CN103253636B - Preparation method of high-purity nanometre calcium peroxide - Google Patents
Preparation method of high-purity nanometre calcium peroxide Download PDFInfo
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Abstract
The invention relates to a preparation method of high-purity nanometre calcium peroxide. The preparation method comprises the following steps of: dissolving calcium chloride in deionized water and filtering at a room temperature, dissolving a surfactant in deionized water to be added into obtained filtrate to form a reaction mother solution, and adjusting the pH value of the reaction mother solution to be 9.5-11 by 25-28% ammonia water; and adding 30% hydrogen peroxide in the reaction mother solution according to a speed of 1.2-1.5 ml/min with mechanical stirring having a speed of 500 r/min, so as to obtain a reaction solution; and adding a NaOH solution serving as precipitator in the reaction solution, performing suction filtration on the generated white precipitate mixed solution to obtain a filter cake, washing the filter cake by absolute ethyl alcohol, performing vacuum freeze-drying at -80 DEG C based on the mixture of deionized water and absolute ethyl alcohol as a medium to obtain a target product, namely, nanometre calcium peroxide powder with a particle size of 20-100 nm, good dispersibility, and a purity of about 80%. The preparation method disclosed by the invention is low in raw material cost, simple to operate, and suitable for large-scale industrialized production.
Description
Technical field:
The present invention relates to a kind of preparation method of high-purity nanometre calcium peroxide, belong to preparation nanometer calcium peroxide method and technology field.
Background technology:
Calcium peroxide appearance white is to faint yellow, and odorless, tasteless, in crystallization or particulate state, meets sour Hydrogen Peroxide, be soluble in acid, be insoluble in water, ethanol equal solvent.Under normal temperature condition, dry and stable, its effective oxygen is 22.2%, and easily the moisture absorption is decomposed in atmosphere, simultaneously slow releasing oxygen.Calcium peroxide is nontoxic, environmentally safe, is a kind of novel, multi-functional, eco-friendly inorganic chemical product, is widely used in the fields such as agricultural, food, aquaculture, medical treatment.
At field of environment protection, comparatively early calcium peroxide is applied in situ chemical oxidation abroad, as a kind of method that soil, settling, surface water are repaired, has good degradation effect to the pollutent in soil and surface water body and improve the repairing performance of soil.Domesticly start from 21 century about calcium peroxide in the applied research of field of environment protection, be still in the starting stage at present, mainly for the treatment of the heavy metal ion in waste water, repair the pollution etc. of river bottom mud, oceanic sediment.
Although calcium peroxide is applicable to the biological degradation of soil and earth's surface water pollutant, the grain diameter of commercially available calcium peroxide is comparatively large, generally in micron level, and purity is not high, below 65%, slow with the speed of reaction of pollutent, be therefore necessary to improve its speed of response.Nano-scale calcium peroxide effectively can increase the surface-area of calcium peroxide, improves the speed of reaction of calcium peroxide and pollutent.Chinese patent 201210513253.X discloses a kind of method preparing nano-scale calcium peroxide, preparation process is in ice-water bath, calcium hydroxide is become the slurries of solid content 15-30% by ball mill grinding, adding the slurries after grinding to concentration is in the hydrogen peroxide of 30%, continuous stirring also reacts 15-20min, mixed solution salt acid for adjusting pH value after having reacted is 6-7, namely obtains calcium peroxide particle after mixed solution filtration, vacuum-drying.But products obtained therefrom particle diameter is 100-200nm, and stricti jurise does not belong to nano material.In addition, all description is not made to product purity in the preparation method of existing nanometer calcium peroxide.Therefore, be necessary to strengthen the research to high-purity nano level calcium 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 nanometer calcium peroxide of uniform particle sizes, good dispersity.
In order to reach above-mentioned purpose, the present invention is according to hydrolysis-sedimentation theory, be that the hydrogen peroxide of 30% is for raw material with calcium chloride and mass concentration, by adding cetomacrogol 1000 or cetyl trimethylammonium bromide as tensio-active agent, avoiding the irreversible agglomeration process of nanometer calcium peroxide particle, and passing through organic solvent washing, the processes such as lyophilize, obtaining particle diameter is 20-100nm, favorable dispersity, and purity is the calcium peroxide powder of about 80%.
