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Preparation method of crystallization II-type ammonium polyphosphate with high degree of polymerization

A high degree of polymerization, ammonium polyphosphate technology, applied in chemical instruments and methods, single crystal growth, phosphorus compounds, etc., can solve problems such as the preparation method of APP with a high degree of polymerization without crystal II

Inactive Publication Date: 2009-09-23
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] Using phosphate as the starting material, such as diammonium hydrogen phosphate as the starting material, and urea as the condensation agent, at present, only crystalline type I APP products w

Method used

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  • Preparation method of crystallization II-type ammonium polyphosphate with high degree of polymerization
  • Preparation method of crystallization II-type ammonium polyphosphate with high degree of polymerization
  • Preparation method of crystallization II-type ammonium polyphosphate with high degree of polymerization

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Diammonium hydrogen phosphate 50kg, urea 4.4kg, melamine 8.2kg, diammonium hydrogen phosphate is first added to the reactor, and the temperature is raised to 160°C. Ammonia gas, or continuously replace with air to discharge water; after reaching 180°C, gradually add urea and stir within half an hour, and continuously discharge the gas released by the reaction. After adding urea, add melamine at 200°C to 250°C at one time and stir, then gradually raise the temperature. Start timing when it rises to 260°C, keep the temperature for 30 minutes, gradually increase the stirring power, and discharge the gas released by the reaction. After 60 minutes, feed ammonia into the reactor with a flow rate of 6m 3 / h, the product is initially solidified after 10 minutes, cooled to 210 ° C, and then matured for 1 hour, the ammonia gas flow rate is 2m 3 / h. 99.0% of the obtained product is crystalline type II ammonium polyphosphate, the average degree of polymerization is 1766, and the...

Embodiment 2

[0030] In this example, the heat preservation reaction temperature is 280°C, and the time is 60 minutes. The rest of the operations are the same as in Example 1, and 99% of the obtained product is crystalline type II ammonium polyphosphate, the average degree of polymerization is 1836, and the 1% thermal weight loss temperature is greater than 275 ℃ (weight loss rate is less than 0.5%).

Embodiment 3

[0032] In this example, the heat preservation reaction temperature is 300°C, and the time is 40 minutes. The remaining operations are the same as in Example 1, and 99% of the obtained product is Type II ammonium polyphosphate, with an average degree of polymerization of 1917, and a temperature of 1% thermal weight loss greater than 285°C (The weight loss rate is less than 0.5%).

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Abstract

The invention relates to a preparation method of crystallization II-type ammonium polyphosphate with high degree of polymerization, the specific steps are as follows: taking diammonium phosphate as original material, taking urea and (or) melamine as condensation agent, reacting for 30-120 minutes in the temperature range of 120-320 DEG C, introducing ammonia gas to aminate for 30-100 minutes till curing and crystallization, then crushing to obtain crystallization II-type fork chain ammonium polyphosphate. The invention has the advantages that: the apparent viscosity of the product is much larger than that of the existing industrial product with average degree of polymerization being up to 1000, the degree of polymerization is generally 1500-2000, the thermolabile temperature is more than 275 DEG C, and the water solubility is less than 0.25g/100ml.

Description

【Technical field】 [0001] The invention relates to the technical field of ammonium polyphosphate preparation, in particular to a method for preparing crystalline type II ammonium polyphosphate with a high degree of polymerization. 【Background technique】 [0002] Ammonium polyphosphate (referred to as APP) molecular formula (NH 4 ) n+2 P n o 3n+1 , the phosphorus content is 30-32%, and the nitrogen content is 14-16%. Hydrogen halides are not produced. APP has good thermal stability, the product is close to neutral, and can be mixed with other flame retardants. It has good dispersibility, smoke elimination, low toxicity, and is safe to use. Therefore, it is widely used in the preparation of intumescent flame retardants, fireproof coatings, Fireproof treatment of cables, flame retardancy of rubber and plastic products. [0003] According to the degree of polymerization, APP can be divided into short chain (n=10~20), also known as water-soluble APP; long chain (n>20), al...

Claims

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Application Information

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IPC IPC(8): C01B25/40C30B29/14
Inventor 刘够生何志俊于建国
Owner EAST CHINA UNIV OF SCI & TECH
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