CN101559353B - Preparation method of zinc chloride modified red mud - Google Patents
Preparation method of zinc chloride modified red mud Download PDFInfo
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- CN101559353B CN101559353B CN2009100151335A CN200910015133A CN101559353B CN 101559353 B CN101559353 B CN 101559353B CN 2009100151335 A CN2009100151335 A CN 2009100151335A CN 200910015133 A CN200910015133 A CN 200910015133A CN 101559353 B CN101559353 B CN 101559353B
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- red mud
- zinc chloride
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Abstract
The invention relates to a preparation method of zinc chloride modified red mud, comprising the steps of taking red mud and zinc chloride as primary raw materials and adopting stirring method in thermostatic waterbath to prepare the modified red mud. The zinc chloride modified red mud prepared by the invention has excellent adsorbability, short synthetic processing time, simple synthetic process and low energy consumption; the obtained zinc chloride solution modified red mud product has stable quality, uniform appearance, lower cost and good effect on processing phosphorus-containing wastewater.
Description
Technical field
The present invention relates to a kind of zinc chloride modified red mud and preparation method thereof, is that adsorbent is used for sewage dephosphorization with the changed red mud, belongs to technical field of chemistry.
Background technology
The preparation research of changed red mud is the focus and the field, forward position of absorption research both at home and abroad at present.Red mud is carried out modification, mainly is by physics and chemical mode, changes the space structure of red mud and the composition and the content of chemical composition.
At present China's changed red mud preparation method commonly used is comparatively narrow, is mainly that modification by calcination changes, hydrochloric acid modification and iron chloride modification.And zinc chloride---as the metal inorganic salt activator, have the mineral surfaces of change chemical composition, eliminate the effect of inhibitor.Originally discover, the red mud volumetric expansion after zinc chloride modified, surface texture coarse (by scanning electron microscopic observation) is done adsorbent for phosphate removal with zinc chloride modified red mud, and its adsorption effect is better than unmodified red mud and with the red mud of above-mentioned other mode modifications.Therefore, adopt zinc chloride that red mud is carried out modification, to solve the utilization of red mud changing waste into resources, to improve the adsorption capacity of red mud in waste water dephosphorization significant.
Summary of the invention
The present invention is directed to the not high problem of red mud dephosphorization absorption affinity in the existing sewage disposal, a kind of preparation method of zinc chloride modified red mud is provided.
Technical scheme of the present invention is as follows:
A kind of preparation method of zinc chloride modified red mud is a raw material with red mud and zinc chloride, and step is as follows:
(1) red mud 5g is placed the triangle round-bottomed flask, add 0.1～0.4mol/L ZnCl
2Solution 100mL.
(2) above-mentioned round-bottomed flask is placed thermostat water bath, regulating temperature is 20～40 ℃, stirring reaction 1～4h.
(3) behind the suction filtration reactant liquor zinc chloride modified red mud, to chloride ion-containing not, 105 ℃ of oven dry are ground, and cross 100 mesh sieves, promptly get the zinc chloride modified red mud product with distilled water washing zinc chloride modified red mud.
Above-mentioned steps (3) washing zinc chloride modified red mud to filtrate not the detection method of chloride ion-containing be: the silver nitrate that drips 0.1mol/L in eluate generates to there being white precipitate.
Red mud raw material that the present invention adopts and zinc chloride (analyzing pure) but equal market buy.
Preferred process conditions are to add 0.3mol/LZnCl in the step (1)
2Temperature is 30 ℃ in the solution, step (2), stirs 1h.
The zinc chloride modified red mud that the present invention prepares is better than original soil red mud, modification by calcination red mud, hydrochloric acid changed red mud and ferric trichloride modified red mud to the adsorption effect of phosphorus, can reach 99.47% to the clearance of phosphorus, is a kind of adsorbent of Cheap highly effective.
Zinc chloride modified red mud preparation method of the present invention, the synthetic processing time is short, and technology is simple, and energy consumption is low; The liquor zinci chloridi changed red mud constant product quality, outward appearance homogeneous, the cost that obtain are lower, and Removal of Phosphorus in Wastewater is effective.
The specific embodiment
The invention will be further described below in conjunction with embodiment.Used raw material, the equipment of embodiment is as follows:
Red mud originates from Shandong Aluminium Industry Co., Ltd, and its main component is in mass fraction, SiO
2: 25.6628%, CaO:26.6260%, Fe
2O
3: 13.5010%, Al
2O
3: 18.1207%, TiO
2: 4.3126%, MgO:2.2235%,, Na
2O:9.5535%.Zinc chloride is pure for analyzing, molecular weight 136.30, ZnCl
2Content is no less than 98%.
Thermostat water bath is a HH.S exact constant temperature water-bath.Nutsch filter is that SHB.B95 type circulation ability of swimming is used vavuum pump more.
