CN101791535A - Method for preparing manganese polysilicate doped manganese dioxide adsorbent - Google Patents
Method for preparing manganese polysilicate doped manganese dioxide adsorbent Download PDFInfo
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- CN101791535A CN101791535A CN 201010158528 CN201010158528A CN101791535A CN 101791535 A CN101791535 A CN 101791535A CN 201010158528 CN201010158528 CN 201010158528 CN 201010158528 A CN201010158528 A CN 201010158528A CN 101791535 A CN101791535 A CN 101791535A
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Abstract
The invention discloses a method for preparing a manganese polysilicate doped manganese dioxide adsorbent, which relates to a method for preparing an adsorbent and application thereof. The method solves the problems that manganese dioxide has poor removal capacity and poor settleability to dimethylamine. The method for preparing the manganese polysilicate doped manganese dioxide adsorbent comprises the following steps of: firstly, preparing a product A; secondly, preparing a product B; and thirdly, adding deionized water into the product B until the product B is pyrolyzed into particles, then removing suspended matters, and drying the particles to obtain the manganese polysilicate doped manganese dioxide adsorbent. The manganese polysilicate doped manganese dioxide adsorbent is applied to water treatments to remove the dimethylamine in water. The adsorbent prepared by the method is an amorphous crystal, and the specific surface area of the adsorbent is 152.79 m<2>/g which is 3 times that of commercially available manganese dioxide. The manganese polysilicate doped manganese dioxide adsorbent can effectively remove the dimethylamine in the water, and has the characteristics of high self stability, simple and convenient method, no need of high-temperature drying, easy recycling and no generation of secondary pollutions.
Description
Technical field
The present invention's invention relates to a kind of preparation of adsorbent method and application.
Background technology
Dimethylamine is the most direct antecedent of nitrosodimethylamine, is a kind of simple short-chain fat amine, the normal trace of this class material be present in environmental sample, in biological fluid and the industrial waste.At normal temperatures and pressures, dimethylamine is a colourless gas has harm to the health of human body.Ozone and other advanced oxidization methods can be removed dimethylamine, but these processing methods can cause the generation of a certain amount of nitrosodimethylamine.
Utilize manganese dioxide to can be used to adsorb heavy metal and the organic matter of removing in the water for the natural manganese ore of main component.The catalysis of artificial synthetic Mn oxide and adsorption capacity can be removed arsenic in the water, agricultural chemicals atrazine, organic dyestuff etc.At present, nascent state manganese dioxide is because characteristics such as its grain diameter is little, dispersed height, high adsorption capacity become the focus of wastewater treatment research gradually.Yet through experimental results demonstrate, commercially available manganese dioxide and nascent state manganese dioxide are indifferent to the removal of dimethylamine, and settleability is relatively poor.In addition, the artificial synthetic manganese dioxide of report maybe need adopt the condition of HTHP at present, needs to consume a large amount of energy; Or the preparation condition complexity, length consuming time.
Summary of the invention
Goal of the invention of the present invention is in order to solve manganese dioxide to the relatively poor problem of removal ability, the settleability of dimethylamine, a kind of preparation method and application of manganese polysilicate doped manganese dioxide adsorbent to be provided.
The preparation method of manganese polysilicate doped manganese dioxide adsorbent of the present invention is as follows: be the ratio of 1.6～4 ﹕ 1 according to potassium permanganate and sodium salt mol ratio one,, mixing speed with 100r/min～300r/min splashes into liquor potassic permanganate in the sodium salt solution while stirring, continue then to stir 30min, promptly get product A with the mixing speed of 100r/min～300r/min; Two, silicate is joined in the product A than the ratio that is 1 ﹕ 1 according to product A and silicate quality, quiet heavy 10min～30min, under 40 ℃～60 ℃ condition, activate 24h～48h again, remove the upper strata settled solution then, with deionized water washing sediment to washing lotion pH value is 8～10, again that sediment is dry under 60 ℃ condition, get product B; Three, in product B, add deionized water to product B and be cracked into graininess, spend deionised water then and repeatedly remove suspension, dry under 60 ℃ condition again, promptly get manganese polysilicate doped manganese dioxide adsorbent; Sodium salt described in the step 1 is sodium thiosulfate or sodium sulfite; Silicate described in the step 2 is sodium metasilicate or potassium silicate.
The application of manganese polysilicate doped manganese dioxide adsorbent in water treatment is used for removing the dimethylamine of water.
