CN104069793A - Preparation method of calcium hydroxide nano particles with high adsorption activity - Google Patents
Preparation method of calcium hydroxide nano particles with high adsorption activity Download PDFInfo
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- CN104069793A CN104069793A CN201410281576.XA CN201410281576A CN104069793A CN 104069793 A CN104069793 A CN 104069793A CN 201410281576 A CN201410281576 A CN 201410281576A CN 104069793 A CN104069793 A CN 104069793A
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- necked bottle
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- sds
- cacl2
- cacl
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Abstract
The invention discloses a preparation method of calcium hydroxide nano particles with high adsorption activity. The preparation method is characterized by comprising the following steps: putting CaCl2 in a three-necked bottle; adding deionized water to dissolve the CaCl2; stirring with a magnetic stirrer; weighing SDS or PEG, wherein the mass ratio is as follows:CaCl2:SDS is equal to 22.2:(0.47-2.34) or CaCl2:SDS is equal to 22.2:(2.65-14.44); adding SDS or PEG into the three-necked bottle; stirring to dissolve; dissolving NaOH in the deionized water, wherein mass ratio of the CaCl2 to the NaOH is 22.2:8;dropwise adding an obtained solution to the three-necked bottle at the speed of 40ml/h; stirring to react for 0.5-2.5 hours to obtain slurry; performing suction filtering on the slurry; and washing and drying. According to the preparation method, the prepared Ca(OH)2 power body is uniform in particles and are in single dispersion; the particle granularity is 200-300nm and the specific surface area is 88m<2>/g; the maximum N2 adsorption amount can reach 80ml/g; meanwhile the removal rate of NOx can reach 98%; the preparation method has important practical significance on leakage treatment of liquid propellant N2O4 at a space launching site.
Description
Technical field
The present invention relates to dinitrogen tetroxide (N
2o
4) there is the Material Field that adsorbs transformation function, be a kind of preparation method with high adsorption activity calcium hydroxide nano particle.
Background technology
Space launching site liquid propellant dinitrogen tetroxide (N
2o
4once) leak, under natural environment temperature and pressure, can volatilize rapidly and be converted into red nitrogen dioxide (NO
2) gas.The higher concentration NO of moment
2gas can cause operating personnel's pulmonary edema and chemical pneumonia, even can cause personnel's death by suffocation.The NO of a large amount of volatilizations
2gas is not only the main cause that acid rain occurs, and can form photochemical fog in air, to environment.Therefore to liquid propellant N
2o
4leaking volatilization gas carries out effectively adsorbing to catch and raffinate is carried out to safe disposal being fast very important.Ca (OH)
2powder can be caught N by suction-operated and neutralization of acid with base
2o
4leak volatilization gas.Because absorption and neutralization reaction are mainly carried out at powder surface, so prepare bigger serface and high surface Ca (OH)
2powder is to improve it for N
2o
4leak the key of disposal efficiency.
As everyone knows, the preparation of loose structure and ultra-fine grain, be improve two of powder specific-surface area detection mainly by way of.Ca (OH)
2crystal is the eight-coordinate crystal structure of the simple grid of trigonal system six side, is strong polar crystal, and in liquid phase reactor, crystal grain is very easily grown up, the Ca (OH) of preparation short distance or long-range order pore structure
2crystal hardly may.Therefore, the fine of particle is to prepare Large ratio surface, high activity Ca (OH)
2the method that crystal is comparatively feasible.The Ca (OH) that adopts CaO digestion process to produce at present
2powder, specific area is 20～25m
2/ g; And adopting liquid chemical precipitation preparation, specific area is also lower, general <15m
2/ g, this is due to Ca (OH)
2powder is unstable especially.Therefore the Ca (OH) of high activity, high-ratio surface is prepared in research
2nano particle is very meaningful.
Summary of the invention
The object of the invention is to adopt the homogeneous precipitation method of surfactant structure induction, prepare a kind of high adsorption activity Ca (OH)
2nano particle.This particle is high to the Adsorption ability of NOx, and operating procedure is simple.
The preparation method of a kind of high adsorption activity calcium hydroxide nano particle provided by the present invention, is characterized in that, comprises the following steps:
The first step, takes the CaCl of certain mass
2, put into three-necked bottle, add deionized water dissolving, making its concentration is 0.2mol/L, adopts magnetic stirrer;
Second step, takes a certain amount of SDS or PEG, they and CaCl
2mass ratio be: CaCl
2: SDS:=22.2:(0.47～2.34), or CaCl
2: PEG=22.2:(2.65～14.44), join stirring and dissolving in three-necked bottle;
The 3rd step, takes certain mass NaOH and is dissolved in deionized water, and making its concentration is 0.2mol/L, CaCl
2: NaOH mass ratio=22.2:8, then splash in three-necked bottle with the speed of 40ml/h, stirring reaction 0.5h～2.5h obtains slurry;
The 4th step, will the slurry suction filtration that obtains of reaction after, first with distilled water washing 2 times, again with ethanol washing 2 times, finally by filter cake vacuum drying 24h under 60 DEG C of environment.
