CN100443416C - Preparation method of hydroxylation cobalt and its application in water treatment - Google Patents
Preparation method of hydroxylation cobalt and its application in water treatment Download PDFInfo
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- CN100443416C CN100443416C CNB2006101512337A CN200610151233A CN100443416C CN 100443416 C CN100443416 C CN 100443416C CN B2006101512337 A CNB2006101512337 A CN B2006101512337A CN 200610151233 A CN200610151233 A CN 200610151233A CN 100443416 C CN100443416 C CN 100443416C
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- Prior art keywords
- cobalt
- hydroxylating
- preparation
- hydroxylated
- solution
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 229910017052 cobalt Inorganic materials 0.000 title claims description 47
- 239000010941 cobalt Substances 0.000 title claims description 47
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 title claims description 47
- 230000033444 hydroxylation Effects 0.000 title 1
- 238000005805 hydroxylation reaction Methods 0.000 title 1
- 239000000725 suspension Substances 0.000 claims abstract description 7
- 239000012153 distilled water Substances 0.000 claims abstract description 4
- 230000000640 hydroxylating effect Effects 0.000 claims description 36
- 239000003513 alkali Substances 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 7
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 238000001556 precipitation Methods 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 4
- 238000007605 air drying Methods 0.000 claims description 3
- 230000007935 neutral effect Effects 0.000 claims description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 2
- 241000220317 Rosa Species 0.000 claims description 2
- GVPFVAHMJGGAJG-UHFFFAOYSA-L cobalt dichloride Chemical compound [Cl-].[Cl-].[Co+2] GVPFVAHMJGGAJG-UHFFFAOYSA-L 0.000 claims description 2
- ZBDSFTZNNQNSQM-UHFFFAOYSA-H cobalt(2+);diphosphate Chemical compound [Co+2].[Co+2].[Co+2].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O ZBDSFTZNNQNSQM-UHFFFAOYSA-H 0.000 claims description 2
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 abstract description 22
- 230000003197 catalytic effect Effects 0.000 abstract description 9
- 239000003795 chemical substances by application Substances 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 5
- 239000000203 mixture Substances 0.000 abstract description 3
- 239000002245 particle Substances 0.000 abstract description 2
- 150000001868 cobalt Chemical class 0.000 abstract 9
- 239000013049 sediment Substances 0.000 abstract 2
- 239000012670 alkaline solution Substances 0.000 abstract 1
- 239000000356 contaminant Substances 0.000 abstract 1
- 239000013078 crystal Substances 0.000 abstract 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract 1
- 239000012535 impurity Substances 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- 230000001376 precipitating effect Effects 0.000 abstract 1
- 239000012266 salt solution Substances 0.000 abstract 1
- 239000002957 persistent organic pollutant Substances 0.000 description 10
- CZGCEKJOLUNIFY-UHFFFAOYSA-N 4-Chloronitrobenzene Chemical compound [O-][N+](=O)C1=CC=C(Cl)C=C1 CZGCEKJOLUNIFY-UHFFFAOYSA-N 0.000 description 7
- 230000000694 effects Effects 0.000 description 2
- 230000008030 elimination Effects 0.000 description 2
- 238000003379 elimination reaction Methods 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000006385 ozonation reaction Methods 0.000 description 2
- 230000035484 reaction time Effects 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 229910018916 CoOOH Inorganic materials 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 230000008878 coupling Effects 0.000 description 1
- 238000010168 coupling process Methods 0.000 description 1
- 238000005859 coupling reaction Methods 0.000 description 1
- -1 hydroxyl radical free radical Chemical class 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000002203 pretreatment Methods 0.000 description 1
- 150000003254 radicals Chemical class 0.000 description 1
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Abstract
This invention discloses a preparation method of hydroxylated cobalt and its application in water treatment. It relates to a preparation method of mixture and its application in water treatment. It is first time to disclose a preparation method of hydroxylated cobalt and its application in water treatment. Prepare hydroxylated cobalt: 1. add alkaline solution into divalence cobalt salt solution until no sediment emerging; 2. adjust suspension PH more than 12, activate; 3. filter, wash sediment to neutrality with distilled water, dry, and get hydroxylated cobalt. Hydroxylated cobalt is used as ozone catalytic agent for water treatment technology. This hydroxylated cobalt is of integrated and uniform particle crystal form, and uniform grain size. This invention avoids impurity precipitating. Hydroxylated cobalt purity reaches more than 99%. Hydroxylated cobalt can promote ozone to transform into hydroxy group free radicle, increase production rate and quantity of free radicle that is in water body. Ability of ozone removing organic contaminant that is in water can be raised 35-42%.
