Preparation of nano magnesium hydrate

A technology of nano-magnesium hydroxide and magnesium hydroxide, which is applied in the preparation of ultrasonic-assisted synthesis of nano-powder and the field of ultrasonic-assisted synthesis of nano-magnesium hydroxide, can solve the problems of difficult operation, long reaction time, long ultrasonic time, etc. The particle size distribution is uniform, the further growth is inhibited, and the product dispersibility is good.

Inactive Publication Date: 2009-03-04
SHENZHEN GRADUATE SCHOOL TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The equipment investment of this method is large, and the magnesium hydroxide generated by the reaction is easy to deposit in the gap between the fillers and block the packed bed.
Chinese patent CN1542036A uses soluble magnesium salt and soluble alkali as raw materials. Under the action of polymer protective agent, magnesium hydroxide nanopowder is prepared by forced emulsification and precipitation through a high-shear homogeneous emulsifier. The aging time after the reaction is long Up to 12 hours, the reaction time is too long
Chinese patent CN1982410A combines precipitation synthesis and hydrothermal treatment to prepare magnesium hydroxide by precipitation method to prepare flaky nano-magnesium hydroxide. The reaction and hydrothermal treatment temperatures are as high as 160°C and 180°C respectively. The reaction conditions of this method are harsh and difficult to operate. Difficult, difficult to industrialize production
This patent uses ultrasonic waves to vibrate the pre-prepared magnesium hydroxide colloid, which has the function of ultrasonic dispersion to prevent agglomeration, but the ultrasonic time is too long, especially the solvent is removed by evaporation, which makes the patented method have a long production cycle, high energy consumption and high cost. , is not conducive to the promotion of industrialization

Method used

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  • Preparation of nano magnesium hydrate
  • Preparation of nano magnesium hydrate
  • Preparation of nano magnesium hydrate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] 28.5g MgCl 2 ·6H 2 O and 0.86g of polyethylene glycol were dissolved in deionized water, and stirred to form a 100ml magnesium salt solution; in addition, 11.2g of NaOH was also dissolved in deionized water to form a 100ml lye solution. First add the magnesium salt solution into a 250ml three-necked flask, start the stirrer, and control the rotation speed to 600rpm; at the same time, turn on the ultrasonic wave, control the ultrasonic frequency to 59KHz, and the ultrasonic power to 100W. Then slowly drop an aqueous sodium hydroxide solution into the three-necked flask, react at 25° C. to obtain a magnesium hydroxide suspension, and then ultrasonically age the magnesium hydroxide suspension for 10 minutes. The suspension was filtered, washed with deionized water until no chloride ions were detected, and the filter cake was dried at 110° C. for 4 hours to obtain flaky magnesium hydroxide powder with an average particle size of 70 nm.

Embodiment 2

[0020] 28.5g MgCl 2 ·6H 2 O and 0.57g of polyvinyl alcohol were dissolved in deionized water and stirred to form a 100ml magnesium salt solution; in addition, 15.7g of KOH was also dissolved in deionized water to form a 100ml lye solution. First add the magnesium salt solution into a 250ml three-neck flask, start the stirrer, and control the rotation speed at 500rpm; at the same time, turn on the ultrasonic wave, control the ultrasonic frequency to 33KHz, and the ultrasonic power to 100W. Then slowly drop an aqueous sodium hydroxide solution into the three-necked flask, react at 25° C. to obtain a magnesium hydroxide suspension, and then ultrasonically age the magnesium hydroxide suspension for 15 minutes. The suspension was filtered, washed with deionized water until no chloride ions were detected, and the filter cake was dried at 120° C. for 3 hours to obtain flaky magnesium hydroxide powder with an average particle size of 90 nm.

Embodiment 3

[0022] 28.5g MgCl 2 ·6H 2 O and 1.14g of zinc stearate were dissolved in deionized water and stirred to form 100ml of magnesium salt solution; 44.0ml of ammonia water was also dissolved in deionized water to form 100ml of lye. First add the magnesium salt solution into a 250ml three-necked flask, start the stirrer, and control the rotation speed to 700rpm; at the same time, turn on the ultrasonic wave, control the ultrasonic frequency to 80KHz, and the ultrasonic power to 100W. Then slowly drop an aqueous sodium hydroxide solution into the three-necked flask, react at 25° C. to obtain a magnesium hydroxide suspension, and then ultrasonically age the magnesium hydroxide suspension for 8 minutes. The suspension was filtered, washed with deionized water until no chloride ions were detected, and the filter cake was dried at 100°C for 6 hours to obtain flaky magnesium hydroxide powder with an average particle size of 50 nm.

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Abstract

The invention relates to a preparation method of nano-sized magnesium hydroxide, which is characterized in that a soluble magnesium salt solution and soluble lye which are added with a dispersant react in a reactor which is put in an ultrasonic tank and provided with a stirrer to obtain magnesium hydrate suspension; the magnesium hydrate suspension is processed through ultrasonic ageing at room temperature; the magnesium hydrate which is processed through ageing is dried through heating to obtain nano-sized magnesium hydroxide powders after being filtered and washed. The ultrasonic wave which is exerted during the reaction process promotes the nucleation, inhibits crystal nucleus growth velocity, and controls the size and the distribution of particles; the ultrasonic cavitation avoids the occurrence of aggregate phenomenon, and increases the uniformity and the dispersibility of nano particles; the thermal effect of the ultrasonic wave increases the crystallinity degree of the nano particles and shortens the ageing time of samples. Therefore, the preparation method has the advantages of simple technology, short production period, mild production conditions, good product dispersibility, and even particle distribution.

Description

technical field [0001] The invention belongs to a nano powder preparation process, in particular to a preparation method for ultrasonic-assisted synthesis of nano-powder, in particular to an ultrasonic-assisted synthesis method for nano magnesium hydroxide. Background technique [0002] Mg(OH) 2 As an important inorganic flame retardant, it is one of the most cost-effective flame retardants. It has the characteristics of high decomposition temperature, high thermal stability, non-toxic, smoke-free and smoke-suppressive, and is an environmentally friendly and green flame retardant. Moreover, most of the properties are better than aluminum hydroxide flame retardants, which cater to the needs of non-halogenated, low-toxicity, and smoke-suppressing flame retardants in the 21st century, and have achieved rapid development. But ordinary Mg(OH) 2 It is used for flame retardancy of polymers, the flame retardancy efficiency is low, and the compatibility with the matrix is ​​poor. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F5/20C01F5/22B82B3/00
Inventor 万军喜唐国翌
Owner SHENZHEN GRADUATE SCHOOL TSINGHUA UNIV
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