For addressing the above problem, the present invention adopts the homogeneous precipitation method of surfactant structure induction, utilizes surfactant can effectively reduce the capillary principle of reaction system, in liquid-phase chemical reaction, controls Ca (OH)
2the growth of crystal grain, prepares uniform particles, is dispersed nano Ca (OH)
2powder, grain graininess is 200nm～300nm; Specific area can reach 88m
2/ g.To N
2maximal absorptive capacity can reach 80mL/g, there is good adsorption capacity; NOx is had to good Adsorption ability, clearance can reach 98% simultaneously, and this is to space launching site liquid propellant N
2o
4leakage processing there is important practical significance.
Brief description of the drawings
The XRD curve of Fig. 1 embodiment Isosorbide-5-Nitrae product
The scanning electron microscope image of Fig. 2 embodiment 2 products
The scanning electron microscope image of Fig. 3 embodiment 3 products
The scanning electron microscope image of Fig. 4 embodiment 5 products
The scanning electron microscope image of Fig. 5 embodiment 6 products
The absorption property curve of Fig. 6 embodiment 3,6 products
Detailed description of the invention
Embodiment 1
1, take 22.2g CaCl
2, put into 250ml three-necked bottle, add 80ml deionized water dissolving, adopt magnetic stirrer;
2, the SDS that takes 0.47g joins in three-necked bottle, stirring and dissolving;
3, take 8.0gNaOH and be dissolved in 20ml deionized water, splash in three-necked bottle stirring reaction 0.5h with the speed of 40ml/h.
4, after will the slurry suction filtration that obtains of reaction, first with distilled water washing 2 times, again with ethanol washing 2 times, finally by filter cake vacuum drying 24h under 60 DEG C of environment.
Embodiment 2
1, take 22.2g CaCl
2, put into 250ml three-necked bottle, add 80ml deionized water dissolving, adopt magnetic stirrer;
2, the SDS that takes 1.17g joins in three-necked bottle, stirring and dissolving;
3, take 8.0gNaOH and be dissolved in 20ml deionized water, splash in three-necked bottle stirring reaction 1.5h with the speed of 40ml/h.
4, after will the slurry suction filtration that obtains of reaction, first with distilled water washing 2 times, again with ethanol washing 2 times, finally by filter cake vacuum drying 24h under 60 DEG C of environment.
Embodiment 3
1, take 22.2g CaCl
2, put into 250ml three-necked bottle, add 80ml deionized water dissolving, adopt magnetic stirrer;
2, the SDS that takes 2.34g joins in three-necked bottle, stirring and dissolving;
3, take 8.0gNaOH and be dissolved in 20ml deionized water, splash in three-necked bottle stirring reaction 2.5h with the speed of 40ml/h.
4, after will the slurry suction filtration that obtains of reaction, first with distilled water washing 2 times, again with ethanol washing 2 times, finally by filter cake vacuum drying 24h under 60 DEG C of environment.
Embodiment 4
1, take 22.2g CaCl
2, put into 250ml three-necked bottle, add 80ml deionized water dissolving, adopt magnetic stirrer;
2, the PEG that measures 2.65g joins in three-necked bottle, stirring and dissolving;
3, take 8.0gNaOH and be dissolved in 20ml deionized water, splash in three-necked bottle stirring reaction 1.0h with the speed of 40ml/h.
4, after will the slurry suction filtration that obtains of reaction, first with distilled water washing 2 times, again with ethanol washing 2 times, finally by filter cake vacuum drying 24h under 60 DEG C of environment.
Embodiment 5
1, take 22.2g CaCl
2, put into 250ml three-necked bottle, add 80ml deionized water dissolving, adopt magnetic stirrer;
2, the PEG that measures 6.84g joins in three-necked bottle, stirring and dissolving;
3, take 8.0gNaOH and be dissolved in 20ml deionized water, splash in three-necked bottle stirring reaction 2.0h with the speed of 40ml/h.
4, after will the slurry suction filtration that obtains of reaction, first with distilled water washing 2 times, again with ethanol washing 2 times, finally by filter cake vacuum drying 24h under 60 DEG C of environment.
Embodiment 6
1, take 22.2g CaCl
2, put into 250ml three-necked bottle, add 80ml deionized water dissolving, adopt magnetic stirrer;
2, the PEG that measures 14.44g joins in three-necked bottle, stirring and dissolving;
3, take 8.0gNaOH and be dissolved in 20ml deionized water, splash in three-necked bottle stirring reaction 2.5h with the speed of 40ml/h.
4, after will the slurry suction filtration that obtains of reaction, first with distilled water washing 2 times, again with ethanol washing 2 times, finally by filter cake vacuum drying 24h under 60 DEG C of environment.
