Preparation method of organic phosphine flame retardant 1-hydroxyl phosphate

A technology of hydroxyphosphonite and flame retardant, which is applied in the field of 1-hydroxyalkylphosphonite, can solve the problems of hypophosphorous acid corrosion, limited application, explosion, etc., and achieve low cost, and the preparation method is environmentally friendly and safe Effect

Inactive Publication Date: 2019-05-24
QUANZHOU NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Hamilton, R. is mainly prepared by reacting hypophosphorous acid as a raw material. Hypophosphorous acid is corrosive, and it is decomposed by high heat to produce highly toxic phosphine gas, and even explodes, which limits its application as a P-C bond, especially 1 Application in Synthesis of -Hydroxybenzylphosphonous Acid

Method used

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  • Preparation method of organic phosphine flame retardant 1-hydroxyl phosphate
  • Preparation method of organic phosphine flame retardant 1-hydroxyl phosphate
  • Preparation method of organic phosphine flame retardant 1-hydroxyl phosphate

Examples

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Effect test

Embodiment 1

[0040] Embodiment 1: Synthesis of sodium 1-hydroxybenzyl phosphinate

[0041] Add 1mol sodium hypophosphite and 1.5mol benzaldehyde into a 5L reaction kettle, add 2L DMF, plug a rubber stopper or a condenser, heat and react at 110°C for 24h, filter the reaction sample with suction after the reaction, wash and dry with alcohol, and the yield is 85%.

[0042] Sodium 1-Hydroxybenzylphosphinate, structural formula 1H NMR (400MHz, D2O): δ7.36-7.47(m, 5H), 7.50(dd, Jp-H=516.2Hz, JH-H=1.0Hz, 0.5H), 4.69-4.72(d, JH-H =9.0Hz, 1H); 13C NMR (100MHz, D2O): δ137.4, 128.6, 127.9, 127.1, 73.9 (d, JC-P = 105.9Hz), 31P NMR (162MHz, D2O): δ26.6. Phosphorus spectrum see figure 1 .

[0043] The synthesized product consists of the following:

[0044] Sodium 1-hydroxybenzylphosphinate: 97mol%;

[0045] Sodium bis(1-hydroxybenzyl)phosphonate: 2mol%

[0046] Sodium 1-hydroxybenzylphosphonate: 1mol%

Embodiment 2

[0047] Embodiment 2: Synthesis of sodium 1-hydroxybenzyl phosphinate

[0048] Add 1 mol of sodium hypophosphite and 1.75 mol of benzaldehyde into a 5L reaction kettle, add 2L of DMF, plug a rubber stopper or a condenser, heat and react at 110°C for 24 hours, filter the reaction sample after the reaction, wash and dry with alcohol, and the yield is 88%.

[0049] The synthesized product consists of the following:

[0050] Sodium 1-hydroxybenzylphosphonite: 98mol%;

[0051] Sodium bis(1-hydroxybenzyl)phosphonate: 1.5mol%;

[0052] Sodium 1-hydroxybenzylphosphonate: 0.5 mol%.

Embodiment 3

[0053] Embodiment 3: Synthesis of sodium 1-hydroxybenzyl phosphonate

[0054] Add 1mol sodium hypophosphite and 2mol benzaldehyde into a 5L reaction kettle, add 2L DMF, plug a rubber stopper or a condenser, heat and react at 110°C for 24h, filter the reaction sample after the reaction, wash and dry with alcohol, and the yield is 89%.

[0055] The synthesized product consists of the following:

[0056] Sodium 1-hydroxybenzylphosphonite: 98.5mol%;

[0057] Sodium bis(1-hydroxybenzyl)phosphonate: 1mol%;

[0058] Sodium 1-hydroxybenzylphosphonate: 0.5 mol%.

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Abstract

The invention discloses a preparation method of an organic phosphine flame retardant 1-hydroxyl phosphate. The method includes the following steps that hypophosphite and aldehyde serve as raw materials, DMF / DMSO / DMP serve as solvents, a heating reaction is carried out, filtering and alcohol washing is performed after the reaction, and 1-hydroxyl alkyl phosphate is obtained; the pH value of 1-hydroxyl alkyl phosphate is adjusted to be 2-3, and 1-hydroxyl alkyl phosphate reacts with melamine, aluminum salt and zinc salt to obtain the product. According to the method, a one-pot method is utilizedto obtain1-hydroxyl alkyl phosphate, the production process is simple, the operation is easy, and the solvent and the raw materials can be repeatedly used.

Description

technical field [0001] The invention relates to a preparation method of an organic phosphine flame retardant 1-hydroxyalkylphosphonite and the use of the 1-hydroxyalkylphosphonite prepared by the process. Background technique [0002] Salts of organophosphates are known as flame retardants. They can be made by various processes. [0003] For example, EP0699708A2 describes flame-retardant polyester molding compositions in which flame retardancy is imparted to the polyester by addition of calcium or aluminum salts of phosphinic or diphosphinic acids. The aforementioned salts are obtained by reacting the corresponding dialkylphosphinic acids with calcium hydroxide or with aluminum hydroxide. [0004] DE 2447727 A1 describes flame-retardant polyamide molding compositions comprising salts of phosphinic or diphosphinic acids. [0005] CN1660858B describes the patent of the flame-retardant polymer of alkyl phosphate, and the above-mentioned salt is obtained by reaction of hypoph...

Claims

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Application Information

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IPC IPC(8): C07F9/30C07F9/38C07D251/56C08K5/51
Inventor 徐文涛尹应武庄华强陈文杰
Owner QUANZHOU NORMAL UNIV
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