Embodiment 1:
The constant temperature paddling process prepares the method for zinc chloride modified red mud, and step is as follows:
(1) the red mud 5g that chose 100 mesh sieves places 250mL triangle round-bottomed flask, adds 100mL0.3mol/LZnCl
2Solution,
(2) above-mentioned flask is placed HH.S exact constant temperature water-bath generator, regulate water temperature to 30 ℃ (being modification temperature) in the water-bath, constant temperature stirring reaction 1h (being modification time);
(3) solid phase that obtains behind the suction filtration reactant liquor is a zinc chloride modified red mud, with distilled water washing zinc chloride modified red mud to filtrate chloride ion-containing (detect: the silver nitrate that drips 0.1mol/L generates to there being white precipitate) not, 105 ℃ of oven dry, grind, cross 100 mesh sieves, prepare the zinc chloride modified red mud product.
Embodiment 2-10: preparation process is with embodiment 1, the ZnCl that different is in the step (1)
2Modification temperature, modification time see table 1 for details in concentration, the step (2).
Each 0.2g of zinc chloride modified red mud product that above embodiment is made is used to simulate the adsorption treatment of phosphorus-containing wastewater, and experimental technique is this area conventional method, and is specific as follows:
Take by weighing 0.2197g KH
2PO
4(analyzing pure) uses deionized water dissolving, changes in the 1000ml volumetric flask and with deionized water and is settled to scale, obtains the phosphoric acid solution that concentration is 50mg/L.
Make the above-mentioned simulation phosphorus-containing wastewater of sorbent treatment with the zinc chloride red mud that changes for preparing, adopt static method to test: the pH value of regulating phosphoric acid solution is 3.0, gets the KH of 50mg/L
2PO
4Aqueous solution 50ml places triangular flask, add the 0.2g zinc chloride modified red mud, with 180r/min constant temperature vibration 4h, the back liquid that will shake is by 0.45 μ m miillpore filter under 25 ℃, get supernatant and adopt the ascorbic acid analytical method, with residual phosphorus concentration in the HP-8453 spectrophotometric determination solution.The results are shown in Table 1.
Table 1 embodiment 1-10 zinc chloride modified red mud orthogonal test
| Embodiment | ZnCl 2Concentration (mol/L) | Modification temperature (℃) | Modification time (h) | P clearance (%) |
| 1 | 0.3mol/L | 30℃ | 1 | 99.47 |
| 2 | 0.1mol/L | 20℃ | 1 | 68.75 |
| 3 | 0.1mol/L | 30℃ | 2 | 85.79 |
| 4 | 0.1mol/L | 40℃ | 4 | 67.95 |
| 5 | 0.2mol/L | 20℃ | 4 | 83.80 |
| 6 | 0.2mol/L | 30℃ | 1 | 79.45 |
| Embodiment | ZnCl 2Concentration (mol/L) | Modification temperature (℃) | Modification time (h) | P clearance (%) |
| 7 | 0.2mol/L | 40℃ | 2 | 82.81 |
| 8 | 0.4mol/L | 20℃ | 2 | 96.68 |
| 9 | 0.4mol/L | 30℃ | 4 | 96.29 |
| 10 | 0.4mol/L | 40℃ | 1 | 94.30 |
As a comparative example, be the adsorption treatment experimental technique that adopts same simulation phosphorus-containing wastewater below, under identical experiment condition to prior art in original soil red mud, hydrochloric acid changed red mud, modification by calcination red mud and ferric trichloride modified red mud experimentize, adsorption effect is as follows:
Comparative example 1. original soil red muds (unmodified) are 25.60% to the clearance of phosphorus.
Comparative example 2. hydrochloric acid changed red muds are to the clearance of phosphorus
Concentration of hydrochloric acid 1,2,3 is represented 1mol/L, 2mol/L, 4mol/L respectively, and modification temperature 1,2,3 is represented 20 ℃, 30 ℃, 40 ℃ respectively, and modification time 1,2,3 is represented 1h, 2h, 4h respectively.
Table 2 hydrochloric acid changed red mud orthogonal test
| Factor | Concentration of hydrochloric acid (mol/L) | Modification temperature (℃) | Modification time (h) | Clearance (%) |
| Experiment 1 | 1 | 1 | 1 | 55.47 |
| Experiment 2 | 1 | 2 | 2 | 47.14 |
| Experiment 3 | 1 | 3 | 3 | 47.94 |
| Experiment 4 | 2 | 1 | 3 | 66.83 |
| Experiment 5 | 2 | 2 | 1 | 61.42 |
| Experiment 6 | 2 | 3 | 2 | 51.72 |
| Experiment 7 | 3 | 1 | 2 | 49.23 |
| Experiment 8 | 3 | 2 | 3 | 65.84 |
| Experiment 9 | 3 | 3 | 1 | 77.66 |
Comparative example 3. modification by calcination red muds are to the clearance of phosphorus
Table 3 modification by calcination red mud is to the clearance of phosphorus
Comparative example 4. ferric trichloride modified red muds are to the clearance of phosphorus
FeCl
3Concentration 1,2,3 is represented 0.1mol/L, 0.2mol/L, 0.4mol/L respectively, and modification temperature 1,2,3 is represented 20 ℃, 30 ℃, 40 ℃ respectively, and modification time 1,2,3 is represented 4h, 12h, 24h respectively.
