CN103420342A

CN103420342A - Preparation method for nano magnesium peroxide

Info

Publication number: CN103420342A
Application number: CN2013103327504A
Authority: CN
Inventors: 李咏梅; 王婕
Original assignee: Tongji University
Current assignee: Tongji University
Priority date: 2013-08-01
Filing date: 2013-08-01
Publication date: 2013-12-04
Anticipated expiration: 2033-08-01
Also published as: CN103420342B

Abstract

The invention relates to a preparation method for nano magnesium peroxide. Using magnesium oxide, ammonium chloride, and oxydol with mass percentage of 30% according to the mass ratio of 1:(1.5-2.5):(30-40); dissolving the magnesium oxide into deionized water and grinding into magnesium oxide size mixture with the mass percentage of 3-4%; dissolving the ammonium chloride into the oxydol, and stirring and slowly adding into the ground magnesium oxide size mixture; keeping the reaction under the continuous stirring at 500 r/min for 3-4 h to obtain white precipitate mixed solution; filtering the white precipitate mixed solution to obtain a wet filter cake; performing freezing vacuum drying at -80 DEG C to obtain a target product of nano magnesium peroxide powder with particle size of 20 nm, good dispersity, and purity higher than 50%. The method is simple to operate and is suitable for large-scaled industrialized production.

Description

A kind of preparation method of nanometer Magnesium peroxide

Technical field

The present invention relates to a kind of preparation method of nanometer Magnesium peroxide, belong to chemical industry synthetic method technical field.

Background technology

Magnesium peroxide, molecular formula is MgO ₂, be a kind of solid inorganic superoxide.Outward appearance is white powder, and odorless, tasteless is water insoluble, is soluble in diluted acid.More stable under normal temperature, heating or understand the slow and stable oxygen that discharges while contact with malaria, produce hydrogen peroxide after being dissolved in acid.Magnesium peroxide is nontoxic, and therefore environmentally safe is used widely at numerous areas such as medical science, textile industry, mining industry, agriculturals.

At field of environment protection, Magnesium peroxide can be used as oxygen-releasing compound and is applied in situ chemical oxidation, a kind of raw material of repairing as soil, settling, surface water and groundwater pollution.The foreign applications Magnesium peroxide carries out environment remediation comparison successful story and comprises the organic compound such as the virus removed in earth's surface and underground water and petroleum hydrocarbon, benzene,toluene,xylene, the improvement highway drainage pollutes, and suppresses the growth of plant plankton with purified water source etc.Other is usually used in the inorganics of in situ chemical oxidation to compare calcium peroxide, sodium carbonate, potassium permanganate, hydrogen peroxide etc., and Magnesium peroxide has the longer oxygen release time, the unit mass oxygen release amount of less pH value fluctuating range and Geng Gao.But because the raw materials cost of synthetic use is higher, the reasons such as sintetics purity lower (being applied to the Magnesium peroxide purity of environment remediation generally below 20%), Magnesium peroxide is not widely used.And nano level product has higher specific surface area and dispersiveness, be conducive to improve speed of reaction, save reaction cost, therefore, preparing nano level Magnesium peroxide can bring into play product performance better, widens its Application Areas.

Chinese patent CN1370736A has announced a kind of preparation method of Magnesium peroxide, in Dilute Hydrogen Peroxide Solution, add pulverous magnesium oxide, add organic phosphoric acid and salt thereof as stablizer simultaneously, make the wet product Magnesium peroxide after reaction, then obtain by drying the magnesium peroxide powder that content is greater than 30%.Chinese patent CN101613088A has announced a kind of method of preparing magnesium peroxide by non-emulsion process, using organic phosphoric acid and salt thereof or inorganic phosphate and salt thereof as stablizer, take solubility magnesium salts, superoxol, alkali is raw material, in water solution system, hierarchy of control temperature is reacted 2-10h under 10-30 ℃, and reaction product after filtration, washing, drying obtain the magnesium peroxide powder that content is greater than 40%.Equal not mentioned product cut size problem in the preparation method of above-mentioned Magnesium peroxide, therefore, be necessary to strengthen the research to nano level Magnesium peroxide preparation method.

Summary of the invention

The purpose of this invention is to provide that a kind of purity is higher, particle diameter evenly, the preparation method of the nanometer Magnesium peroxide of good dispersity.

In order to reach purpose of the present invention, it is raw material that the hydrogen peroxide of magnesium oxide and mass concentration 30% is take in the present invention, obtain by wet grinding the magnesium oxide slurries that granularity is less, and take ammonium chloride as buffering salt, alleviate the pH fluctuation of solution in reaction process, finally, by suction filtration, the processes such as lyophilize, obtain target product.

