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Method for preparing and detecting crystallization II type ammonium polyphosphate

An ammonium polyphosphate, detection method technology, applied in the direction of phosphate, phosphorus oxyacid, chemical instruments and methods, etc., to achieve the effect of high accuracy and good reliability

Inactive Publication Date: 2005-06-22
ZHEJIANG RES INST OF CHEM IND CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The present invention will solve the problem of the method for producing crystalline type II ammonium polyphosphate that has not been reported so far, and provide the preparation method and detection method of the crystalline type II ammonium polyphosphate of the present invention

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  • Method for preparing and detecting crystallization II type ammonium polyphosphate

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Embodiment 1

[0025] Add phosphorus pentoxide 108kg, diammonium hydrogen phosphate 100kg, ammonium sulfate 1000g into 0.5m 3 In the reactor, mix for 10 minutes, then raise the temperature to 300°C, and melt at 10m 3 Ammonia gas is fed at a flow rate of / h, and the ammonia gas flow time is 1 hour, and then the ammonia flow rate is reduced to 3m 3 / h, the temperature is lowered to 250°C and then matured for 3 hours, the product obtained is 100% crystalline type II ammonium polyphosphate, the average degree of polymerization is 1313, and the thermal decomposition temperature is greater than 275°C (weight loss rate is less than 0.5%).

[0026] Preparation method embodiment 2

[0027] Add 225kg of phosphorus pentoxide, 210kg of diammonium hydrogen phosphate, and 2175g of melamine into the 1.0m 3 In the reactor, mix for 10 minutes, then raise the temperature to 300°C, melt at 20m 3 The flow rate of / h is passed through the ammonia gas, and the ammonia gas is passed for 1 ho...

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Abstract

The invention provides a process for preparing inorganic highly performance combustion inhibitor crystallization II type ammonium polyphosphate, which comprises selecting equal mol of phosphorus pentoxide and ammonium monohydric phosphate, under 150-350 deg. C, charging ammonium sulfate, melamine or ammonium hydrogen carbonate polycondensation agent, mixing, liquating, crystallizing, and disintegrating at the presence of ammonia gas atmosphere, thus obtaining crystallization II type polyphosphoric acid (APP-II). The method for detecting crystallization II type ammonium polyphosphate consists of measuring crystallization form of the APP-II through X-ray diffraction analysis, measuring polymerization degree of the APP-II through nuclear magnetic resonance method, measuring the decomposition temperature of the APP-II through heat weight / differential heat synchronization analytic method.

Description

technical field [0001] The invention relates to a preparation and detection method of ammonium polyphosphate, in particular to a preparation and detection method of crystalline type II ammonium polyphosphate. Background technique [0002] Ammonium polyphosphate (English name Ammonium Polyphosphate) is referred to as APP, and its molecular formula is (NH 4 ) n+2 P n o 3n+1 , when n is large, it can be approximated as (NH 4 PO 3 ) n , is a nitrogen-containing polyphosphate, white powder. From the X-ray pattern analysis, ammonium polyphosphate has five different crystal forms I-V. Among the five crystal forms, the crystalline states of types III and IV are unstable, and type V is stable, but a feasible manufacturing method has not yet been found. Therefore, Type I and Type II are generally used as flame retardants. Compared with type I and type II, the water resistance and heat resistance of type II are much better than type I. Due to the influ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/28C01C1/00G01N23/20G01N24/08G01N25/00
Inventor 楼芳彪陆凤英白瑞瑜姚巍杨箭
Owner ZHEJIANG RES INST OF CHEM IND CO LTD
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