Method for synthesizing phosphorus and nitrogen flame retardant (spiro phosphoryl pyrrolidine)

A technology of spirocyclic phosphoryl tetrahydropyrrole and phosphorus-nitrogen flame retardants, which is applied in the field of synthesis of phosphorus-nitrogen flame retardants, can solve the problems of high cost, many raw materials, cumbersome operation process, etc., and achieve cost saving and good flame retardancy The effect, the effect of simple operation of the process

Inactive Publication Date: 2013-04-17
NORTHEAST FORESTRY UNIVERSITY
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Problems solved by technology

[0004] The present invention provides a method for synthesizing the phosphorus-nitrogen flame retardant spirophosphoryl tetrahydropyrrole in order to solve the technical problem that many raw materials are required for the synthesis of the existing expansion-type phosphorus-nitrogen flame retardant, which leads to cumbersome operation process and high cost.

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  • Method for synthesizing phosphorus and nitrogen flame retardant (spiro phosphoryl pyrrolidine)
  • Method for synthesizing phosphorus and nitrogen flame retardant (spiro phosphoryl pyrrolidine)
  • Method for synthesizing phosphorus and nitrogen flame retardant (spiro phosphoryl pyrrolidine)

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specific Embodiment approach 1

[0015] Specific implementation mode one: the synthesis method of the phosphorus nitrogen flame retardant spirophosphoryl tetrahydropyrrole of the present embodiment is carried out according to the following steps:

[0016] a, with spirophosphoryl chloride and tetrahydropyrrole as raw materials, carry out reflux reaction in acetone; wherein the mol ratio of spirophosphoryl chloride and tetrahydropyrrole is 1: (4~4.6), the consumption of spirophosphoryl chloride and acetone The ratio is 1g: (10~18)ml, the reaction temperature is controlled at 50~60°C, and the reaction time is 6~8h; b, filter after cooling to room temperature, then wash, recrystallize with distilled water after washing, and finally dry in vacuum Dried in a device to obtain spirocyclic phosphoryl tetrahydropyrrole, the reaction equation is:

[0017]

[0018] The synthesis method of the phosphorus-nitrogen flame retardant spirophosphoryl tetrahydropyrrole of the present embodiment is a new type of phosphorus-nit...

specific Embodiment approach 2

[0019] Specific embodiment two: the difference between this embodiment and specific embodiment one is: in the reaction process, spirophosphoryl chloride is first added to acetone, and tetrahydropyrrole is added dropwise under stirring state, other steps and parameters and specific embodiment One is the same.

specific Embodiment approach 3

[0020] Specific embodiment three: this embodiment differs from specific embodiment one or two in that: in the reaction process, when spirophosphoryl chloride is completely dissolved in acetone, tetrahydropyrrole is added dropwise, and other steps and parameters are the same as in specific embodiment one or two the same.

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Abstract

The invention discloses a method for synthesizing a phosphorus and nitrogen flame retardant (spiro phosphoryl pyrrolidine) and relates to a method for synthesizing a phosphorus and nitrogen flame retardant, which solves the technical problems that the operation process is complicated and the cost is high because multiple raw materials are required for synthesizing the conventional expansive type phosphorus and nitrogen flame retardant. The synthesizing method comprises the following steps of: adding spiro phosphoryl chloride into acetone, adding pyrrolidine dropwise in a stirring state, carrying out heating reflux reaction after dripping is finished, and then washing by using ice water and acetone so as to obtain the spiro phosphoryl pyrrolidine. According to the method, the operation is easy, the cost is saved, a product has 30 percent of residual volume at the temperature of 800 DEG C, the coal bed of the flame retardant formed at high temperature has high stability, the coal bed is prevented from being contacted with air on the surface of the flame-retardant material and has a good flame-retardant effect on high polymer materials, the yield is over 75 percent, and the flame retardant is of expanded type, and integrates a carbon source, an acid source and an air source and is applied to the field of expanded phosphorus and nitrogen flame retardants.

Description

technical field [0001] The invention relates to a method for synthesizing a phosphorus-nitrogen flame retardant. Background technique [0002] With the rapid development of the material synthesis industry, the requirements for its flame retardant safety are getting higher and higher. Therefore, the development and research of flame retardants has gradually become a hot spot. In 1963, Ratz et al synthesized spirophosphoryl chloride with pentaerythritol and phosphorus oxychloride (chemical name is 3,9-dichloro-2,4,8,10-tetrachloro-3,9-diphosphorous spirocyclic -3,9-dioxo[5.5]undecane). In 2002, Li Bin, Sun Caiying and others improved their synthesis method to make the reaction more stable and yield higher, and applied for a Chinese invention patent with the patent number ZL02133071.9. Spirocyclic phosphorus oxychloride is a cage structure and is highly symmetrical. It generates a large amount of charcoal and acid during combustion. Therefore, spirocyclic phosphorus oxychlori...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574C08K5/5399
Inventor 孙才英宋秋丽王红陈佩佩张依夏
Owner NORTHEAST FORESTRY UNIVERSITY
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