Manganese polysilicate doped manganese dioxide adsorbent uniform particles of the present invention densification and even aperture distribution are about 8nm.Adsorbent of the present invention is a metamict crystals, and specific area is 152.79m
2/ g is three times of commercially available manganese dioxide.Adsorbent of the present invention is behind adsorption reaction 24h, and the manganese stripping quantity only is 0.03～0.04mg/L in the water, far below national drinking water standard (0.1mg/L).The manganese polysilicate doped manganese dioxide adsorbent of invention is joined in the sewage that contains dimethylamine according to the dosage of 0.5g/L, and preceding 5h manganese polysilicate doped manganese dioxide adsorbent can adsorb dimethylamine fast, and absorption can reach balance behind the 18h.When the absorption initial concentration was the dimethylamine of 1.125mg/L, the dimethylamine residual concentration only was 7 μ g/L after the adsorption equilibrium; When absorption high concentration dimethylamine (22.5mg/L), the adsorbance behind the 24h is more than 43%.Manganese polysilicate doped manganese dioxide adsorbent of the present invention can be removed the dimethylamine that exists in the water effectively, has the self stability height, and method is easy, does not need hyperthermia drying, is easy to recycle, and does not produce the characteristics of secondary pollution.
Description of drawings
Fig. 1 be in the specific embodiment 11 manganese polysilicate doped manganese dioxide adsorbent to the design sketch of dimethylamine clearance, among the figure-■-expression manganese polysilicate doped manganese dioxide adsorbent is the clearance curve of 1.125mg/L dimethylamine to initial concentration;-●-expression manganese polysilicate doped manganese dioxide adsorbent is the clearance curve of 4.5mg/L dimethylamine to initial concentration;-▲-expression manganese polysilicate doped manganese dioxide adsorbent is the clearance curve of 11.25mg/L dimethylamine to initial concentration;-▼-expression manganese polysilicate doped manganese dioxide adsorbent is the clearance curve of 22.5mg/L dimethylamine to initial concentration.Fig. 2 is the XRD figure of manganese polysilicate doped manganese dioxide adsorbent in the specific embodiment 11.
The specific embodiment
Technical solution of the present invention is not limited to the following cited specific embodiment, also comprises any combination between each specific embodiment.
The specific embodiment one: the preparation method of manganese polysilicate doped manganese dioxide adsorbent is as follows in the present embodiment: be the ratio of 1.6～4 ﹕ 1 according to potassium permanganate and sodium salt mol ratio one,, mixing speed with 100r/min～300r/min splashes into liquor potassic permanganate in the sodium salt solution while stirring, continue then to stir 30min, promptly get product A with the mixing speed of 100r/min～300r/min; Two, silicate is joined in the product A than the ratio that is 1 ﹕ 1 according to product A and silicate quality, quiet heavy 10min～30min, under 40 ℃～60 ℃ condition, activate 24h～48h again, remove the upper strata settled solution then, with deionized water washing sediment to washing lotion pH value is 8～10, again that sediment is dry under 60 ℃ condition, get product B; Three, in product B, add deionized water to product B and be cracked into graininess, spend deionised water then and repeatedly remove suspension, dry under 60 ℃ condition again, promptly get manganese polysilicate doped manganese dioxide adsorbent; Sodium salt described in the step 1 is sodium thiosulfate or sodium sulfite; Silicate described in the step 2 is sodium metasilicate or potassium silicate.
The manganese polysilicate doped manganese dioxide adsorbent uniform particles densification of present embodiment preparation and even aperture distribution are about 8nm.Manganese dioxide is added to the water, and manganese dioxide can be cracked behind vibration absorption 24h, becomes suspension manganese dioxide and make and present pale brown look in the water.After the manganese polysilicate doped manganese dioxide adsorbent that adopts present embodiment to prepare adds in the entry, behind the oscillating reactions 24h above phenomenon can not appear, the proof manganese polysilicate doped manganese dioxide adsorbent has tangible lifting in hardness, intensity with respect to manganese dioxide, is more suitable for water treatment applications.
Manganese polysilicate doped manganese dioxide adsorbent is a metamict crystals, and specific area is 152.79m
2/ g is three times of commercially available manganese dioxide.This adsorbent is behind adsorption reaction 24h, and the manganese stripping quantity only is 0.03mg/L～0.04mg/L in the water, far below national drinking water standard (0.1mg/L).
The specific embodiment two: present embodiment and the specific embodiment one are different is that the mol ratio of potassium permanganate and sodium salt is 2～3 ﹕ 1 in the step 1.Other is identical with the specific embodiment one.
The specific embodiment three: present embodiment is different with one of the specific embodiment one or two is that the mol ratio of potassium permanganate and sodium salt is 2.5 ﹕ 1 in the step 1.Other is identical with one of the specific embodiment one or two.
The specific embodiment four: what present embodiment was different with one of specific embodiment one to three is that the speed that stirs in the step 1 is 150r/min～250r/min.Other is identical with one of specific embodiment one to three.