Description
Technical field
The present invention relates to a kind of preparation process of mixture.
Background technology
Hydroxylating cobalt is a kind of mixture, by Co (OH)
2Form with CoOOH.The report that hydroxylating cobalt preparation method or application are not arranged at present as yet.
Summary of the invention
The present invention discloses a kind of preparation method of hydroxylating cobalt first.Hydroxylating cobalt prepares according to the following steps: (one) constantly stirs the solubility divalent cobalt solution that concentration is 0.2mol/L～2.0mol/L, and slowly to drip concentration be that the strong alkali solution of 0.25mol/L～2.1mol/L does not produce until there being precipitation; (2) pH value＞12 of suspension liquid that regulating step one becomes place 30 ℃～100 ℃ environment to activate 12～20h then; (3) filter, throw out is washed with distilled water to neutral after drying, promptly obtain hydroxylating cobalt.
The hydroxylating cobalt particle crystalline form of the present invention preparation is complete, even compact and size distribution are even.Hydroxylating cobalt of the present invention has adopted alkali formula Preparation by Uniform Precipitation to avoid contamination precipitation, and hydroxylating cobalt purity reaches more than 99%.Hydroxylating cobalt can promote that ozone changes into hydroxyl radical free radical, increases the generating rate and the quantity of free radical in the water body, has improved the oxidisability and the utilization ratio of ozone, and the ability that ozone is removed organic pollutant in the water can be enhanced 35～42 percentage points.Agent has catalytic elimination organic pollutant activity by force to hydroxylating cobalt as ozone catalytic, and the self stability height does not produce the advantage of secondary pollution.
Description of drawings
Fig. 1 is the design sketch that embodiment 19 contrast experiments remove organic pollutant parachloronitrobenzene in the water, and the ■ curve representation adds the organic pollutant removal rate curve of ozone and catalyzer hydroxylating cobalt among the figure; Among the figure ◆ curve representation only adds the organic pollutant removal rate curve of ozone; Among the figure ▲ curve representation catalyzer hydroxylating cobalt is adsorbed with the organic pollutants curve.
Embodiment
Embodiment one: the present embodiment hydroxylating cobalt prepares according to the following steps: (one) constantly stirs the solubility divalent cobalt solution that concentration is 0.2mol/L～2.0mol/L, and slowly to drip concentration be that the strong alkali solution of 0.25mol/L～2.1mol/L does not produce until there being precipitation; (2) regulating step () becomes pH value＞12 of suspension liquid, places 30 ℃～100 ℃ environment to activate 12～20h then; (3) filter, throw out is washed with distilled water to neutral after drying, promptly obtains hydroxylating cobalt.
Throw out is dark pink colour in the present embodiment.
Embodiment two: the difference of present embodiment and embodiment one is: the concentration of solubility divalent cobalt solution is 0.5mol/L～1.5mol/L in the step ().Other step is identical with embodiment one.
Embodiment three: the difference of present embodiment and embodiment one is: the concentration of solubility divalent cobalt solution is 0.7mol/L～1.3mol/L in the step ().Other step is identical with embodiment one.
Embodiment four: the difference of present embodiment and embodiment one is: the concentration of strong alkali solution is 0.6mol/L～1.6mol/L in the step ().Other step is identical with embodiment one.
Embodiment five: the difference of present embodiment and embodiment one is: the concentration of strong alkali solution is 1.0mol/L～1.2mol/L in the step ().Other step is identical with embodiment one.
Embodiment six: the difference of present embodiment and embodiment one is: solubility divalent cobalt solution is Xiao Suangu, rose vitriol, cobalt chloride or cobaltous phosphate solution in the step ().Other step is identical with embodiment one.
