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Preparation method of chlorophosphazene

A technology of chlorophosphazene and phosphorus pentachloride, which is applied in the field of preparation of chlorophosphazene, can solve the problems of ammonium chloride easy to absorb moisture, the scale of industrialization, the back suction of the tail gas device, and safety problems affecting the operation of the production device, etc., and achieve good industrialization Application prospects, increased reaction area, and the effect of saving reaction raw materials

Inactive Publication Date: 2017-11-24
DONGYING DAOYI BIOLOGICAL MEDICINE TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The moisture and particle size of ammonium chloride affect the reaction yield and product quality. Because crushing ammonium chloride is dangerous and ammonium chloride is very easy to absorb moisture, the expansion of industrial scale is limited to a certain extent; at the same time, when using hydrochloric acid tail gas During absorption, due to the inconstant amount of hydrogen chloride produced in the reaction process, the tail gas device will suck back, which will cause safety problems and affect the operation of the production device.

Method used

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  • Preparation method of chlorophosphazene
  • Preparation method of chlorophosphazene
  • Preparation method of chlorophosphazene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Add 830 g of chlorobenzene solution containing 208 g of phosphorus pentachloride into a 1 L glass-lined pressure reactor, and add 59 g of ammonium chloride (particle size: 170 μm, see Particle Size figure 1 ), add catalyst ferric chloride zinc oxide compound 2.2g, after the device is installed, connect the lye tail gas recovery device. Turn on stirring and heat. When the temperature rises to 100°C, control the heating rate, continue heating to 130°C, and keep this temperature for 5 hours. After the reaction was completed, the temperature was lowered, and the feed liquid was suction filtered. The organic layer was added with 650ml of water to stir and stratified, and the lower organic layer was added with 500ml of water to stir and stratified. Heptane recrystallization, get white solid 81.2g yield 70% (analysis triploid 72.9%, tetraploid 25.4%) Figure 6 )

Embodiment 2

[0035] Add 830 g of chlorobenzene solution containing 208 g of phosphorus pentachloride into a 1L glass-lined pressure reactor, add 59 g of ammonium chloride that was previously dried and pulverized, (see particle size for particle size 133.18 μm) figure 2 ) Add 2.2 g of catalyst ferric chloride zinc oxide compound, install the device and connect the alkali liquor tail gas recovery device. Turn on stirring and heat. When the temperature rises to 100°C, control the heating rate, continue heating to 130°C, and keep this temperature for 5 hours. After the reaction was completed, the temperature was lowered, and the feed liquid was suction filtered. The organic layer was added with 650ml of water to stir and stratified, and the lower organic layer was added with 500ml of water to stir and stratified. Heptane recrystallization, get white solid 92.8g yield 80% (analysis triploid 83.1%, tetraploid 16% HPLC detection chromatographic column: C18, mobile phase: acetonitrile detector w...

Embodiment 3

[0037] Add 830 g of chlorobenzene solution of 208 g of phosphorus pentachloride into a 1 L glass-lined pressure reactor, add 14.8 g of crushed and dried ammonium chloride (particle size 81.49 μm, see particle size image 3 ), add catalyst ferric chloride zinc oxide compound 2.2g, after the device is installed and leak test. Turn on the stirring and turn on the heating device. When the temperature rises to 100°C, control the heating rate. When the temperature rises to 130°C, keep it warm for 1 hour. When the pressure in the kettle is 0.1Mpa, the reaction kettle is cooled to 80-90°C and ammonia gas is introduced. The temperature rises and the ammonia is controlled. The speed of the gas keeps the temperature at 2° C. / min, and the feeding of ammonia gas is stopped when the amount of ammonia gas is 68 g. Control the heating rate, when the temperature rises to 130°C, keep it warm for 5 hours, after the reaction is completed, cool down, hydraulically filter the material, wash the so...

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Abstract

The invention provides a preparation method of chlorophosphazene. The preparation method comprises the following steps: introducing ammonia gas to react with hydrogen chloride to generate ammonium chloride, utilizing the ammonium chloride to substitute partial reaction raw material to react, and obtaining a phosphazene compound. According to the preparation method, the ammonia gas is introduced to react with the hydrogen chloride to generate the ammonium chloride which is used as a raw material, so that the complex treatment for absorbing the tail gas hydrogen chloride generated in the reaction can be avoided, and the reaction after-treatment procedures are simplified; the particle size of the ammonium chloride produced by this way is smaller, the reaction can be performed successfully, and not only is the yield high, but also the crushing step is omitted, so that the reaction treatment is simple, the safety is high, the cost is relatively low, and the yield is high.

Description

technical field [0001] The invention relates to the technical field of chemical industry, in particular to a preparation method of chlorophosphazene. Background technique [0002] Phosphazene compounds are a new type of inorganic-organic hybrid polymers with nitrogen and phosphorus atoms as the main chain structure and alternating single and double bonds. The inorganic main chain and organic chain of phosphazene compounds make them have both inorganic and organic characteristics, and have incomparable properties of traditional polymers. They are used in the manufacture of fireproof materials, engineering plastics, and medicine. The intermediate chlorophosphazene is the raw material for the synthesis of phosphazene compounds, and its structural formula is as follows: [0003] At present, the factors restricting the industrial production of the intermediate chlorophosphazene are the low yield, the highly corrosive hydrochloric acid absorption of the generated tail gas or the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6581
CPCC07F9/65815C07F9/65817
Inventor 宋伟国
Owner DONGYING DAOYI BIOLOGICAL MEDICINE TECH CO LTD
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