The eliminating rate of absorption of the each embodiment specific area of table 1 and NOx
Claims (1)
1. a preparation method for high adsorption activity calcium hydroxide nano particle, is characterized in that, comprises the following steps:
The first step, takes the CaCl of certain mass
2, put into three-necked bottle, add deionized water dissolving, making its concentration is 0.2mol/L, adopts magnetic stirrer;
Second step, takes a certain amount of SDS or PEG, they and CaCl
2mass ratio be: CaCl
2: SDS=22.2:(0.47～2.34), or CaCl
2: PEG=22.2:(2.65～14.44), join stirring and dissolving in three-necked bottle;
The 3rd step, takes certain mass NaOH and is dissolved in deionized water, and making its concentration is 0.2mol/L, CaCl
2: NaOH mass ratio=22.2:8, then splash in three-necked bottle with the speed of 40ml/h, stirring reaction 0.5h～2.5h obtains slurry;
The 4th step, will the slurry suction filtration that obtains of reaction after, first with distilled water washing 2 times, again with ethanol washing 2 times, finally by filter cake vacuum drying 24h under 60 DEG C of environment.
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|---|---|---|---|
| CN201410281576.XA CN104069793A (en) | 2014-06-21 | 2014-06-21 | Preparation method of calcium hydroxide nano particles with high adsorption activity |
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| CN104069793A true CN104069793A (en) | 2014-10-01 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106111082A (en) * | 2016-04-25 | 2016-11-16 | 河池学院 | Highly active CO2adsorbent and preparation method thereof |
| CN109052608A (en) * | 2018-08-07 | 2018-12-21 | 米易东立矿业有限公司 | Sulfuric acid method titanium pigment waste water treating agent and preparation method thereof |
| CN109261117A (en) * | 2018-08-08 | 2019-01-25 | 河南工程学院 | A kind of preparation method loading spherical nanometer calcium salt oxidizing agent based on rectorite |
| CN111185136A (en) * | 2020-01-18 | 2020-05-22 | 中国人民解放军火箭军工程大学 | Dinitrogen tetroxide absorbent, preparation method and application |
| CN111250041A (en) * | 2020-01-18 | 2020-06-09 | 中国人民解放军火箭军工程大学 | Propellant processing bag and preparation method and application thereof |
Citations (3)
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| CA2009731A1 (en) * | 1989-02-11 | 1990-08-11 | Carl-Ernst Van Der Smissen | Process for the production of an absorption mass for carbon dioxide |
| CN1189814A (en) * | 1996-04-24 | 1998-08-05 | 矢桥工业株式会社 | Process for producing clacium hydroxide |
| CN101254935A (en) * | 2008-04-03 | 2008-09-03 | 武汉工程大学 | Method for preparing calcium hydroxide with high purity and high activity |
-
2014
- 2014-06-21 CN CN201410281576.XA patent/CN104069793A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CA2009731A1 (en) * | 1989-02-11 | 1990-08-11 | Carl-Ernst Van Der Smissen | Process for the production of an absorption mass for carbon dioxide |
| CN1189814A (en) * | 1996-04-24 | 1998-08-05 | 矢桥工业株式会社 | Process for producing clacium hydroxide |
| CN101254935A (en) * | 2008-04-03 | 2008-09-03 | 武汉工程大学 | Method for preparing calcium hydroxide with high purity and high activity |
Non-Patent Citations (1)
| Title |
|---|
| 侯瑞琴等: ""纳米氢氧化钙颗粒制备、表征及NOx捕获性能研究"", 《非金属矿》, vol. 33, no. 5, 30 September 2010 (2010-09-30), pages 5 - 6 * |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106111082A (en) * | 2016-04-25 | 2016-11-16 | 河池学院 | Highly active CO2adsorbent and preparation method thereof |
| CN106111082B (en) * | 2016-04-25 | 2019-01-29 | 河池学院 | The CO of high activity2Adsorbent and preparation method thereof |
| CN109052608A (en) * | 2018-08-07 | 2018-12-21 | 米易东立矿业有限公司 | Sulfuric acid method titanium pigment waste water treating agent and preparation method thereof |
| CN109052608B (en) * | 2018-08-07 | 2022-08-30 | 米易东立矿业有限公司 | Sulfuric acid method titanium dioxide wastewater treating agent and preparation method thereof |
| CN109261117A (en) * | 2018-08-08 | 2019-01-25 | 河南工程学院 | A kind of preparation method loading spherical nanometer calcium salt oxidizing agent based on rectorite |
| 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 |
| CN111185136A (en) * | 2020-01-18 | 2020-05-22 | 中国人民解放军火箭军工程大学 | Dinitrogen tetroxide absorbent, preparation method and application |
| CN111250041A (en) * | 2020-01-18 | 2020-06-09 | 中国人民解放军火箭军工程大学 | Propellant processing bag and preparation method and application thereof |
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Application publication date: 20141001 |