Embodiment seven: the difference of present embodiment and embodiment one is: strong alkali solution is sodium hydroxide or potassium hydroxide solution in the step ().Other step is identical with embodiment one.
Embodiment eight: the difference of present embodiment and embodiment one is: regulate in the step (two) in the environment that suspension liquid pH value is placed on 40 ℃～90 ℃ and activate 13～18h.Other step is identical with embodiment one.
Embodiment nine: the difference of present embodiment and embodiment one is: regulate in the step (two) in the environment that suspension liquid pH value is placed on 50 ℃～80 ℃ and activate 15～17h.Other step is identical with embodiment one.
Embodiment ten: the difference of present embodiment and embodiment one is: dry or the natural air drying throw out under 30 ℃～120 ℃ condition in the step (three).Other step is identical with embodiment one.
Embodiment 11: the difference of present embodiment and embodiment one is: dry or the natural air drying throw out under 50 ℃～100 ℃ condition in the step (three).Other step is identical with embodiment one.
Embodiment 12: the difference of present embodiment and embodiment one is: adopt power to stir divalent cobalt solution in the step (), stirring intensity is 100r/min～300r/min.Other step is identical with embodiment one.
Embodiment 13: agent is applied to water technology to the present embodiment hydroxylating cobalt as ozone catalytic.
Water pretreatment in the present embodiment, pre-treatment and aftertreatment technology are identical with existing water treatment method.In the present embodiment ozone can with other gaseous oxidizer coupling (as oxygen and chlorine).
Embodiment 14: the difference of present embodiment and embodiment 13 is: the ozone dosage is 0.5～3mg/L, and the hydroxylating cobalt dosage is 50～150mg/L.Other is identical with embodiment 13.
The dosage that increases ozone or hydroxylating cobalt can improve the clearance of organic pollutant, but cost of water treatment is too high.
Embodiment 15: the difference of present embodiment and embodiment 13 is: the ozone dosage is 1mg/L, and the hydroxylating cobalt dosage is 60～90mg/L.Other is identical with embodiment 13.
Embodiment 16: the difference of present embodiment and embodiment 13 is: the ozone dosage is 2mg/L, and the hydroxylating cobalt dosage is 75mg/L.Other is identical with embodiment 13.
Embodiment 17: the difference of present embodiment and embodiment 13 is: the catalytic ozonation reaction times is 15～25min.Other is identical with embodiment 13.
Embodiment 18: the difference of present embodiment and embodiment 13 is: the catalytic ozonation reaction times is 20min.Other is identical with embodiment 13.
Embodiment 19: agent is applied to water technology to the present embodiment hydroxylating cobalt as ozone catalytic, and the ozone dosage is 0.9mg/L, and the hydroxylating cobalt dosage is 100mg/L.
The contrast experiment:
Remove the organic pollutant parachloronitrobenzene (pCNB) of same concentrations in the water respectively, one group adds ozone separately, and the ozone dosage is 0.9mg/L; Another group adds ozone and catalyzer hydroxylating cobalt, and the ozone dosage is 0.9mg/L, and the hydroxylating cobalt dosage is 100mg/L; The removal effect of parachloronitrobenzene (pCNB) as shown in Figure 1 in two groups of water.The adding of ozone catalytic agent hydroxylating cobalt makes parachloronitrobenzene clearance (reaction 20min) improve 38.5 percentage points, and the catalyzer hydroxylating cobalt is not adsorbed with organic pollutants (parachloronitrobenzene).Experimental data explanation catalytic elimination organic pollutant is active strong, the self stability height.
Claims (8)
1, the preparation method of hydroxylating cobalt, it is characterized in that hydroxylating cobalt prepares according to the following steps: (one) constantly stirs the solubility divalent cobalt solution that concentration is 0.2mol/L～2.0mol/L, and slowly to drip concentration be that the strong alkali solution of 0.25mol/L～2.1mol/L does not produce until there being precipitation; (2) regulating step () becomes pH value＞12 of suspension liquid, places 30 ℃～100 ℃ environment to activate 12～20h then; (3) filter, throw out is washed with distilled water to neutral after drying, promptly obtain hydroxylating cobalt.
