synthesis of PEPA: Add 67.2g (0.50mol) of pentaerythritol and 200mL of 1,4-dioxane to a 500mL four-necked flask equipped with a nitrogen conduit, a thermometer, a constant pressure dropping funnel, a stirrer, and a reflux condenser ring, start stirring, pass nitrogen protection, heat up to 80°C, add 91.9g (0.60mol) phosphorus oxychloride quickly and then slowly within 2h, after dropping, add 2~3 drops of triethylamine, and reflux for 6h , stand to cool to room temperature, filter to obtain a white solid, wash once with 100mL of n-hexane, 100mL of absolute ethanol once, and 50mL of diethyl ether once, and then put it in a vacuum oven at 60°C for 5h to obtain a white solid. The yield is 89.9%;

[0063] (2) In a 250mL four-neck flask equipped with a condenser, a thermometer and a stirring device, add 0.025mol of cyanu...

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Abstract

The invention discloses reactive phosphorus triazine flame retardant for dyeing, and a preparation method and application thereof, which belong to the technical field of flame retardants and relate to flame retardant for cotton. A molecular structure of the reactive phosphorus triazine flame retardant for dyeing is OPO3OCLO3OO3PO. The preparation method includes: mixing pentaerythritol with dioxane under protection of inert gases, dropwise adding phosphorus oxychloride at 80 DEG C for two hours, adding two to three drops of triethylamine, allowing for reaction for 4-10 hours, cooling, filtering, vacuum-drying to obtain PEPA after rinsing; and mixing cyanuric chloride with reaction solvent, adjusting the temperature to 10-20DEG C, initially dropwise adding the PEPA and acid-binding agent, allowing for continuous reaction for 6 hours, dropwise adding again the PEPA and the acid-binding agent, allowing for reaction for 6 hours, adding precipitant for precipitation after cooling, filtering, rinsing, and drying to obtain the fished product. The preparation method is simple, the prepared flame retardant has a carbon source, an acid source and a gas source integrated and is higher in thermal stability and better in carbon forming performance, and the PEPA and the triazine structure are complemented while both being given to full play to the advantages.

Description

technical field [0001] The invention belongs to the technical field of flame retardants and relates to a flame retardant for cotton, in particular to a reactive phosphorus-containing triazine flame retardant used in dyeing process and its preparation method and application. Background technique [0002] Cotton fabrics are widely welcomed and accepted by people because of their excellent physical and mechanical properties, good hygroscopicity, comfortable wearing, and wide range of sources. However, the limiting oxygen index (LOI) of cotton is only about 18%, which is a flammable fiber. With the development of science and technology and the progress of the textile industry, the types of textiles have been increasing, and the application range has been extended to all aspects of production and life, such as clothing, decoration and industry. conditions. Halogenated flame retardants were mostly used in the early stage, which have the characteristics of less addition, obvious ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D06M13/44C07F9/6574D06M101/06
Inventor 刘亚青赵培华孙付宇张美赵贵哲
Owner ZHONGBEI UNIV
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