CN109896722A - A kind of spherical nanometer calper calcium peroxide preparation method for deeply dehydrating sludge - Google Patents
A kind of spherical nanometer calper calcium peroxide preparation method for deeply dehydrating sludge Download PDFInfo
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- CN109896722A CN109896722A CN201910294781.2A CN201910294781A CN109896722A CN 109896722 A CN109896722 A CN 109896722A CN 201910294781 A CN201910294781 A CN 201910294781A CN 109896722 A CN109896722 A CN 109896722A
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Abstract
The invention discloses a kind of spherical nanometer calper calcium peroxide preparation methods for deeply dehydrating sludge, this method is using calcium chloride as raw material, include the following steps: for a certain amount of dispersing agent to be added as reaction mother liquor in calcium saline solution, and reaction mother liquor pH value is adjusted to 9 ~ 11 with ammonium hydroxide；Magnetic agitation after a certain period of time, certain density hydrogen peroxide given pace is added still in the reaction mother liquor of magnetic agitation, stands 2h after being added dropwise to complete；A certain amount of sodium hydroxide, which is added, makes calper calcium peroxide precipitate to form mixed liquor, is filtered with the machine of suction filtration, obtains after filter cake dehydrated alcohol wash repeatedly, be placed in vacuum freeze drier and dry 12 ~ for 24 hours to get having arrived spherical nanometer calcium peroxide powder.The present invention is prepared under normal temperature conditions, easy to operate, and raw material is cheap and easy to get, and good product dispersibility, partial size is small, provides the synthetic method of spherical nanometer calper calcium peroxide for the deep dehydration of sludge.
Description
Technical field
The invention belongs to environmental technology fields, and in particular to a kind of spherical nanometer calper calcium peroxide for deeply dehydrating sludge
Preparation method.
Background technique
With the increase of China human mortality quantity and the raising of economic level, sludge yield is dramatically increased.Sludge be by water and
Generated solid sediment matter in sewage disposal process is inevitable product in sewage treatment.It has moisture content height,
Complicated component is easy the features such as corruption is smelly.Untreated sludge then has volume big, and inconvenience transport constitutes the ecosystem
The features such as significant threat.Currently, the processing method in China is broadly divided into two kinds: natural desiccation method, mechanical dehydration method.Wherein, certainly
Right desiccation method is to utilize moisture in sun evaporative removal sludge.It is by influences such as temperature, humidity, rainfalls and drying bed takes up an area
Area is big, and time-consuming, cannot be widely applied.Mechanical dehydration method is to reach sludge dewatering by applying pressure on filter medium
Purpose.And dewatering performance of sludge can be improved by adding sludge conditioner, improve mechanical dehydration effect.Common sludge conditioning
Agent has inorganic coagulant (such as aluminium salt, molysite) and high-molecular coagulant adopting (such as polyacrylamide), though moisture percentage in sewage sludge can be reduced
To 80%, realizes minimizing to a certain extent, but still be not able to satisfy requirement of the subsequent landfill burning of country to moisture percentage in sewage sludge.
Calper calcium peroxide is a kind of faint yellow or white inorganic metal peroxide, is in powdered, relative density 2.92, melts
275 DEG C of point, is insoluble in water, insoluble in organic solvents such as ethyl alcohol.It can stablize preservation under the conditions of drying at room temperature, in moist ring
It can react slowly to decompose with water in border and generate oxygen, be a kind of environmental-friendly slow-release oxygen material.It is not only supported in agricultural, aquatic products
Grow, there is wide application in the fields such as food fresh keeping, be also used in sludge dewatering in recent years.In practical applications, peroxidating is utilized
The oxidation and flocculation of calcium can be effectively improved dewatering performance of sludge.But there is particles for traditional calper calcium peroxide greatly,
Problem easy to reunite has seriously affected utilization rate of the calper calcium peroxide in deeply dehydrating sludge.The spherical modification of nanometer is carried out to it
Specific surface area can be significantly improved, increases the contact site with sludge, to improve reaction rate and utilization rate.Its spherical characteristics is also
The lattice structure that rigidity can be formed, plays the role of framework construction body, keeps the dehydration channel of sludge unobstructed, improves dehydration effect
Rate.
