Method for preparing linear chlorophosphoronitrile

A chlorophosphazene and linear technology, which is applied in the field of preparation of linear polydichlorophosphazene, can solve the problems of high energy consumption, complicated operation, and many waste liquids, and achieves the advantages of simplified process flow, high-efficiency synthesis process and cost reduction. Effect

Inactive Publication Date: 2018-08-24
JINAN TAIXING FINE CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The purpose of the present invention is to propose a more efficient one-step catalytic synthesis of PDCP synthesis process to overcome the current problems of complex operation, high energy consumption and large waste liquid of this type of process

Method used

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  • Method for preparing linear chlorophosphoronitrile
  • Method for preparing linear chlorophosphoronitrile

Examples

Experimental program
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Effect test

Embodiment 1

[0019] Put 0.1g of calcium sulfate dihydrate, 0.22g of ferric chloride, 17g of NH 4 Cl (0.32mol), 60g ground PCl 5 (0.26mol) and 300mL of 1,2,4-trichlorobenzene, stirred and protected by nitrogen, gradually heated up to 190 degrees, reacted for 5 hours, the reaction solution became viscous, cooled to 50 degrees, quickly filtered out insolubles, and the filtrate was added to normal Heptane, a colloidal precipitate was obtained, and centrifuged several times to obtain a colloidal product, linear chlorophosphazene. Yield 40%, total preparation time 7 hours.

[0020] figure 1 Shown is the infrared spectrum of the product, where 1232cm-1 is the stretching vibration peak of the P=N bond, 750cm-1 is the stretching vibration peak of the P-N bond, and 525cm-1 and 575cm-1 are the P-Cl bond stretching vibration peak. The product was judged to be polydichlorophosphazene.

[0021] figure 2 shown for the product 31 In the P-NMR spectrum, the single peak that appears at the chemical ...

Embodiment 2

[0023] Put 0.2g calcium sulfate dihydrate, 0.2g aluminum trichloride, 15g NH 4 Cl (0.28mol) 60g ground PCl 5 (0.26mol) and 600mL of 1,2,4-trichlorobenzene, stirred and protected by nitrogen, gradually heated up to 190 degrees, reacted for 5 hours, the reaction solution became viscous, cooled to 50 degrees, quickly filtered out insolubles, and added 350ml of filtrate n-heptane, to obtain a gel-mounted precipitate, which was centrifuged several times to obtain a linear chlorophosphazene product. Yield 48%, total preparation time 7 hours.

Embodiment 3

[0025] Put 0.3g calcium sulfate dihydrate, 0.2g p-toluenesulfonic acid, 20.9g NH 4 Cl (0.39mol) 60g ground PCl 5 (0.26mol) and 500mL chlorinated naphthalene, stirring and nitrogen protection, gradually warming up to 180 degrees, reacted for 5 hours, the reaction solution became viscous, cooled to 50 degrees, rapidly filtered out insolubles, and the filtrate was added with 400ml n-heptane to obtain Precipitate in glue, centrifuge several times to obtain the linear phosphazene product, the yield is 42%, and the preparation time is 7 hours in total.

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Abstract

The invention discloses a method for preparing linear chlorophosphoronitrile. Ammonium chloride, phosphorus pentachloride, a composite catalyst and a solvent are adopted as raw materials, and all thecomponents are added into a reactor to be mixed; under nitrogen protection, a reaction is carried out for 4-5 hours, and cooling is gradually carried out after the reaction is finished; undissolved substances are subjected to extraction filtration, the filtrate is added into normal heptane, centrifugation is carried out, and a gelatineous linear chlorophosphoronitrile product is obtained. According to the method, the two-step reaction is completed through one step of catalyzing, the technological process is simplified, and the reaction time of the whole process is shortened; energy consumptionis reduced, generated liquid waste is reduced, and compared with a previous synthetic method, the method is a more energy-saving, environment-friendly and efficient synthetic process.

Description

technical field [0001] The invention relates to a preparation method of linear polydichlorophosphazene, which belongs to the field of synthesis of phosphazene flame retardants. Background technique [0002] Linear polydichlorophosphazene (PDCP) is an important intermediate in the synthesis of substituted polyphosphazenes, and the Cl atom on the P atom of the main chain has strong reactivity, and can react with a variety of nucleophiles to prepare linear functionalized polyphosphazene. Through the side group functionalization reaction of PDCP, a large number of new structures and new materials have been synthesized, which are widely used in flame retardants, medical materials, special rubbers, low-temperature elastomers and other fields. □ [0003] At present, the main synthesis methods of PDCP include thermal ring-opening method of hexachlorocyclotriphosphazene fusion, catalytic thermal ring-opening method of hexachlorocyclotriphosphazene solution, and room temperature pol...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B21/098
CPCC01B21/0986C01P2002/82C01P2002/86
Inventor 朱宁肖学文侯进京白振华房林林刘彦余周生刚王艳辉
Owner JINAN TAIXING FINE CHEM
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