2, the preparation method of hydroxylating cobalt according to claim 1 is characterized in that the concentration of solubility divalent cobalt solution in the step () is 0.5mol/L～1.5mol/L.
3, the preparation method of hydroxylating cobalt according to claim 1 is characterized in that the concentration of strong alkali solution in the step () is 0.6mol/L～1.6mol/L.
4, the preparation method of hydroxylating cobalt according to claim 1 is characterized in that adopting in the step () power to stir divalent cobalt solution, and stirring intensity is 100r/min～300r/min.
5, the preparation method of hydroxylating cobalt according to claim 1 is characterized in that solubility divalent cobalt solution is Xiao Suangu, rose vitriol, cobalt chloride or cobaltous phosphate solution in the step ().
6, the preparation method of hydroxylating cobalt according to claim 1 is characterized in that strong alkali solution is sodium hydroxide or potassium hydroxide solution in the step ().
7, the preparation method of hydroxylating cobalt according to claim 1 is characterized in that regulating in the step (two) in the environment that suspension liquid pH value is placed on 40 ℃～90 ℃ and activates 13～18h.
8, the preparation method of hydroxylating cobalt according to claim 1 is characterized in that drying or the natural air drying throw out under 30 ℃～120 ℃ condition in the step (three).
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| CNB2006101512337A CN100443416C (en) | 2006-12-31 | 2006-12-31 | Preparation method of hydroxylation cobalt and its application in water treatment |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB2006101512337A CN100443416C (en) | 2006-12-31 | 2006-12-31 | Preparation method of hydroxylation cobalt and its application in water treatment |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2008101288082A Division CN101323479B (en) | 2006-12-31 | 2006-12-31 | Use of hydroxylating cobalt in water treatment |
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| CN100999337A CN100999337A (en) | 2007-07-18 |
| CN100443416C true CN100443416C (en) | 2008-12-17 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102718299A (en) * | 2012-07-09 | 2012-10-10 | 青岛理工大学 | Method for preparing efficient coagulation dephosphorization agent |
| CN103408124B (en) * | 2013-08-05 | 2015-07-08 | 东华大学 | Method for treating printing and dyeing wastewater through catalytic oxidation |
| CN105869892B (en) * | 2016-04-05 | 2018-03-06 | 上海交通大学 | A kind of High-performance graphene membrane electrode and preparation method thereof |
| CN110331416B (en) * | 2019-08-09 | 2020-07-24 | 河南大学 | CoOOH nanosheet modified Fe2O3Preparation method and application of composite photo-anode |
| CN112844386B (en) * | 2020-12-25 | 2021-12-24 | 湖南大学 | Preparation method and application of trace boron-doped cobalt oxyhydroxide |
| CN113385174B (en) * | 2021-07-17 | 2022-08-26 | 安徽农业大学 | Cobalt modified hydrated iron oxide catalyst and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1559938A (en) * | 2004-03-03 | 2005-01-05 | 哈尔滨工业大学 | Process for water supply deep treatment of catalyzing ozone oxydation by hydroxy ferric oxide as catalyst |
| US7141173B2 (en) * | 2003-12-19 | 2006-11-28 | Bethke Craig M | In situ treatment process to remove metal contamination from groundwater |
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- 2006-12-31 CN CNB2006101512337A patent/CN100443416C/en not_active Expired - Fee Related
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US7141173B2 (en) * | 2003-12-19 | 2006-11-28 | Bethke Craig M | In situ treatment process to remove metal contamination from groundwater |
| CN1559938A (en) * | 2004-03-03 | 2005-01-05 | 哈尔滨工业大学 | Process for water supply deep treatment of catalyzing ozone oxydation by hydroxy ferric oxide as catalyst |
Non-Patent Citations (4)
| Title |
|---|
| "羟基"氧化在水处理技术中的应用. 张锦.化学工程师，第99卷第6期. 2003 |
| "羟基"氧化在水处理技术中的应用. 张锦.化学工程师，第99卷第6期. 2003 * |
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| 水处理中的羟基自由基·OH. 李明波，申欢，崔喜勤等.陕西环境，第10卷第4期. 2003 * |
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