Concrete steps are as follows:
First measure the hydrogen peroxide that mass concentration is 30%: calcium chloride=(4-6): 1 mol ratio, then at room temperature, is dissolved in deionized water by calcium chloride, filter after dissolving, filtrate is the calcium chloride solution containing 5-10% mass percent calcium chloride; Tensio-active agent is dissolved in deionized water, is then added in calcium chloride solution, obtain reaction mother liquor, the add-on of tensio-active agent is the 5-10% of calcium chloride quality, and regulates reaction mother liquor pH to be 9.5-11 with the ammoniacal liquor of 25-28%; Under the mechanical stirring of 500r/min, according to the speed of 1.2-1.5ml/min, hydrogen peroxide is joined in reaction mother liquor, obtain reaction solution; Joined by precipitation agent in reaction solution and obtain white precipitate mixed solution, the add-on of precipitation agent is as the criterion for making reaction solution pH=10-12; By after white precipitate mixed solution suction filtration filter cake, use absolute ethanol washing filter cake, and with the mixture of deionized water and dehydrated alcohol as medium,-80 DEG C of vacuum freezedryings, obtaining particle diameter is 20-100nm, favorable dispersity, and purity is the target product calcium peroxide powder of about 80%;
Described tensio-active agent is commercially available analytical pure cetomacrogol 1000 or cetyl trimethylammonium bromide;
Described deionized water and dehydrated alcohol mixture are deionized water: dehydrated alcohol=1:0.5-1 volume ratio;
Described precipitation agent is the NaOH solution of 12-13 by the pH value that commercially available analytical pure NaOH configures.
Prepared by the present invention, the advantage of nanometer calcium peroxide method is:
Raw materials cost is lower, simple to operate, and gained nanometer calcium peroxide uniform particle sizes, good dispersity, purity is high.
Accompanying drawing illustrates:
Fig. 1 is the XRD figure spectrum of embodiment 1 nanometer calcium peroxide;
Fig. 2 is the XRD figure spectrum of embodiment 2 nanometer calcium peroxide;
The SEM collection of illustrative plates of Fig. 3 nanometer calcium peroxide prepared by embodiment 1;
The SEM collection of illustrative plates of Fig. 4 nanometer calcium peroxide prepared by embodiment 2.
Embodiment:
Embodiment 1
Accurately take commercially available analytical pure Calcium Chloride Powder Anhydrous 3g, in 500ml beaker, add 30ml deionized water, filter after dissolving, filtrate is the calcium chloride solution containing about 9% mass percent calcium chloride.Take 6g cetomacrogol 1000, after being dissolved in 100ml deionized water, joining in calcium chloride solution and become reaction mother liquor, and regulate reaction mother liquor pH value to be about 9.5 with the ammoniacal liquor of massfraction about 27%.Under the mechanical stirring of 500r/min, in reaction mother liquor, dripping commercially available analytical pure massfraction according to the speed of 1.5ml/min is the hydrogen peroxide of about 30%, and the mol ratio of added hydrogen peroxide and calcium chloride is 6:1, obtains reaction solution.Using pH value be 13 NaOH solution add in reaction solution as precipitation agent, to be reaction solution pH be the add-on of NaOH solution about 11 is as the criterion, and generates white precipitate mixed solution, after white precipitate mixed solution suction filtration, obtain filter cake.With absolute ethanol washing filter cake 5 times, with deionized water and dehydrated alcohol mixture (volume ratio is for 1:1) as medium ,-80 DEG C of vacuum freezedryings.Obtain target product nanometer calcium peroxide powder.
Obtain through X-ray diffractometer test the XRD figure spectrum that Fig. 1 is nanometer calcium peroxide prepared by the embodiment of the present invention 1, warp and standard card comparison, the prepared material of display is calcium peroxide, and purity is about 80%.
As shown in Figure 3, the SEM collection of illustrative plates of nanometer calcium 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 20-100nm, favorable dispersity.
Embodiment 2
Accurately take commercially available analytical pure Calcium Chloride Powder Anhydrous 3g, in 500ml beaker, add 30ml deionized water, filter after dissolving, filtrate is the calcium chloride solution containing about 9% mass percent calcium chloride.Take 7g cetyl trimethylammonium bromide, after being dissolved in 100ml deionized water, joining in calcium chloride solution and become reaction mother liquor.And be about 10.5 with the ammoniacal liquor regulator solution pH of 27%.Under the mechanical stirring of 500r/min, in reaction mother liquor, dripping commercially available analytical pure mass percentage concentration according to the speed of 1.5ml/min is the hydrogen peroxide of about 30%, and the mol ratio of added hydrogen peroxide and calcium chloride is 6:1, formation reaction liquid.Using pH value be about 13 NaOH solution be about 11 as precipitation agent adjustment reaction solution pH, generate white precipitate mixed solution, after white precipitate mixed solution suction filtration, obtain filter cake.With absolute ethanol washing filter cake 5 times, with deionized water and dehydrated alcohol mixture (volume ratio is for 1:1) as medium ,-80 DEG C of vacuum freezedryings.Obtain target product nanometer calcium peroxide powder.
