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Novel method for synthesizing and purifying phosphonitrilic chloride trimer

A technology of hexachlorocyclotrimeric phosphazene and a new method, which is applied in the field of preparing and purifying fine chemical intermediates, and synthesizing and purifying hexachlorocyclotrimeric phosphazene, which can solve the impact of yield, the destruction of cyclic trimers, and the inability to obtain High-purity products and other issues to achieve the effect of increasing yield and reducing costs

Inactive Publication Date: 2014-02-12
上海永鸿实业集团化学科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Publication No. US4567028 and CN101157704A disclose the traditional preparation method of hexachlorocyclotriphosphazene, which is based on PCl 5 and NH 4 Cl as raw material, using pyridine as catalyst, reflux in an inert solvent for a certain period of time, then distill off chlorobenzene, and recrystallize to obtain the product, but actually using pyridine as a catalyst is not conducive to the recovery and utilization of chlorobenzene, and recrystallization cannot completely remove the system The cyclic tetramer in the product cannot be obtained with high purity
There is also a patent with a publication number of US4605539 that uses water washing to remove the cyclic tetramer, but at the same time the cyclic trimer will also be damaged, and the product with high purity cannot be obtained, and the yield is also affected.
These traditional production methods have low yield, low product purity and high cost, and are not suitable for industrialized large-scale production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] In a 500 mL three-necked reaction flask, add 20 g of ammonium chloride, 300 mL of chlorobenzene and 50.8 g of phosphorus pentachloride, and add 0.4 g of FeCl 3 Catalyst, reacts at 125 o C temperature reaction for 8 hours, evaporate part of chlorobenzene at normal pressure, cool to 40-50 o C filter to remove excess ammonium chloride, then remove the remaining chlorobenzene under reduced pressure, cool to room temperature, add n-hexane to dissolve the product and filter to remove linear polymers, remove the n-hexane solution under reduced pressure to obtain crude hexachlorocyclotrimeric phosphazene product. 10 g of hexachlorocyclotrimeric phosphazene with a yield of 35% was obtained by sublimation purification.

Embodiment 2

[0021] In a 500 mL three-neck reaction flask, add 20 g of ammonium chloride, 300 mL of chlorobenzene and 50.8 g of phosphorus pentachloride, and add 0.4 g of AlCl 3 Catalyst, reacts at 125 o C temperature reaction for 8 hours, evaporate part of chlorobenzene at normal pressure, cool to 40-50 o C filter to remove excess ammonium chloride, then remove the remaining chlorobenzene under reduced pressure, cool to room temperature, add n-hexane to dissolve the product and filter to remove linear polymers, remove the n-hexane solution under reduced pressure to obtain crude hexachlorocyclotrimeric phosphazene product. 12 g of hexachlorocyclotrimeric phosphazene with a yield of 42% was obtained by sublimation purification. Example 3:

Embodiment 3

[0022] In a 5 L three-necked reaction flask, add 200 g of ammonium chloride, 3000 mL of chlorobenzene and 500 g of phosphorus pentachloride, and add 2.0 g of ZnCl 2 Catalyst, reacted at 128 o C temperature reaction for 15 hours, evaporate part of chlorobenzene at normal pressure, cool to 40-50 o C filter to remove excess ammonium chloride, then remove the remaining chlorobenzene under reduced pressure, cool to room temperature, add n-hexane to dissolve the product and filter to remove linear polymers, remove the n-hexane solution under reduced pressure to obtain crude hexachlorocyclotrimeric phosphazene product. 166 g of hexachlorocyclotrimeric phosphazene with a yield of 60% was obtained by sublimation purification.

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PUM

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Abstract

The invention discloses a novel method for synthesizing and purifying phosphonitrilic chloride trimer by taking Lewis acid as the catalyst and adopting the sublimation method. The method disclosed by the invention is characterized by comprising the following steps of: synthesizing phosphonitrilic chloride trimer in chlorobenzene as the solvent by selecting Lewis acid as the catalyst and taking ammonium chloride and phosphorus pentachloride as the raw materials, after removing chlorobenzene, dissolving phosphonitrilic chloride trimer by using normal hexane to eliminate linear polymer, and finally, purifying by adopting the sublimation method to obtain phosphonitrilic chloride trimer with the purity of above 99%, wherein the total yield is about 60%. Compared with the prior art, the catalytic system is optimized; the purity of the prepared phosphonitrilic chloride trimer is high; and the novel method disclosed by the invention is applied to industrialized mass production.

Description

technical field [0001] The invention relates to a new method for preparing and purifying fine chemical intermediates, in particular to a new method for synthesizing and purifying hexachlorocyclotrimeric phosphazene, which belongs to the field of chemical synthesis and purification. Background technique [0002] Phosphazenes are a class of inorganic-organic compounds whose skeletons are alternately arranged with phosphorus atoms and nitrogen atoms, and can be divided into cyclic phosphazenes and polyphosphazenes. Cyclic phosphazene compounds are a class of inorganic substances formed by changing the two substituents on the phosphorus atom with a polycyclic ring in which phosphorus and nitrogen atoms are alternately arranged as the skeleton. The diversification of the side groups of phosphazene compounds endows them with a variety of material properties after polymerization, such as good flame retardancy, high temperature resistance, oxidation resistance and organic solvent re...

Claims

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Application Information

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IPC IPC(8): C07F9/6593
Inventor 金伊男陈恒伟
Owner 上海永鸿实业集团化学科技有限公司
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