Summary of the invention
The present invention in order to solve shortcoming in the prior art, provide a kind of easy to operate, at low cost, energy conservation and environmental protection,
The high spherical nanometer calper calcium peroxide preparation method for deeply dehydrating sludge of utilization rate.
In order to solve the above technical problems, the present invention adopts the following technical scheme: a kind of for the spherical of deeply dehydrating sludge
Nanometer calper calcium peroxide preparation method, includes the following steps:
(1) calcium salt is added in deionized water, the calcium salt soln being configured to；
(2) a certain amount of dispersing agent is added in calcium salt soln and forms reaction mother liquor, and adjusts reaction mother liquor pH value 9 with ammonium hydroxide
Between ~ 11；20 ~ 40min of magnetic agitation reaction mother liquor is used at room temperature, is sufficiently mixed above-mentioned substance；
(3) in the reaction mother liquor being stirred continuously for being added drop-wise to the hydrogen peroxide that mass fraction is 30%, reaction solution is obtained；
(4) the reaction was continued 30 ~ 60min after hydrogen peroxide is added dropwise to complete；
(5) sodium hydroxide is added in reaction solution as precipitating reagent and obtains white suspension；
(6) white suspension is filtered, is washed repeatedly after obtained filter cake with dehydrated alcohol；
(7) filter cake is placed in freeze drier dry 12 after washing ~ for 24 hours to get spherical nanometer calper calcium peroxide.
The dispersing agent being added in step (2) is polyethylene glycol, and average molecular weight is between 200 ~ 1000.
The molar ratio of calcium salt and dispersing agent is 1:(15 ~ 20).
The molar ratio that the hydrogen peroxide and calcium salt in reaction mother liquor are added drop-wise in step (3) is (4 ~ 6): 1.
The drop rate for the hydrogen peroxide that mass fraction is 30% in step (3) is 0.8 ~ 1.3mL/min.
By adopting the above technical scheme, the invention has the following advantages:
1, raw material of the present invention and production equipment are cheap and easy to get, and technological operation is simple.
2, raw material and product used in the present invention are nontoxic, do not generate pollution to environment.
3, the spherical calper calcium peroxide of nanoscale that the present invention is prepared can be used for the deep dehydration of sludge, the spherical peroxide of nanometer
The granularity for changing calcium is small, large specific surface area, reacts that contact site is more, and utilization rate is high with sludge.
4, chondritic plays framework construction body, is that the holding dehydration channel of sludge is unobstructed, improves dehydration efficiency.
Detailed description of the invention
Fig. 1 is commercially available calper calcium peroxide scanning electron microscope (SEM) photograph；
Fig. 2 is the scanning electron microscope (SEM) photograph of the spherical calper calcium peroxide of synthesized nanometer；
Fig. 3 is the transmission electron microscope picture of the spherical calper calcium peroxide of synthesized nanometer；
Fig. 4 is the X ray diffracting spectrum of the spherical calper calcium peroxide of synthesized nanometer.
Specific embodiment
The present invention is described in further detail combined with specific embodiments below.
Embodiment one
(1) 3g calcium chloride is accurately weighed, is dissolved in 30mL deionized water, the poly- second of 100mL is added in the calcium salt soln being configured to
Glycol (PEG 200) forms reaction mother liquor；
(2) adjusting reaction mother liquor pH with 1mol/L ammonium hydroxide is 10；20min is stirred through room temperature mechanical, is sufficiently mixed above-mentioned substance；
(3) hydrogen peroxide that 15mL mass fraction is 30% is added it is characterized in that in the reaction mother liquor being stirred continuously entered, is obtained
Reaction solution；
(4) the reaction was continued 60min after hydrogen peroxide is added dropwise to complete；
(5) sodium hydroxide is added in reaction solution as precipitating reagent and obtains white suspension, then white suspension is filtered, is obtained
To filter cake washed repeatedly with dehydrated alcohol；Filter cake is placed in freeze drier dry 12h to get spherical nanometer mistake after washing
Calcium oxide；
Synthesized sample carries out X-ray diffraction characterization, with standard card ratio, it was demonstrated that synthesized calper calcium peroxide.
