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Process for producing crystallization type II branched-chain poly-ammonium phosphate

A branched-chain ammonium polyphosphate and crystallization technology, which is applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve problems such as high investment, high pollution, and high energy consumption, and achieve good reliability, simple raw materials, and thermal stability good sex effect

Inactive Publication Date: 2011-01-19
EAST CHINA UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Phosphorus pentoxide has strong hygroscopicity and reactivity, so it will be dangerous to the human body
And yellow phosphorus, P 2 o 5 , Thermal phosphoric acid is a "four high" product of high energy consumption, high pollution, high investment, and high cost. Gradually restricting thermal phosphoric acid is an inevitable requirement for energy conservation, emission reduction, and sustainable development of resources

Method used

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  • Process for producing crystallization type II branched-chain poly-ammonium phosphate
  • Process for producing crystallization type II branched-chain poly-ammonium phosphate
  • Process for producing crystallization type II branched-chain poly-ammonium phosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Add 200L of refined phosphoric acid (85%) into the reactor and raise the temperature to 250°C. During this period, it is best to operate under negative pressure and keep stirring, so as to remove a large amount of water from steaming, or to continuously replace with air to remove water; reach 250 After ℃, gradually add 17.688kg of urea within half an hour and stir, and continuously remove the released gas. After adding urea, add 46.431kg of melamine at 240°C to 250°C at one time and stir, gradually increasing the temperature. When the temperature rises to 300°C, start timing the heat preservation reaction for half an hour, gradually increase the stirring power, and remove the released gas. After half an hour, feed ammonia into the reaction period with a flow rate of 10m 3 / h, the product is initially solidified after a few minutes. The semi-finished products are all transferred to the broken reactor which has been preheated to 250°C. After the transfer, pass the ammo...

Embodiment 2

[0034] In this embodiment, the heat preservation reaction is at 310° C. for half an hour; after turning into crushing reaction gas, ammoniation is passed through ammonia at 310° C. for one hour, and the rest of the operations are the same as in Example 1. 99% of the obtained product is type II ammonium polyphosphate, the average degree of polymerization is 1286, and the 1% weight loss temperature is greater than 275° C. (the weight loss rate is less than 0.5%).

Embodiment 3

[0036] In the embodiment, the heat preservation reaction is at 320° C. for half an hour; after being transferred to the crushing reactor, the ammonification is carried out at 320° C. for 1 hour, and the rest of the operations are the same as in Example 1. The obtained product is a mixed ammonium polyphosphate of type I and type II, with an average degree of polymerization of 1112 and a 1% weight loss temperature of less than 275°C (weight loss rate of less than 0.5%).

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Abstract

The invention discloses a preparation method of crystal II-shaped branched chain ammonium polyphosphate, which comprises the following steps: selecting refined phosphoric acid as main raw material, as well as carbamide, trimeric cyanamide, melam, melem or a mixture thereof as a condensing agent; reacting for half an hour at the temperature of 150 to 320 DEG C; introducing ammonia; and obtaining the crystal II-shaped branched chain ammonium polyphosphate after the ammonia is aminated, cured, crystallized and crushed. The product the apparent viscosity which is greatly larger than that of the prior industrial product with the average polymerization degree up to 1000 and the thermal decomposition temperature which is larger than 300 DEG C, and can be used as a flame retardant with high efficiency, low mammalian toxicity and non-drip. The invention has the advantages of simplicity, good reliability and high accuracy rate.

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 branched-chain 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 III and IV are unstable, and V is stable, but no feasible manufacturing method has been found yet. Therefore, generally type I and type II are used as flame retardants. Among them, the water resistance and heat resistance of type II are much better than that of type I. Due to the influence of its own physical properties, the applicatio...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/40
Inventor 刘够生赵宏宇盛勇梅胜明徐仟伍于建国
Owner EAST CHINA UNIV OF SCI & TECH
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