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Method for performing phosphorite magnesium-removal and preparing flame retardant by organic acid

A flame retardant and organic acid technology, applied in the field of phosphorus chemical industry, can solve the problems of unrealized industrial application, high cost, and inability to effectively solve the recycling and utilization of magnesium removal waste liquid, and achieve convenient operation, high economic value, and short process Effect

Active Publication Date: 2017-07-28
云南三磷科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] In the Chinese patent database, there are some patents related to the demagnesization of phosphate rock and the recycling of demagnesium waste liquid, such as CN 102776267 A "A kind of demagnesization of phosphate rock and preparation of MgHPO 4 ·3H 2 O Method", CN 102674278 A "A Method for Pretreating Phosphate Rock Using Titanium White Waste Acid", CN 1050170 A "Method for Removing Magnesium from Phosphate Rock", CN 103071580 A "A Method for Demagnesizing Phosphate Rock" , CN 102115819A "Method for Recovering Magnesium from Medium and Low Grade High Magnesium Phosphate Rock", CN102583302 A "Technology for Removing Magnesium from Extracted Phosphate", etc. Although these methods have their own characteristics, they all have high cost and cannot effectively solve the waste of magnesium removal. Due to problems such as liquid recycling and utilization, industrial application has not been realized

Method used

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  • Method for performing phosphorite magnesium-removal and preparing flame retardant by organic acid
  • Method for performing phosphorite magnesium-removal and preparing flame retardant by organic acid

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Chemical composition of a phosphate ore: P 2 o 5 23.84%, MgO4.6%, CaO34.08%, SiO 2 9.39%.

[0038] Such as figure 1 A method for utilizing organic acid to remove magnesium from phosphate rock and prepare a flame retardant comprises the following steps:

[0039] 1) Weigh 180g of diethylenetriaminepentamethylenephosphonic acid, dilute it to a solution with a mass fraction of 28%, place the solution of diethylenetriaminepentamethylenephosphonic acid in a clean 500mL three-necked bottle, and use ammonia water Adjust its pH=1.5. Weigh 25g of the raw ore powder, and gradually add the raw ore powder into the three-necked flask. Start stirring after adding ore, and stir and react at 80°C for 20 minutes. After the reaction is completed, heat-preserve and filter at 60°C to obtain demagnesium filtrate and phosphorus concentrate. Wash the phosphorous concentrate with 100mL distilled water three times, and combine the first water wash with the demagnesium filtrate.

[0040] ...

Embodiment 2

[0047] Chemical composition of a phosphate ore: P 2 o 5 24.38%, MgO4.2%, CaO35.11%, SiO 2 8.87%.

[0048] A method for utilizing organic acid to remove magnesium from phosphate rock and prepare a flame retardant, comprising the following steps:

[0049] 1) Weigh 160g of diethylenetriaminepentamethylenephosphonic acid, dilute it to a solution with a mass fraction of 45%, place the solution of diethylenetriaminepentamethylenephosphonic acid in a clean 500mL three-necked bottle and adjust it with ammonia water pH=2. Weigh 25g of the raw ore powder, and gradually add the raw ore powder into the three-necked flask. Start stirring after adding ore, and stir and react at 60°C for 40 minutes. After the reaction is completed, heat-preserve and filter at 60°C to obtain demagnesium filtrate and phosphorus concentrate. Wash the phosphorous concentrate with 100mL distilled water three times, and combine the first water wash with the demagnesium filtrate.

[0050] 2) Place the demagn...

Embodiment 3

[0057] Chemical composition of a phosphate ore: P 2 o 5 24.74%, MgO3.8%, CaO35.48%, SiO 2 10.31%.

[0058] A method for utilizing organic acid to remove magnesium from phosphate rock and prepare a flame retardant, comprising the following steps:

[0059] 1) Weigh 155g of diethylenetriaminepentamethylenephosphonic acid, dilute it to a solution with a mass fraction of 50%, place the diethylenetriaminepentamethylenephosphonic acid solution in a clean 500mL three-necked bottle and adjust it with ammonia water pH=2.5. Weigh 25g of the raw ore powder, and gradually add the raw ore powder into the three-necked flask. Start stirring after adding ore, and stir and react at 70°C for 50 minutes. After the reaction is completed, heat-preserve and filter at 60°C to obtain demagnesium filtrate and phosphorus concentrate. Wash the phosphorous concentrate with 100mL distilled water three times, and combine the first water wash with the demagnesium filtrate.

[0060] 2) Place the demagn...

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Abstract

The invention relates to a method for performing phosphorite magnesium-removal and preparing flame retardant by organic acid, wherein the method includes steps of mixing low-grade raw ore with diethylenetriaminepenta acid to perform acidolysis and phosphoritemagnesium-removal reaction; after preserving temperature and separating solid from fluid, acquiring phosphorus concentrate and magnesium-removal waste liquid; adjusting pH value of magnesium-removal waste liquid to 4-7, adding equal volume of ethanol solution to perform aging treatment; separating solid from fluid to acquire initial product and fluid phase of the flame retardant; performing depressurizing distillation on the fluid phase twice and acquiring the recycled ethanol and secondary product of the flame retardant; at last, compounding the initial product and secondary product of the flame retardant with tetramethylolmethane and tripolycyanamide, and acquiring the two flame-retardant products with excellent performances. After being treated by middle and low grade phosphorites, the low-magnesium content phosphorus concentrate is acquired; the recycle of magnesium-removal waste liquid is realized. The method is environment-friendly and economic.

Description

technical field [0001] The invention relates to the technical field of phosphorus chemical industry, in particular to a method for using organic acid to remove magnesium from phosphate rock and prepare a flame retardant. Background technique [0002] my country is rich in phosphate rock resources, but most of them are low-grade collophosite that are difficult to select, and are generally associated with dolomite minerals, and contain a large amount of impurities. Magnesium in phosphate rock is one of the most important impurities, and most of the magnesium impurities are in the form of dolomite (MgCO 3 ·CaCO 3 ) in the form of phosphate rock acid hydrolysis and calcium sulfate crystallization will have adverse effects. In the production process of wet-process phosphoric acid, impurities such as Mg, Fe, K, and Na in phosphate rock are brought into phosphoric acid. These harmful impurities not only affect the production of wet-process phosphoric acid, but also have a signifi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08K3/32C08K5/053C08K5/3492C08L23/12C01B25/01
CPCC01B25/01C08K3/32C08K5/053C08K5/34922C08L2201/02C08L23/12
Inventor 张华丽潘志权吴汉军梁欢
Owner 云南三磷科技有限公司
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