Embodiment two
(1) 3g calcium chloride is accurately weighed, is dissolved in 30mL deionized water, the poly- second two of 80mL is added in the calcium salt soln being configured to
Alcohol (PEG 200) forms reaction mother liquor.
(2) adjusting reaction mother liquor pH with 1mol/L ammonium hydroxide is 10；30min is stirred through room temperature mechanical, keeps above-mentioned substance abundant
Mixing.
(3) hydrogen peroxide that 15mL mass fraction is 30% is added it is characterized in that in the reaction mother liquor being stirred continuously entered,
Obtain reaction solution.
(4) the reaction was continued 60min after hydrogen peroxide is added dropwise to complete.
(5) sodium hydroxide is added in reaction solution as precipitating reagent and obtains white suspension, then take out white suspension
Filter, obtained filter cake are washed repeatedly with dehydrated alcohol；Filter cake is placed in freeze drier dry 12h to get spherical after washing
Nanometer calper calcium peroxide.
Synthesized sample carries out X-ray diffraction characterization, it was demonstrated that has synthesized calper calcium peroxide.
Embodiment three
(1) 3g calcium chloride is accurately weighed, is dissolved in 30mL deionized water, the PEG of 50g is added in the calcium salt soln being configured to
1000 form reaction mother liquor.
(2) adjusting reaction mother liquor pH with 1mol/L ammonium hydroxide is 10；30min is stirred through room temperature mechanical, keeps above-mentioned substance abundant
Mixing.
(3) hydrogen peroxide that 15mL mass fraction is 30% is added it is characterized in that in the reaction mother liquor being stirred continuously entered,
Obtain reaction solution.
(4) the reaction was continued 60min after hydrogen peroxide is added dropwise to complete.
(5) sodium hydroxide is added in reaction solution as precipitating reagent and obtains white suspension, then take out white suspension
Filter, obtained filter cake are washed repeatedly with dehydrated alcohol；Filter cake is placed in freeze drier after washing and is dried for 24 hours to get spherical
Nanometer calper calcium peroxide.
Synthesized sample carries out X-ray diffraction characterization, it was demonstrated that has synthesized calper calcium peroxide.
Fig. 1 is the microscopic appearance for amplifying the commercially available calper calcium peroxide under 10,000 times, it can be seen that commercially available calper calcium peroxide is mutually rolled into a ball
Poly-, adhesion, particle diameter are larger.
Fig. 2 is the microscopic appearance for amplifying spherical nanometer calper calcium peroxide synthesized under 10,000 times, and monomer can be clearly seen
Spherical particle, distribution uniform, favorable dispersibility, particle diameter are less than 500nm.
Fig. 3 shows CaO2Particle dispersion, glomeration is obvious, and diameter is in 100nm or so.
Belong to CaO as seen from Figure 42Characteristic peak 2 θ=30.1,35.6,47.3, it was demonstrated that synthesized nanometer peroxidating
Calcium.
Above three embodiments not shape of the invention, material, structure etc. are made any form of restriction, it is all according to
According to technical spirit any simple modification, equivalent change and modification to the above embodiments of the invention, the present invention is belonged to
The protection scope of technical solution.
Claims (5)
1. a kind of spherical nanometer calper calcium peroxide preparation method for deeply dehydrating sludge, characterized by the following steps:
(1) calcium salt is added in deionized water, the calcium salt soln being configured to；
(2) a certain amount of dispersing agent is added in calcium salt soln and forms reaction mother liquor, and adjusts reaction mother liquor pH value 9 with ammonium hydroxide
Between ~ 11；20 ~ 40min of magnetic agitation reaction mother liquor is used at room temperature, is sufficiently mixed above-mentioned substance；
(3) in the reaction mother liquor being stirred continuously for being added drop-wise to the hydrogen peroxide that mass fraction is 30%, reaction solution is obtained；
(4) the reaction was continued 30 ~ 60min after hydrogen peroxide is added dropwise to complete；
(5) sodium hydroxide is added in reaction solution as precipitating reagent and obtains white suspension；
(6) white suspension is filtered, is washed repeatedly after obtained filter cake with dehydrated alcohol；
(7) filter cake is placed in freeze drier dry 12 after washing ~ for 24 hours to get spherical nanometer calper calcium peroxide.