The ferric trichloride modified red mud orthogonal test of table 4
| Factor | FeCl 3Concentration (mol/L) | Modification temperature (℃) | Modification time (h) | Clearance (%) |
| Experiment 1 | 1 | 1 | 1 | 49.13 |
| Experiment 2 | 1 | 2 | 2 | 78.65 |
| Experiment 3 | 1 | 3 | 3 | 47.94 |
| Experiment 4 | 2 | 1 | 3 | 63.79 |
| Experiment 5 | 2 | 2 | 1 | 69.74 |
| Experiment 6 | 2 | 3 | 2 | 62.01 |
| Experiment 7 | 3 | 1 | 2 | 83.80 |
| Experiment 8 | 3 | 2 | 3 | 54.09 |
| Experiment 9 | 3 | 3 | 1 | 44.77 |
Relatively above table 1-4 learns ZnCl
2The solution modification red mud is better than original soil red mud, modification by calcination red mud, hydrochloric acid changed red mud and ferric trichloride modified red mud to the adsorption effect of phosphorus, by to ZnCl
2The best modified condition of solution modification red mud is inquired into, and obtaining best modified condition is ZnCl
2Solution concentration 0.3mol/L, modification time is 1h, and modification temperature is 30 ℃, and this moment, the clearance of changed red mud was 99.47%.This shows ZnCl
2Solution has clear improvement to the absorption property of original soil red mud, is a kind of good modifier, and changed red mud is a kind of good adsorbent to the advantages of good adsorption effect of phosphorus-containing wastewater.
Claims (3)
1. the preparation method of a zinc chloride modified red mud is a raw material with red mud and zinc chloride, and step is as follows:
(1) red mud 5g is placed the triangle round-bottomed flask, add 0.1～0.4mol/L ZnCl
2Solution 100mL;
(2) above-mentioned triangle round-bottomed flask is placed thermostat water bath, regulating temperature is 20～40 ℃, stirring reaction 1～4h;
(3) behind the suction filtration reactant liquor zinc chloride modified red mud, to chloride ion-containing not, 105 ℃ of oven dry are ground, and cross 100 mesh sieves, make the zinc chloride modified red mud product with distilled water washing zinc chloride modified red mud.
2. the preparation method of zinc chloride modified red mud as claimed in claim 1 is characterized in that, adds 0.3mol/L ZnCl in the described step (1)
2Temperature is 30 ℃ in the solution, step (2), stirring reaction 1h.
3. the preparation method of zinc chloride modified red mud as claimed in claim 1 is characterized in that, described zinc chloride is pure for analyzing, molecular weight 136.30, ZnCl
2Content is no less than 98%.
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2013032419A2 (en) * | 2011-08-30 | 2013-03-07 | Joseph Iannicelli | Methods for treating waste waters using sulfidized red mud sorbents |
| CN102886247B (en) * | 2012-09-29 | 2014-07-09 | 广西大学 | Method for preparing adsorbent by virtue of red mud in alumina industry and sludge in sewage treatment |
| CN104785200B (en) * | 2015-04-21 | 2017-11-03 | 武汉中科水生环境工程股份有限公司 | A kind of preparation method of renewable modified haydites of book structure dephosphorization filler |
| CN108996641B (en) * | 2018-08-30 | 2021-08-24 | 贺州市骏鑫矿产品有限责任公司 | Method for treating acid leaching and iron removing waste liquid of potassium feldspar by utilizing red mud |
| CN109107524B (en) * | 2018-09-28 | 2020-05-08 | 同济大学 | Red mud adsorbent and preparation method and application thereof |
| CN113651652A (en) * | 2021-09-15 | 2021-11-16 | 西南交通大学 | Preparation of red mud-based slow release fertilizer and method for synchronously recycling nitrogen and phosphorus in wastewater |
| CN114377681A (en) * | 2022-01-21 | 2022-04-22 | 广西宏业环保节能工程有限公司 | Process for preparing spherical ozone catalyst by high-temperature modified red mud |
| CN116492978B (en) * | 2023-05-05 | 2024-02-09 | 陕西科技大学 | Zn 2+ Modified industryZAS/GRM composite material of waste red mud, and preparation method and application thereof |
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| CN1443600A (en) * | 2002-03-12 | 2003-09-24 | 拜尔公司 | Adsorbent mixture |
| CN1903754A (en) * | 2005-07-29 | 2007-01-31 | 南京理工大学 | Preparation method of sludge adsorber used for polluted water treatment |
| CN101176840A (en) * | 2006-11-09 | 2008-05-14 | 中国科学院生态环境研究中心 | Application method of iron modified red mud arsenic-removing adsorption agent |
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Patent Citations (3)
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|---|---|---|---|---|
| CN1443600A (en) * | 2002-03-12 | 2003-09-24 | 拜尔公司 | Adsorbent mixture |
| CN1903754A (en) * | 2005-07-29 | 2007-01-31 | 南京理工大学 | Preparation method of sludge adsorber used for polluted water treatment |
| CN101176840A (en) * | 2006-11-09 | 2008-05-14 | 中国科学院生态环境研究中心 | Application method of iron modified red mud arsenic-removing adsorption agent |
Non-Patent Citations (2)
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