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A dopo-type reactive flame retardant whose end group is an epoxy group and its preparation method and application

A reactive flame retardant and epoxy group technology, which is applied to DOPO reactive flame retardants with epoxy groups as end groups and their preparation and application fields, can solve the problems of harsh and complicated synthesis conditions, and avoid production processes. , the effect of high yield and simple synthesis process

Inactive Publication Date: 2017-09-01
QUANGANG PETROCHEM RES INST OF FUJIAN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The purpose of the present invention is to overcome the problems of harsh and complicated synthetic conditions in the production of the existing structural flame-retardant polyurethane materials, and provide a kind of non-polymeric compound with simple synthesis process, high yield, containing DOPO groups and taking epoxy groups as end groups. Preparation method of halogen environment-friendly polyurethane end-blocking flame retardant

Method used

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  • A dopo-type reactive flame retardant whose end group is an epoxy group and its preparation method and application
  • A dopo-type reactive flame retardant whose end group is an epoxy group and its preparation method and application
  • A dopo-type reactive flame retardant whose end group is an epoxy group and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0047] Add 110g (0.5mol) of 1,4-butanediol diglycidyl ether and 200mL of absolute ethanol into a dry three-necked flask, raise the temperature to 120°C, and stir well. Add 108g (0.5mol) of DOPO into the reaction flask in 5 batches, stir until the solid is completely dissolved and the solution is transparent. After heat preservation at 120°C for 10 hours, cool to room temperature, remove the solvent under reduced pressure to obtain a colorless transparent viscous liquid, dry at 80°C to obtain a phosphorus-containing glycidyl flame retardant with a phosphorus content of 7.41%. Infrared and NMR characterization of samples, such as figure 1 , figure 2 As shown, it can be seen from the graph that the prepared phosphorus-containing glycidyl flame retardant is phosphorus-containing 1,4-butanediol diglycidyl ether.

[0048] 112g (0.056mol) polyester ethylene adipate diol, 6g (0.097mol) ethylene glycol, 5g (0.055mol) 1,4-butanediol, 120mL N,N-dimethylformamide, 0.02 g dibutyltin di...

Embodiment 2

[0050] Add 120g (0.5mol) of resorcinol diglycidyl ether and 200mL of absolute ethanol into a dry three-necked flask, raise the temperature to 120°C, and stir evenly. Add 108g (0.5mol) of DOPO into the reaction flask in 5 batches, stir until the solid is completely dissolved and the solution is transparent. After heat preservation at 120°C for 10 hours, cool to room temperature, remove the solvent under reduced pressure to obtain a colorless transparent viscous liquid, and dry at 80°C to obtain a phosphorus-containing glycidyl flame retardant with a phosphorus content of 6.80%.

[0051] 112g (0.056mol) polyester ethylene adipate diol, 6g (0.097mol) ethylene glycol, 5g (0.055mol) 1,4-butanediol, 120mL N,N-dimethylformamide, 0.02g dibutyltin dilaurate, mix well under stirring at 85 ℃, first add 37.5g (0.15mol) and 12.5g (0.05mol) of MDI in batches, toluene to adjust the viscosity, then add 10.42g (0.041mol) in batches ) MDI, until the viscosity of the polyurethane is 40000-80000...

Embodiment 3

[0053] Add 154.5g (0.5mol) of triglycidyl p-aminophenol and 200mL of absolute ethanol into a dry three-necked flask, heat up to 120°C, and stir evenly. Add 108g (0.5mol) of DOPO into the reaction flask in 5 batches, stir until the solid is completely dissolved and the solution is transparent. After heat preservation at 120°C for 10 hours, cool to room temperature, remove the solvent under reduced pressure to obtain a colorless transparent viscous liquid, and dry at 80°C to obtain a phosphorus-containing glycidyl flame retardant with a phosphorus content of 8.37%.

[0054] 112g (0.056mol) polyester ethylene adipate diol, 6g (0.097mol) ethylene glycol, 5g (0.055mol) 1,4-butanediol, 120mL N,N-dimethylformamide, 0.02g dibutyltin dilaurate, mix well under stirring at 83 ℃, first add 37.5g (0.15mol) and 12.5g (0.05mol) of MDI in batches, toluene to adjust the viscosity, then add 10.07g (0.041mol) in batches ) MDI, until the viscosity of the polyurethane is 40000-80000pps, add 23.65...

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Abstract

The invention discloses a DOPO type reactive flame retardant with a terminal group as an epoxy group, a preparation method therefor and an application thereof. The preparation method comprises: heating DOPO and a poly(glycidol)-based compound in a reaction molar ratio to react in an organic solvent; and removing the solvent under reduced pressure, thereby obtaining the reactive flame retardant which is a viscous liquid at the room temperature, contains a DOPO flame retardant radical and has the terminal group which is the epoxy group. The flame retardant synthetic method is simple, easy to control, good in repeatability, high in yield, suitable for enlarged production, and can be used as an end-sealed type flame retardant which is applied to flame resistance of a polyurethane material. The flame retardant is applied to the polyurethane material, so that not only are defects of poor compatibility between the added flame retardant and a basal body, easy run-off in a using process and the like overcome, but also a complex process for synthesizing polyhydric alcohols by use of a conventional reactive flame retardant is avoided; and the flame resistance of the material is obviously improved, the oxygen index of polyurethane leather is increased to 26-28%, and the flame retardant level can reach level UL94 V-0.

Description

technical field [0001] The invention relates to a preparation method of a DOPO type reactive flame retardant whose end group is an epoxy group and its application in polyurethane. Background technique [0002] Polyurethane is a material with relatively comprehensive properties, which has the advantages of good physical and mechanical properties, excellent weather resistance and elasticity. It is widely used in aviation, electronics, machinery, medical treatment, chemical industry and other fields. However, since the polyurethane material is an organic polymer material, it is extremely flammable, and its limiting oxygen index (LOI) is only 18. It releases a large amount of heat during combustion, which is not only prone to dripping, but also produces a large amount of HCN, CO, and NH. 3 and other toxic fumes, seriously endangering life and property safety. Therefore, the research on flame retardant modification of polyurethane materials has attracted more and more attention...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G18/38C08G18/66C08G18/76C08G18/42C07F9/6574
CPCC07F9/657172C08G18/388C08G18/4238C08G18/66C08G18/7671
Inventor 郑雪琳翁家宝李毅辉陈登龙
Owner QUANGANG PETROCHEM RES INST OF FUJIAN NORMAL UNIV