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Method for preparing melamine polyphosphate by recycling phosphoric acid waste liquid

A technology of melamine polyphosphate and acid waste liquid is applied in the preparation of urea derivatives, chemical instruments and methods, preparation of organic compounds, etc. The effect of low implementation cost, obvious economic and environmental benefits, and simple method

Active Publication Date: 2020-05-08
SHENZHEN SHENTOU ENVIRONMENT TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Zhang Licai disclosed a method for preparing feed-grade calcium hydrogen phosphate using waste etching acid containing phosphoric acid as a raw material in "The Process of Preparing Feed-Grade Calcium Hydrogen Phosphate from Phosphoric Acid-Containing Etching Waste Acid". The added value of hydrogen calcium is relatively low
Bi Yafan disclosed in "Preparation of Waste Etching Solution and Low-grade Phosphate Rock as Raw Material Phosphate Compound Fertilizer" a method for preparing phosphorus compound fertilizer using aluminum etching waste liquid and low-grade phosphate rock as raw material, but the method used The concentration of various harmful metal cations except aluminum and copper in the aluminum etching waste liquid must meet the standard of acid for fertilizer production, which limits the scope of application of this method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

no. 1 approach

[0037] The first embodiment of the present invention provides a method for recycling phosphoric acid-containing waste liquid, which treats and processes the phosphoric acid-containing waste liquid into a urea phosphate product. This first embodiment comprises the following steps:

[0038] S100: obtaining waste liquid containing phosphoric acid;

[0039] S101: removing solid impurities and / or suspended matter in the phosphoric acid waste liquid to obtain a clear phosphoric acid waste liquid;

[0040] S102: Evaporating the phosphoric acid-containing waste liquid supernatant to obtain a phosphoric acid-containing waste liquid concentrate;

[0041] S103: cooling the phosphoric acid waste liquid concentrate;

[0042] S104: adding a certain amount of urea to the concentrated phosphoric acid waste liquid to obtain a first reaction liquid;

[0043] S105: After the reaction has been carried out for a period of time, cool and crystallize to obtain crystals and mother liquor containin...

no. 2 approach

[0056] The second embodiment of the present invention provides a method for recycling phosphoric acid-containing waste liquid, processing the waste liquid containing high-concentration phosphoric acid into urea phosphate, and further preparing a nitrogen-phosphorus flame retardant containing melamine polyphosphate This second embodiment of the product comprises the following steps:

[0057] S200: obtaining waste liquid containing phosphoric acid;

[0058] S201: removing solid impurities and / or suspended matter in the phosphoric acid-containing waste liquid to obtain a phosphoric acid-containing waste liquid clear liquid;

[0059] S202: Evaporate the phosphoric acid-containing waste liquid supernatant to obtain a phosphoric acid-containing waste liquid concentrate;

[0060] S203: cooling the phosphoric acid waste liquid concentrate;

[0061] S204: adding a certain amount of urea to the concentrated phosphoric acid waste liquid to obtain a first reaction liquid;

[0062] S205...

Embodiment 1

[0077] Obtain a kind of spent aluminum etching acid A from a certain manufacturer, and the relative density of the spent aluminum etching acid A is 1.11. After analysis and testing, the total phosphorus content in the aluminum etching waste acid A is 61g / L, the aluminum content is 3.5g / L, the iron content is 8mg / L, the copper content is 5mg / L, the zinc content is 7mg / L, and the lead content is 7mg / L. The content is 0.02mg / L. The aluminum etching spent acid A contains about 0.3% by weight of acetic acid and about 0.05% by weight of nitric acid. The method for recycling this aluminum etching waste acid A may further comprise the steps:

[0078] S601: Take 1000 ml of the spent aluminum etching acid A, filter to remove solid impurities and suspended matter in the spent aluminum etching acid A, and obtain a waste acid clear liquid.

[0079] S602: Evaporate the waste acid clear liquid obtained in step S601 to obtain a waste acid concentrate, and the relative density of the waste a...

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Abstract

The invention provides a method for preparing melamine pyrophosphate. The method mainly comprises the following steps: firstly, evaporating a phosphorus-containing acid waste liquid to obtain a phosphorus-containing acid waste liquid concentrated solution; secondly, adding urea into the phosphorus-containing acid waste liquid concentrated solution to obtain a first reaction solution; thirdly, carrying out cooling and crystallizing on the reacted first reaction solution to obtain a crystal containing urea phosphate and a mother solution; fourthly, diluting the filtrated mother solution and then adding melamine to obtain a second reaction solution; filtering the reacted second reaction solution to obtain a reaction intermediate; fifthly, carrying out washing, drying and calcining treatment on the reaction intermediate to obtain the melamine polyphosphate. The invention also provides a recycling method for the phosphorus-containing acidic waste liquid. The method provided by the invention is simple and feasible and large-scale production can be easily realized; in addition, an obtained product has higher added value and higher economic and environmental benefits.

Description

technical field [0001] The invention relates to a method for recycling industrial wastewater, in particular to a method for recycling phosphorus-containing acidic waste liquid. Background technique [0002] In recent years, my country has become the world's largest display production base. The etching process is widely used in the processing of liquid crystal display devices and organic light emitting display devices used as flat panel displays. The etching solution used in the etching process usually contains more than 50% by weight of phosphoric acid, and also includes a certain amount of nitric acid and acetic acid as stabilizers. When the etching solution is consumed or its purity decreases during the etching process, it needs to be replaced, thereby generating a large amount of phosphoric acid-containing etching waste. In 2012, the output of industrial etching waste liquid in my country was about 2 million tons, with an annual growth rate of more than 5%. Since the d...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D251/54C07C273/02C07C275/02C08K5/3492
CPCC07C273/02C07D251/54C08K5/34922
Inventor 周兆安唐瑜钟徐丽阳陈志传慎义勇米永红
Owner SHENZHEN SHENTOU ENVIRONMENT TECH CO LTD