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Chelating coordination type phosphorus-boron-nitrogen synergistic flame retardant and preparation method thereof

A synergistic flame retardant and coordination technology, used in the field of flame retardant materials, can solve the problems of insufficient surface treatment technology, poor compatibility between flame retardants and materials, and poor thermal stability.

Pending Publication Date: 2021-03-05
TIANJIN POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Phosphorus-based flame retardants have the advantages of high flame retardant efficiency and wide flame retardant adaptability (Cellulose, 2019; 26(6): 4225), but there are still some problems in their wide adaptation, such as: the relationship between flame retardants and materials The compatibility is not good, the surface treatment technology is not perfect; most of the organophosphorus flame retardants are liquid, with strong volatility, large smoke generation, poor thermal stability, etc., so that their application is limited

Method used

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preparation example Construction

[0012] The invention provides a chelating coordination type phosphorus-boron-nitrogen synergistic intumescent flame retardant and a preparation method thereof, which is characterized in that the specific steps are as follows:

[0013] 1) Add reactant phytic acid, polyhydric alcohol and boric acid and solvent in the flask, preferably (or without solvent), at a certain temperature, stir the reaction until the end of the reaction;

[0014] 2) After the reaction is completed, the solvent is removed (there is no such step without a solvent) to obtain an intermediate;

[0015] 3) Add deionized water and urea to the intermediate product, and continue to heat and stir the reaction at a certain temperature until the end of the reaction to obtain a viscous liquid, which is the target flame retardant.

[0016] 4) Use the target flame retardant directly as an additive, or configure it into an aqueous solution with a certain solubility, and arrange the target flame retardant by means of di...

Embodiment 1

[0032] 1) Add the reactant phytic acid (0.4mol), ethylene glycol (0.8mol) and boric acid (0.4mol) and solvent toluene 100mL in the flask, stir the water separation and reflux reaction until the reaction is completed;

[0033] 2) After the reaction is completed, cool down and remove the solvent toluene to obtain an intermediate;

[0034] 3) Add deionized water (0.5 mol) and urea (2.0 mol) to the intermediate product, heat and stir at 100°C until the reaction ends at pH=2-8, and a viscous liquid is obtained, which is the target flame retardant.

[0035] 4) The prepared flame retardant is configured into a 120g / L aqueous solution, and the cotton fabric is finished by dipping, padding, ultrasonication, etc. After drying and curing, the target flame retardant product can be obtained. After 50 washing cycles of the obtained cotton fabric, the oxygen index >28 and above, the vertical burning carbon length is less than 60mm.

Embodiment 2

[0037] 1) Add reactant phytic acid (0.4mol), glycerol (0.6mol) and boric acid (0.4mol) and solvent toluene 100mL in the flask, stir and reflux until the reaction ends;

[0038] 2) After the reaction is completed, cool down and remove the solvent toluene to obtain an intermediate;

[0039] 3) Add deionized water (0.5 mol) and urea (1.0 mol) to the intermediate product, heat and stir at 100°C until the reaction is completed at pH=2-8, and a viscous liquid is obtained, which is the target flame retardant.

[0040] 4) The prepared flame retardant is configured into a 90g / L aqueous solution, and the cotton fabric is finished by dipping, padding, ultrasonication, etc. After drying and curing, the target flame retardant product can be obtained. After 50 washing cycles of the obtained cotton fabric, the oxygen index >28 and above, the vertical burning carbon length is less than 60mm.

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Abstract

The invention discloses a chelating coordination type phosphorus-boron-nitrogen synergistic flame retardant and a preparation method and application thereof. The flame retardant is prepared from phytic acid, polyol, boric acid and urea through esterification, chelating coordination and other reactions. The chelating coordination type phosphorus-boron-nitrogen synergistic flame retardant can be used as a raw material additive of cellulose, polyester, polylactic acid, epoxy resin, wood, moso bamboos, plywood, shaving boards, rubber, plastics, elastomers and the like, or can be used as a main functional object of a flame-retardant coating, and can also be used as a grafting or curing function object of fabric or non-woven fabric. The flame retardant adopts a chelating coordination mode, and durable application of a boron element is achieved; the flame retardant property of the flame retardant is improved through a phosphorus-nitrogen-boron synergistic flame retardant mode; the defects that an existing phosphorus-nitrogen flame retardant is poor in compatibility with a matrix and prone to migration and loss can be overcome; and the flame retardant has the advantages of being environmentally friendly, renewable, cheap in raw material, easy and convenient to prepare, good in flame retardant effect and the like.

Description

technical field [0001] The invention relates to the field of flame retardant materials, in particular to a phosphorus-boron-nitrogen synergistic flame retardant and its preparation method and application. Background technique [0002] Flame retardants, also known as fire retardants or flame retardants, are a class of functional additives that can impart flame retardancy to combustibles. At present, there are many research fields and classifications of flame retardants. Halogenated flame retardants are widely used in market applications. However, during the use of halogenated flame retardants, the burning smoke is large, toxic and corrosive gases are released, and the environment is polluted. The market has strictly prohibited their use. Research It is urgent to develop high-efficiency, low-toxicity, smoke-free, green and environmentally friendly flame retardants. Phosphorus-based flame retardants and nitrogen-based flame retardants in intumescent flame retardants have excel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): D06M13/503C08K5/55C07F9/6596D06M101/06
CPCD06M13/503C08K5/55C07F9/6596D06M2101/06D06M2200/30
Inventor 朱文举程博闻杨名扬
Owner TIANJIN POLYTECHNIC UNIV
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