The specific embodiment five: what present embodiment was different with one of specific embodiment one to four is that the speed that stirs in the step 1 is 200r/min.Other is identical with one of specific embodiment one to four.
The specific embodiment six: present embodiment is different with one of specific embodiment one to five is that quiet heavy time in the step 2 is 15min～25min.Other is identical with one of specific embodiment one to five.
The specific embodiment seven: what present embodiment was different with one of specific embodiment one to six is to activate under 50 ℃ condition in the step 2.Other is identical with one of specific embodiment one to six.
The specific embodiment eight: what present embodiment was different with one of specific embodiment one to seven is that soak time is 30h in the step 2.Other is identical with one of specific embodiment one to seven.
The specific embodiment nine: present embodiment is different with one of specific embodiment one to eight is to be 9 with deionized water washing sediment to washing lotion pH value in the step 2.Other is identical with one of specific embodiment one to eight.
The specific embodiment ten: the application of manganese polysilicate doped manganese dioxide adsorbent in water treatment in the present embodiment is used for removing the dimethylamine of water.
The specific embodiment 11: the preparation method of manganese polysilicate doped manganese dioxide adsorbent is as follows in the present embodiment: be the ratio of 8 ﹕ 3 according to potassium permanganate and sodium thiosulfate mol ratio one,, with the mixing speed of 100r/min～300r/min is that the liquor potassic permanganate of 18.17g/L splashes in the hypo solution that concentration is 6.794g/L while stirring with concentration, continue then to stir 30min, promptly get product A with the mixing speed of 100r/min～300r/min; Two, be that the ratio of 1 ﹕ 1 joins the 10g sodium metasilicate in the product A according to product A and sodium metasilicate mass ratio, quiet heavy 10min～30min, under 40 ℃ condition, activate 48h again, remove the upper strata settled solution then, with deionized water washing sediment to washing lotion pH value is 9.5, again that sediment is dry under 60 ℃ condition, get product B; Three, in product B, add deionized water to product B and be cracked into graininess, spend deionised water then and repeatedly remove suspension, dry under 60 ℃ condition again, promptly get manganese polysilicate doped manganese dioxide adsorbent.
The manganese polysilicate doped manganese dioxide adsorbent uniform particles densification of present embodiment preparation and even aperture distribution are about 8nm.Manganese dioxide is added to the water, and manganese dioxide can be cracked behind vibration absorption 24h, becomes suspension manganese dioxide and make and present pale brown look in the water.After the manganese polysilicate doped manganese dioxide adsorbent that adopts present embodiment to prepare adds in the entry, behind the oscillating reactions 24h above phenomenon can not appear, the proof manganese polysilicate doped manganese dioxide adsorbent has tangible lifting in hardness, intensity with respect to manganese dioxide, is more suitable for water treatment applications.
Manganese polysilicate doped manganese dioxide adsorbent is a metamict crystals, and specific area is 152.79m
2/ g is three times of commercially available manganese dioxide.This adsorbent is behind adsorption reaction 24h, and the manganese stripping quantity only is 0.03mg/L～0.04mg/L in the water, far below national drinking water standard (0.1mg/L).
The manganese polysilicate doped manganese dioxide adsorbent of the present embodiment preparation dosage according to 0.5g/L is joined in the sewage that contains dimethylamine, preceding as seen from Figure 1 5h manganese polysilicate doped manganese dioxide adsorbent can adsorb dimethylamine fast, and absorption can reach balance behind the 18h.When the absorption initial concentration was the dimethylamine of 1.125mg/L, the dimethylamine residual concentration only was 7 μ g/L after the adsorption equilibrium; When absorption high concentration dimethylamine (22.5mg/L), the adsorbance behind the 24h is more than 43%.Because contained dimethylamine concentration generally is in about 100 μ g/L in the actual water body, so should the throwing amount can effectively remove the dimethylamine that exists in the water.
The manganese polysilicate doped manganese dioxide adsorbent that is drawn the present embodiment preparation by Fig. 2 is unformed.
Claims (10)
1. the preparation method of manganese polysilicate doped manganese dioxide adsorbent, the preparation method who it is characterized in that manganese polysilicate doped manganese dioxide adsorbent is as follows: be the ratio of 1.6～4 ﹕ 1 according to potassium permanganate and sodium salt mol ratio one,, mixing speed with 100r/min～300r/min splashes into liquor potassic permanganate in the sodium salt solution while stirring, continue then to stir 30min, promptly get product A with the mixing speed of 100r/min～300r/min; Two, silicate is joined in the product A than the ratio that is 1 ﹕ 1 according to product A and silicate quality, quiet heavy 10min～30min, under 40 ℃～60 ℃ condition, activate 24h～48h again, remove the upper strata settled solution then, with deionized water washing sediment to washing lotion pH value is 8～10, again that sediment is dry under 60 ℃ condition, get product B; Three, in product B, add deionized water to product B and be cracked into graininess, spend deionised water then and repeatedly remove suspension, dry under 60 ℃ condition again, promptly get manganese polysilicate doped manganese dioxide adsorbent; Sodium salt described in the step 1 is sodium thiosulfate or sodium sulfite; Silicate described in the step 2 is sodium metasilicate or potassium silicate.
