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Dicyclic phosphonate fire retardant and its synthesis

A kind of bicyclic phosphonate, technology of synthesis method

Inactive Publication Date: 2007-01-03
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] However, the existing synthetic route and synthesis method have many steps to synthesize from basic raw materials, and the possible synthetic yield is low and has no industrial production value.

Method used

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  • Dicyclic phosphonate fire retardant and its synthesis
  • Dicyclic phosphonate fire retardant and its synthesis
  • Dicyclic phosphonate fire retardant and its synthesis

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Example 1: Take 13.6 grams (0.1 mole) of pentaerythritol and 27.3 grams (0.22 mole) of dimethyl methylphosphonate in a 100 ml round bottom flask and stir well. Then 0.3 g of sodium methoxide was added as a catalyst. Stir at 180°C for 24 hours under nitrogen protection. Then the temperature was raised slowly to 190° C. for 6 hours, and excess dimethyl methylphosphonate was released under vacuum conditions. After cooling down to room temperature, 100ml of cyclohexane was added to the reaction system. After fully stirring, it was washed twice with 10ml of water. After phase separation, the organic phase was concentrated, cooled, and crystallized to obtain white needle-like crystals with a yield of 62%. The analysis test results are as follows:

[0025] Elemental analysis (%): C is 26.67 (26.25), H is 5.54 (5.38), P is 19.15 (19.38), and the theoretical values ​​are in brackets. Infrared spectroscopy and NMR analysis confirmed the structure of the synthesized product.

Embodiment 2

[0026] Embodiment 2: other is the same as embodiment 1, uses sodium ethylate instead as catalyzer, yield 65%.

Embodiment 3

[0027] Embodiment 3: Others are the same as in Embodiment 1, the addition of diethyl ammonium methyl phosphate is 31.0 g (0.25 mol), and the yield is 73%.

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Abstract

The present invention discloses one kind of dicyclic phosphonate fire retardant in the structure as shown. Its synthesis process includes the following steps: 1. setting pentaerythritol and dimethyl methyl phosphonate or diethyl methyl phosphonate in the molar ratio of 1 to 2-3 in some connector, adding solvent and catalyst, and stirring at 150-190 deg.c under the protection of inert gas for 3-28 hr; and 2. slowly raising the temperature to 150-180 deg.c, maintaining for 6-26 hr, eliminating excessive dimethyl methyl phosphonate or diethyl methyl phosphonate under vacuum, and lowering the temperature to room temperature to obtain the fire retardant. The synthesis process is simple, efficient, no halogen and environment friendly, and the fire retardant has high phosphorus content, is solid at normal temperature, heat stable and compatible with polymer, and may be used in different fire retardant systems.

Description

technical field [0001] The invention relates to a phosphorus-containing organic compound and a synthesis method thereof, in particular to a spiropentaerythritol methylphosphonate which can be used as a flame retardant and a synthesis method thereof. Background technique [0002] Since the 1980s, flame retardants have become the largest additives used in synthetic materials next to plasticizers. Among the flame retardants of organic compounds, the amount of organophosphorus flame retardants is second only to organobromine flame retardants, but the latter has limited application in some fields due to the problems of corrosion and release of toxic substances during combustion, and its usage has increased Slow, while organophosphorus flame retardants have received extensive attention in recent years due to their high flame retardant efficiency and relatively little release of toxic substances during combustion. [0003] Most of the traditional phosphate flame retardants are liq...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K21/04C07F9/40
Inventor 彭治汉
Owner DONGHUA UNIV
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