Process for producing in-situ modified nano-magnesium hydroxide by taking phosphate tailings as raw materials

A nano-magnesium hydroxide and in-situ modification technology, which is applied in the field of waste resource utilization and functional nanomaterials, can solve the problems of environmental damage and achieve the effects of reducing energy consumption, simple process and low production cost

Inactive Publication Date: 2015-04-22
WUHAN INSTITUTE OF TECHNOLOGY +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0012] The purpose of the present invention is to provide a process for producing in-situ modified nano-magnesium hydroxide using phosphorus tailings as raw material. The utilization rate of magnesium in phosphorus tailings is more than 95%, which effectively solves the problem of phosphorus tailings accumulation and environmental damage. Comprehensive problems, improve the comprehensive utilization rate of magnesium resources associated with phosphate ore, and realize the closed cycle of process wastewater; the surface modified nano-magnesium hydroxide particles produced by this process have uniform size distribution, and have good interfacial adhesion in the polymer matrix. Good knot and dispersion

Method used

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  • Process for producing in-situ modified nano-magnesium hydroxide by taking phosphate tailings as raw materials

Examples

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Effect test

Embodiment 1

[0044] Put 52 kg of phosphorus tailings obtained from flotation into the acidolysis reactor, add 470 liters of water and stir to mix evenly. After reaching the preset temperature of 25°C, slowly add 29 liters of 98wt% sulfuric acid to react. After reacting for 2 hours, filter and wash For solid-liquid separation; add 0.347 liters of H 2 o 2 Oxidation, use ammonia water to control the pH of the filtrate to 6.7, and obtain a refined magnesium sulfate solution after removing impurities; add the silane coupling agent KH-570 and the dispersant polyethylene glycol to the refined magnesium sulfate solution, and fully stir for 2.5 hours; move into the crystallization In the reactor, the temperature of the solution is controlled at 25°C, and ammonia gas is slowly introduced for 1.5 hours. After the reaction, the final pH value is 10.7, aged at a constant temperature of 30°C for 20 minutes, filtered, washed, and dried to obtain in-situ modified nano-hydroxide Magnesium products.

Embodiment 2

[0046] Put 104 kg of phosphorus tailings obtained from flotation into the acidolysis reactor, add 470 liters of water and stir to mix evenly. After reaching the preset temperature of 35°C, slowly add 29 liters of 98wt% sulfuric acid to react. After reacting for 2 hours, filter and wash Carry out solid-liquid separation; add 0.694 liters of H 2 o 2 Oxidation, use ammonia water to control the pH of the filtrate to 6.5, remove impurities to obtain a refined magnesium sulfate solution; add the silane coupling agent KH-560 and dispersant sodium polyphosphate to the refined magnesium sulfate solution, and fully stir for 3 hours; move into the crystallization In the reactor, the temperature of the solution is controlled at 35°C, and ammonia gas is slowly introduced for 2 hours. After the reaction, the final pH value is 11, aged at a constant temperature of 45°C for 30 minutes, filtered, washed, and dried to obtain in-situ modified nano-hydroxide Magnesium products.

Embodiment 3

[0048] Put 36.5 kg of phosphorous tailings obtained from flotation into the acidolysis reactor, add 440 liters of water and stir and mix evenly. After reaching the preset temperature of 45°C, slowly add 60 liters of 98wt% sulfuric acid to react. After reacting for 3 hours, filter and wash Carry out solid-liquid separation; add 0.243 liters of H 2 o 2 Oxidation, use ammonia water to control the pH of the filtrate to 6.5, and remove impurities to obtain a refined magnesium sulfate solution; add the silane coupling agent KH-550 and the dispersant polyethylene glycol to the refined magnesium sulfate solution, and fully stir for 2.5 hours; move into the crystallization In the reactor, the temperature of the solution is controlled at 55°C, and ammonia gas is slowly introduced for 2 hours. After the reaction, the final pH value is 10.5, aged at a constant temperature of 50°C for 40 minutes, filtered, washed, and dried to obtain in-situ modified nano-hydroxide Magnesium products.

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Abstract

The invention discloses a process for producing in-situ modified nano-magnesium hydroxide by taking phosphate tailings as raw materials. The process comprises the following steps: putting the phosphate tailings obtained by flotation into an acidolysis reactor, reacting for a certain period of time, and then filtering; adding filtrate into an impurity removal reactor, firstly adding an oxidant for oxidation, further adding an alkaline compound, controlling the pH value, filtering a precipitate, then adding the filtrate, a silane coupling agent and a dispersant into an in-situ modification reactor, stirring for a period of time, then adding into a crystallization reactor, introducing ammonia gas, and performing crystallization and precipitation reaction to obtain surface-modified nano-magnesium hydroxide; and producing the filtrate which is rich in free ammonia after crystallization and filtration, obtaining the ammonia gas by air stripping, returning the ammonia gas into the crystallization working section, crystallizing a liquid phase to remove a large amount of ammonium sulfate, and then circulating to the acidolysis reaction process step, thereby realizing closed-loop circulation of wastewater of the process. Surface-modified nano-magnesium hydroxide produced by an in-situ modification method has good interfacial adhesion property and dispersivity in a polymer matrix and can be widely applied to the fields of plastics, coatings, environmental friendliness and the like.

Description

technical field [0001] The invention belongs to the field of resource utilization of waste and functional nanometer materials, and in particular relates to a process for producing in-situ modified nano magnesium hydroxide using phosphorus tailings as raw materials. Background technique [0002] Phosphate rock is the main fertilizer required for global agricultural production—the raw material of phosphate fertilizer, an important guarantee for global food production; it is also the raw material for the production of fine phosphorus chemical products. At present, my country has developed into a major country in the world's phosphate rock, phosphate fertilizer and phosphorus chemical industries. The development and utilization of phosphate rock resources has an important influence and role in the development of the world's economy and society. More than 90% of the phosphate rock grade in my country is lower than 26%, with an average grade of about 17%. With the continuous expl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F5/14B82Y30/00B09B3/00
CPCC01F5/14B09B3/00
Inventor 刘生鹏丁一刚盛昌和许莉莉吴梦胡仙林龙秉文邓伏礼
Owner WUHAN INSTITUTE OF TECHNOLOGY
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