CN103420342B

CN103420342B - Preparation method for nano magnesium peroxide

Info

Publication number: CN103420342B
Application number: CN201310332750.4A
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: 2015-06-03
Anticipated expiration: 2033-08-01
Also published as: CN103420342A

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 nano magnesium peroxide

Technical field

The present invention relates to a kind of preparation method of nano 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 system white powder, odorless, tasteless, water insoluble, be soluble in diluted acid.More stable under normal temperature, heating or can be slow and stable when contacting with malaria discharge oxygen, then produce hydrogen peroxide after being dissolved in acid.Magnesium peroxide is nontoxic, environmentally safe, is therefore 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, as a kind of raw material that soil, settling, surface water and groundwater pollution are repaired.Foreign applications Magnesium peroxide carries out environment remediation and compares successful story and comprise and remove virus in earth's surface and underground water and the organic compound such as petroleum hydrocarbon, benzene,toluene,xylene, 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 synthesis 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 improving speed of reaction, save reaction cost, therefore, preparing nano level Magnesium peroxide can play product performance better, widens its Application Areas.

Chinese patent CN1370736A discloses 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, obtained wet product Magnesium peroxide after reaction, then by the dry magnesium peroxide powder obtaining content and be greater than 30%.Chinese patent CN101613088A discloses 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, with solubility magnesium salts, superoxol, alkali for raw material, in water solution system, hierarchy of control temperature reacts 2-10h at 10-30 DEG C, and reaction product after filtration, washing, drying obtains the magnesium peroxide powder that content is greater than 40%.All not mentioned product cut size problem in the preparation method of above-mentioned Magnesium peroxide, therefore, is necessary to strengthen the research to nano level Magnesium peroxide preparation method.

Summary of the invention

The object of this invention is to provide that a kind of purity is higher, the preparation method of the nano magnesium peroxide of uniform particle sizes, good dispersity.

In order to reach object of the present invention, the present invention with the hydrogen peroxide of magnesium oxide and mass concentration 30% for raw material, the less magnesia slurry of granularity is obtained by wet grinding, and be buffering salt with ammonium chloride, 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 magnesium oxide in mass ratio: ammonium chloride: hydrogen peroxide=1:(1.5-2.5): (30-40); Then the magnesia slurry that massfraction is 3-4% is ground to form after magnesium oxide being dissolved in deionized water; Ammonium chloride is joined in hydrogen peroxide, be configured to hydrogen peroxide-ammonium chloride mixed solution, then stir while slowly hydrogen peroxide-ammonium chloride mixed solution is joined in ground magnesia slurry, continue reaction 3-4h, whole reaction process is carried out under the mechanical stirring of 500r/min, obtains mixed solution; Finally obtain wet cake by after reaction mixture suction filtration, wet cake is vacuum freezedrying at-80 DEG C, obtains particle diameter at about 20nm, favorable dispersity, and purity is the target product nano magnesium peroxide powder of more than 50%;

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

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 nano magnesium peroxide is:

Raw materials cost is lower, simple to operate, and gained nano magnesium peroxide uniform particle sizes, good dispersity, purity reaches more than 50%.

Accompanying drawing explanation

The XRD figure spectrum of Fig. 1 nano magnesium peroxide prepared by embodiment 1;

The XRD figure spectrum of Fig. 2 nano magnesium peroxide prepared by embodiment 2;

The SEM collection of illustrative plates of Fig. 3 nano magnesium peroxide prepared by embodiment 1;

The SEM collection of illustrative plates of Fig. 4 nano magnesium peroxide prepared by embodiment 2.

Embodiment

Embodiment 1

Accurately take commercially available analytical pure magnesium oxide 0.5g, in 250ml beaker, add 15ml deionized water, after dissolving, grinding about 1h, obtains the magnesia slurry of mass percent about 3.2%.Taking commercially available analytical pure ammonium chloride 1g, to be dissolved in commercially available analytical pure massfraction be in the hydrogen peroxide 15ml of about 30%, join slowly while stirring in ground magnesia slurry after mixing completely, and under the mechanical stirring of 500r/min, continue reaction 3.5h, obtain the mixed solution of white, in-80 DEG C of vacuum freezedryings after suction filtration.Obtain target product nano magnesium peroxide powder.

Obtain through X-ray diffractometer test the XRD figure spectrum that Fig. 1 is nano magnesium peroxide prepared by the embodiment of the present invention 1, warp and standard card comparison, the prepared material of display is Magnesium peroxide, and purity is 54%.Wherein containing small amounts magnesium and magnesium hydroxide.

As shown in Figure 3, the SEM collection of illustrative plates of nano magnesium peroxide prepared by the embodiment of the present invention 1, as seen from the figure, particle is spherical, and size is relatively even, size distribution at about 20nm, favorable dispersity.

Embodiment 2

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

Obtain through X-ray diffractometer test the XRD figure spectrum that Fig. 2 is nano magnesium peroxide prepared by the embodiment of the present invention 2, warp and standard card comparison, the prepared material of display is Magnesium peroxide, and purity is 52%.Containing small amounts magnesium and magnesium hydroxide.

As shown in Figure 4, the SEM collection of illustrative plates of nano magnesium peroxide prepared by the embodiment of the present invention 2, as seen from the figure, particle is spherical, and size is relatively even, size distribution at about 20nm, favorable dispersity.

Claims

1. a preparation method for nano magnesium peroxide, is characterized in that:

First measure magnesium oxide in mass ratio: ammonium chloride: hydrogen peroxide=1:(1.5-2.5): (30-40); Then the magnesia slurry that massfraction is 3-4% is ground to form after magnesium oxide being dissolved in deionized water; Ammonium chloride is joined in hydrogen peroxide, be configured to hydrogen peroxide-ammonium chloride mixed solution, then stir while slowly hydrogen peroxide-ammonium chloride mixed solution is joined in ground magnesia slurry, continue reaction 3-4h and obtain mixed solution, whole reaction process is carried out under the mechanical stirring of 500r/min, finally obtain wet cake by after mixed solution suction filtration, wet cake is vacuum freezedrying at-80 DEG C, obtains target product nano 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 commercially available analytical pure massfraction to be the hydrogen peroxide of 30%.