2. a kind of spherical nanometer calper calcium peroxide preparation method for deeply dehydrating sludge according to claim 1, special
Sign is: the dispersing agent being added in step (2) is polyethylene glycol, and average molecular weight is between 200 ~ 1000.
3. a kind of spherical nanometer calper calcium peroxide preparation method for deeply dehydrating sludge according to claim 1 or 2,
Be characterized in that: the molar ratio of calcium salt and dispersing agent is 1:(15 ~ 20).
4. a kind of spherical nanometer calper calcium peroxide preparation method for deeply dehydrating sludge according to claim 1, special
Sign is: the molar ratio that the hydrogen peroxide and calcium salt in reaction mother liquor are added drop-wise in step (3) is (4 ~ 6): 1.
5. a kind of spherical nanometer calper calcium peroxide preparation method for deeply dehydrating sludge according to claim 1, special
Sign is: the drop rate for the hydrogen peroxide that mass fraction is 30% in step (3) is 0.8 ~ 1.3mL/min.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112647193A (en) * | 2020-12-31 | 2021-04-13 | 上海市第六人民医院 | Preparation method of electron beam irradiation crosslinked calcium peroxide-carbon quantum dot @ zein antibacterial film |
| CN112919756A (en) * | 2021-03-22 | 2021-06-08 | 大连海事大学 | Method for treating antibiotic resistance genes in medical wastewater or sludge generated by medical wastewater treatment process |
| CN115490340A (en) * | 2022-05-16 | 2022-12-20 | 华中科技大学 | Nitrogen, phosphorus and algae removal agent and preparation method and application thereof |
| WO2023165388A1 (en) * | 2022-03-01 | 2023-09-07 | 南京大学 | Deep biological denitrification strengthening and endocrine disrupting toxicity reducing method |
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| CN103253636A (en) * | 2013-05-15 | 2013-08-21 | 同济大学 | Preparation method of high-purity nanometre calcium peroxide |
| CN103601155A (en) * | 2013-11-18 | 2014-02-26 | 同济大学 | Method for preparing nano calcium peroxide by chemical modification |
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Patent Citations (2)
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| CN103253636A (en) * | 2013-05-15 | 2013-08-21 | 同济大学 | Preparation method of high-purity nanometre calcium peroxide |
| CN103601155A (en) * | 2013-11-18 | 2014-02-26 | 同济大学 | Method for preparing nano calcium peroxide by chemical modification |
Non-Patent Citations (3)
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| CHEN ZHAN 等: "Enhancement of waste activated sludge dewaterability using calcium peroxide preoxidation and chemical re-flocculation", 《WATER RESEARCH》 * |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112647193A (en) * | 2020-12-31 | 2021-04-13 | 上海市第六人民医院 | Preparation method of electron beam irradiation crosslinked calcium peroxide-carbon quantum dot @ zein antibacterial film |
| CN112919756A (en) * | 2021-03-22 | 2021-06-08 | 大连海事大学 | Method for treating antibiotic resistance genes in medical wastewater or sludge generated by medical wastewater treatment process |
| WO2023165388A1 (en) * | 2022-03-01 | 2023-09-07 | 南京大学 | Deep biological denitrification strengthening and endocrine disrupting toxicity reducing method |
| CN115490340A (en) * | 2022-05-16 | 2022-12-20 | 华中科技大学 | Nitrogen, phosphorus and algae removal agent and preparation method and application thereof |
| CN115490340B (en) * | 2022-05-16 | 2023-08-22 | 华中科技大学 | Denitrification dephosphorization algaecide, preparation method and application thereof |
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