Obtain through X-ray diffractometer test the XRD figure spectrum that Fig. 2 is nanometer calcium peroxide prepared by the embodiment of the present invention 2, warp and standard card comparison, the prepared material of display is calcium peroxide, and purity is about 80%.
As shown in Figure 4, for the embodiment of the present invention 2 prepares the SEM collection of illustrative plates of nanometer calcium peroxide, as seen from the figure, particle is spherical, and size is relatively even, size distribution at 20-100nm, favorable dispersity.
Claims (1)
1. the preparation method of a high-purity nanometre calcium peroxide, it is characterized in that: first measure hydrogen peroxide: calcium chloride=(4-6): 1 mol ratio, then at room temperature, calcium chloride is dissolved in deionized water, filter after dissolving, filtrate is the calcium chloride solution containing 5-10% mass percent calcium chloride, add in calcium chloride solution after tensio-active agent being dissolved in deionized water and become reaction mother liquor, the add-on of tensio-active agent is the 5-10% of calcium chloride quality, and regulates reaction mother liquor pH value to be 9.5-11 with the ammoniacal liquor of 25-28% mass percent; Under the mechanical stirring of 500r/min, according to the speed of 1.2-1.5mL/min, be that the hydrogen peroxide of 30% joins in reaction mother liquor by mass concentration, obtain reaction solution; Precipitation agent is joined in reaction solution and obtain white precipitate mixed solution, the add-on of precipitation agent is as the criterion for making reaction solution pH=10-12, then by white precipitate mixed solution suction filtration, filter cake, finally use absolute ethanol washing filter cake, and with deionized water and dehydrated alcohol mixture as medium,-80 DEG C of vacuum freezedryings, obtaining particle diameter is 20-100nm, favorable dispersity, and purity is the target product nanometer calcium peroxide powder of 80%;
Described tensio-active agent is commercially available analytical pure cetomacrogol 1000 or cetyl trimethylammonium bromide;
Described deionized water and dehydrated alcohol mixture are deionized water: commercially available analytical pure dehydrated alcohol=1:0.5-1 volume ratio;
Described precipitation agent is the NaOH solution of 12-13 by the pH value that commercially available analytical pure NaOH configures.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103601155A (en) * | 2013-11-18 | 2014-02-26 | 同济大学 | Method for preparing nano calcium peroxide by chemical modification |
| CN104843649A (en) * | 2014-12-16 | 2015-08-19 | 江苏金桥盐化集团有限责任公司 | Preparation method for calcium peroxide |
| CN105668521B (en) * | 2016-01-06 | 2017-11-28 | 华东交通大学 | A kind of preparation method of the smooth calper calcium peroxide in high-purity nano particle diameter surface |
| CN108658047B (en) * | 2018-07-28 | 2021-06-11 | 华中科技大学 | Method for preparing high-content nano magnesium peroxide by one-pot precipitation method and product thereof |
| CN109261117B (en) * | 2018-08-08 | 2021-06-22 | 河南工程学院 | Preparation method of rectorite-based spherical nano calcium salt loaded oxidant |
| US11453587B2 (en) * | 2018-11-19 | 2022-09-27 | Lixivia, Inc. | Compositions and methods for production of metal peroxides |
| CN109896722A (en) * | 2019-04-12 | 2019-06-18 | 河南工程学院 | A kind of spherical nanometer calper calcium peroxide preparation method for deeply dehydrating sludge |
| CN112062100A (en) * | 2020-04-27 | 2020-12-11 | 同济大学 | Nano calcium peroxide, preparation method and application |
| CN112717143B (en) * | 2021-01-15 | 2022-08-12 | 洛兮医疗科技(杭州)有限公司 | Biodegradable nano-carrier and targeting drug-loading system thereof |
| CN113150516B (en) * | 2021-02-04 | 2022-09-02 | 华东理工大学 | Polylactic acid-based layered nano modified membrane and preparation method and application thereof |
| CN112919756B (en) * | 2021-03-22 | 2022-08-30 | 大连海事大学 | Method for treating antibiotic resistance genes in medical wastewater or sludge generated by medical wastewater treatment process |
| CN113577276B (en) * | 2021-08-02 | 2023-06-23 | 浙江理工大学 | Ion-doped polydopamine coated calcium peroxide composite nanoparticle as well as preparation method and application thereof |
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| CN101186277A (en) * | 2006-11-17 | 2008-05-28 | 上海中远化工有限公司 | Method for preparing calcium peroxide from calcium chloride |
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| CN101186277A (en) * | 2006-11-17 | 2008-05-28 | 上海中远化工有限公司 | Method for preparing calcium peroxide from calcium chloride |
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