Concrete steps are as follows:

First measure in mass ratio magnesium oxide: ammonium chloride: hydrogen peroxide=1:(1.5-2.5): (30-40); Then after magnesium oxide being dissolved in to deionized water, grind to form the magnesium oxide slurries that massfraction is 3-4%; Ammonium chloride is joined in hydrogen peroxide, be configured to hydrogen peroxide-ammonium chloride mixed solution, then while stirring slowly, hydrogen peroxide-ammonium chloride mixed solution is joined in ground magnesium oxide slurries, continue reaction 3-4h, whole reaction process is carried out under the mechanical stirring of 500r/min, obtains mixed solution; Finally will obtain wet cake after the reaction mixture suction filtration, wet cake ,-80 ℃ of lower vacuum freezedryings, obtains particle diameter in the 20nm left and right, favorable dispersity, and purity is the target product nanometer magnesium peroxide powder more than 50%;

Above-mentioned hydrogen peroxide is adopted as the hydrogen peroxide that commercially available analytical pure massfraction is 30%.

Described magnesium oxide is commercially available analytical pure magnesium oxide.

Described ammonium chloride is commercially available analytical pure ammonium chloride.

The advantage that the present invention prepares the nanometer Magnesium peroxide is:

The raw materials cost is lower, simple to operate, and gained nanometer Magnesium peroxide particle diameter is even, good dispersity, and purity reaches more than 50%.

The accompanying drawing explanation

The XRD figure spectrum that Fig. 1 is the prepared nanometer Magnesium peroxide of embodiment 1;

The XRD figure spectrum that Fig. 2 is the prepared nanometer Magnesium peroxide of embodiment 2;

The SEM collection of illustrative plates that Fig. 3 is the prepared nanometer Magnesium peroxide of embodiment 1;

The SEM collection of illustrative plates that Fig. 4 is the prepared nanometer Magnesium peroxide of embodiment 2.

Embodiment

Embodiment 1

Accurately take commercially available analytical pure magnesium oxide 0.5g, in the 250ml beaker, add the 15ml deionized water, grind the 1h left and right after dissolving, obtain the magnesium oxide slurries of mass percent 3.2% left and right.Taking commercially available analytical pure ammonium chloride 1g is dissolved in the hydrogen peroxide 15ml that commercially available analytical pure massfraction is 30% left and right, after mixing fully, join slowly while stirring in ground magnesium oxide slurries, and 3.5h is reacted in continuation under the mechanical stirring of 500r/min, obtain white mixed solution, after suction filtration in-80 ℃ of vacuum freezedryings.Obtain target product nanometer magnesium peroxide powder.

Through X-ray diffractometer, test obtains the XRD figure spectrum of the nanometer Magnesium peroxide that Fig. 1 is the embodiment of the present invention 1 preparation, through comparing with standard card, shows that prepared material is Magnesium peroxide, and purity is 54%.Wherein contain a small amount of magnesium oxide and magnesium hydroxide.

As shown in Figure 3, be the SEM collection of illustrative plates of the prepared nanometer Magnesium peroxide of the embodiment of the present invention 1, as seen from the figure, it is spherical that particle is, and size is more even, and size distribution is at 20nm left and right, favorable dispersity.

Embodiment 2

Accurately take commercially available analytical pure magnesium oxide 1g, in the 250ml beaker, add the 25ml deionized water, after dissolving, grind 1.5h, obtain the magnesium oxide slurries of mass percent 3.8% left and right.Accurately take commercially available analytical pure ammonium chloride 2g and be dissolved in the hydrogen peroxide 35ml that commercially available analytical pure massfraction is 30% left and right, and continue reaction 4h under the mechanical stirring of 500r/min, obtain white mixed solution, after suction filtration in-80 ℃ of vacuum freezedryings.Obtain target product nanometer magnesium peroxide powder.

Through X-ray diffractometer, test obtains the XRD figure spectrum of the nanometer Magnesium peroxide that Fig. 2 is the embodiment of the present invention 2 preparations, through comparing with standard card, shows that prepared material is Magnesium peroxide, and purity is 52%.Contain a small amount of magnesium oxide and magnesium hydroxide.

As shown in Figure 4, be the SEM collection of illustrative plates of the prepared nanometer Magnesium peroxide of the embodiment of the present invention 2, as seen from the figure, it is spherical that particle is, and size is more even, and size distribution is at 20nm left and right, favorable dispersity.

Claims

1. the preparation method of a nanometer Magnesium peroxide is characterized in that:

First measure in mass ratio magnesium oxide: ammonium chloride: hydrogen peroxide=1:(1.5-2.5): (30-40); Then after magnesium oxide being dissolved in to deionized water, grind to form the magnesium oxide slurries that massfraction is 3-4%; Ammonium chloride is joined in hydrogen peroxide, be configured to hydrogen peroxide-ammonium chloride mixed solution, then while stirring slowly, hydrogen peroxide-ammonium chloride mixed solution is joined in ground magnesium oxide slurries, continue reaction 3-4h and obtain mixed solution, whole reaction process is carried out under the mechanical stirring of 500r/min, finally will obtain wet cake after the mixed solution suction filtration, wet cake ,-80 ℃ of lower vacuum freezedryings, obtains target product nanometer Magnesium peroxide;

Described magnesium oxide is commercially available analytical pure magnesium oxide;

Described ammonium chloride is commercially available analytical pure ammonium chloride;

Above-mentioned hydrogen peroxide adopts the hydrogen peroxide that commercially available analytical pure massfraction is 30%.