2. the preparation method of manganese polysilicate doped manganese dioxide adsorbent according to claim 1 is characterized in that the mol ratio of potassium permanganate and sodium salt is 2～3 ﹕ 1 in the step 1.
3. the preparation method of manganese polysilicate doped manganese dioxide adsorbent according to claim 1 is characterized in that the mol ratio of potassium permanganate and sodium salt is 2.5 ﹕ 1 in the step 1.
4. the preparation method of manganese polysilicate doped manganese dioxide adsorbent according to claim 1 and 2 is characterized in that the speed that stirs in the step 1 is 150r/min～250r/min.
5. the preparation method of manganese polysilicate doped manganese dioxide adsorbent according to claim 1 and 2 is characterized in that the speed that stirs in the step 1 is 200r/min.
6. the preparation method of manganese polysilicate doped manganese dioxide adsorbent according to claim 4 is characterized in that the quiet heavy time in the step 2 is 15min～25min.
7. according to the preparation method of claim 1,2 or 6 described manganese polysilicate doped manganese dioxide adsorbents, it is characterized in that under 50 ℃ condition, activating in the step 2.
8. the preparation method of manganese polysilicate doped manganese dioxide adsorbent according to claim 7 is characterized in that soak time is 30h in the step 2.
9. according to the preparation method of claim 1,2,6 or 8 described manganese polysilicate doped manganese dioxide adsorbents, it is characterized in that in the step 2 with deionized water washing sediment to washing lotion pH value being 9.
10. the application of manganese polysilicate doped manganese dioxide adsorbent is characterized in that the application of described manganese polysilicate doped manganese dioxide adsorbent in water treatment, is used for removing the dimethylamine of water.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103933968A (en) * | 2014-03-18 | 2014-07-23 | 中原工学院 | Preparation method and application of polymanganese silicate doped hydroxy manganese oxide catalyst |
| CN109824056A (en) * | 2019-04-04 | 2019-05-31 | 河北工业大学 | The method for preparing the compound selective absorbent of nano-sheet manganous silicate using iron tailings |
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| US4227023A (en) * | 1977-12-13 | 1980-10-07 | Mitsui Toatsu Chemicals, Incorporated | Process for the selective ortho-alkylation of phenolic compounds |
| CN1625538A (en) * | 2002-01-29 | 2005-06-08 | 埃克森美孚研究工程公司 | Catalyst enhancement |
| CN1750876A (en) * | 2002-01-29 | 2006-03-22 | 埃克森美孚研究工程公司 | Catalyst regeneration |
| CN1812835A (en) * | 2003-04-29 | 2006-08-02 | 约翰逊马西有限公司 | Manganese ozone decomposition catalysts and process for its preparation |
| CN101690882A (en) * | 2009-10-14 | 2010-04-07 | 南开大学 | Natural adsorbent for removing heavy metal ions in water and preparation method and application thereof |
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2010
- 2010-04-28 CN CN2010101585283A patent/CN101791535B/en not_active Expired - Fee Related
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4227023A (en) * | 1977-12-13 | 1980-10-07 | Mitsui Toatsu Chemicals, Incorporated | Process for the selective ortho-alkylation of phenolic compounds |
| CN1625538A (en) * | 2002-01-29 | 2005-06-08 | 埃克森美孚研究工程公司 | Catalyst enhancement |
| CN1750876A (en) * | 2002-01-29 | 2006-03-22 | 埃克森美孚研究工程公司 | Catalyst regeneration |
| CN1812835A (en) * | 2003-04-29 | 2006-08-02 | 约翰逊马西有限公司 | Manganese ozone decomposition catalysts and process for its preparation |
| CN101690882A (en) * | 2009-10-14 | 2010-04-07 | 南开大学 | Natural adsorbent for removing heavy metal ions in water and preparation method and application thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103933968A (en) * | 2014-03-18 | 2014-07-23 | 中原工学院 | Preparation method and application of polymanganese silicate doped hydroxy manganese oxide catalyst |
| CN103933968B (en) * | 2014-03-18 | 2015-06-24 | 中原工学院 | Preparation method and application of polymanganese silicate doped hydroxy manganese oxide catalyst |
| CN109824056A (en) * | 2019-04-04 | 2019-05-31 | 河北工业大学 | The method for preparing the compound selective absorbent of nano-sheet manganous silicate using iron tailings |
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