CN104291353B - A kind of method preparing 4A zeolite for raw material with lateritic nickel ore acid leaching residue - Google Patents
A kind of method preparing 4A zeolite for raw material with lateritic nickel ore acid leaching residue Download PDFInfo
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- CN104291353B CN104291353B CN201310305197.5A CN201310305197A CN104291353B CN 104291353 B CN104291353 B CN 104291353B CN 201310305197 A CN201310305197 A CN 201310305197A CN 104291353 B CN104291353 B CN 104291353B
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- nickel ore
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- lateritic nickel
- acid leaching
- leaching residue
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B39/00—Compounds having molecular sieve and base-exchange properties, e.g. crystalline zeolites; Their preparation; After-treatment, e.g. ion-exchange or dealumination
- C01B39/02—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof; Direct preparation thereof; Preparation thereof starting from a reaction mixture containing a crystalline zeolite of another type, or from preformed reactants; After-treatment thereof
- C01B39/14—Type A
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Abstract
The present invention provides a kind of method preparing 4A zeolite for raw material with lateritic nickel ore acid leaching residue, relate to environment, field of material technology, specifically include following steps: melt reaction with lateritic nickel ore acid leaching residue and sodium hydroxide alkali, alkali melts product through water-soluble, filtration, obtain filtrate, by gained filtrate, aluminum source mix homogeneously by a certain percentage, through hydro-thermal reaction, final prepared 4A zeolite.The technique of the present invention is simple, cost is low, and the quantity of slag is few, the high added value realizing lateritic nickel ore acid leaching residue is comprehensively utilized and has important practical significance, be suitable to popularization and application.
Description
Technical field
The invention belongs to environment, field of material technology, be specifically related to a kind of method preparing 4A zeolite for raw material with lateritic nickel ore acid leaching residue.
Background technology
Nickel minerals mainly includes nickel sulfide ore and the big class of lateritic nickel ore two, and wherein nickel sulfide ore is of high grade, economic worth is high, but along with the high speed development of industry, nickel sulfide resource is day by day exhausted, and the exploitation of low-grade lateritic nickel ore cause global extensive concern.The mixture that the Ore that lateritic nickel ore is nickeliferous is formed through long-term weathering, leaching pouring, enrichment, has the advantages that lean ore is many, rich ore is few, amount of storage is big, cost is low.Lateritic nickel ore acid leaching residue is the solid waste after lateritic nickel ore extracts nickel.Along with world's nickel resources demand continues to increase, the discharge capacity of lateritic nickel ore acid leaching residue grows with each passing day.Under normal circumstances, the utilization rate of lateritic nickel ore acid leaching residue is relatively low, mainly air storage, occupies substantial amounts of soil, and serious environment pollution.Therefore the high value added utilization realizing lateritic nickel ore acid leaching residue has important practical significance.
4A zeolite belongs to LTA type zeolite, uniform pore diameter, has very strong adsorption selectivity and cation exchange capacity (CEC), is widely used in the aspect such as gas purification and separation, detergent builders, wastewater treatment.Business 4A zeolite is mainly by industrial chemicals by traditional water heat transfer, and this technique is subject to the restriction of raw material sources, and cost of material is higher.Utilize lateritic nickel ore acid leaching residue synthesis 4A zeolite not only can reduce the cost of synthesis 4A zeolite, and the high value added utilization of lateritic nickel ore acid leaching residue can be realized, be with a wide range of applications.
Summary of the invention
Goal of the invention
It is an object of the invention to provide a kind of method preparing 4A zeolite for raw material with lateritic nickel ore acid leaching residue, with the 4A zeolite preparing purity height, gas absorption separating property is excellent, low in raw material price that this technique uses, the quantity of slag is few, added value of product is high.
Advantages of the present invention is as follows with good effect:
The present invention, with lateritic nickel ore acid leaching residue for silicon source, adopts alkali melt water full-boiled process to prepare 4A zeolite, and technique is simple, cost is low, the high added value realizing lateritic nickel ore acid leaching residue is comprehensively utilized and has important practical significance.
Detailed description of the invention
The present invention proposes a kind of method preparing 4A zeolite for raw material with lateritic nickel ore acid leaching residue, it is characterised in that:
The method step is as follows:
(1) after lateritic nickel ore acid leaching residue being ground with sodium hydroxide, by sodium silicon mol ratio n (Na2O)/n(SiO2) it is 1.2 ~ 1.6:1 mix homogeneously, at 450 ~ 650 DEG C of temperature, alkali melts reaction 2 ~ 4h, by water sodium mol ratio n (H2O)/n(Na2O) it is that the amount of 50 ~ 110:1 adds after water, is filtered obtaining filtrate；
The chemical reaction related to is:
SiO2+2NaOH=Na2SiO3+H2O。
(2) by silica alumina ratio n (SiO in system in the filtrate obtained to step (1)2)/n(Al2O3) it is that the amount of 1.5 ~ 3:1 adds aluminum source, gained suspension is transferred in reactor crystallization 6 ~ 24h at 70 ~ 100 DEG C, is cooled to room temperature, through filtering, washing, dry, final prepare 4A zeolite.
The chemical reaction related to is:
Na2SiO3+NaOH+NaAlO2+H2O → 4A zeolite.
Lateritic nickel ore acid leaching residue described in step (1) be lateritic nickel ore with sulphuric acid or ammonium sulfate roasting after, gained roasting grog is through water logging, the filtering residue that is filtrated to get.
Aluminum source described in step (2) is sodium metaaluminate or aluminium sesquioxide.
The purity of the 4A zeolite of preparation is more than 90%.
Embodiment 1
After lateritic nickel ore acid leaching residue is ground with sodium hydroxide, by sodium silicon mol ratio n (Na2O)/n(SiO2) for 1.6:1 mix homogeneously, at 450 DEG C of temperature, alkali melts reaction 4h, by water sodium mol ratio n (H2O)/n(Na2O), after adding water for the amount of 110:1, it is filtered obtaining filtrate.By silica alumina ratio n (SiO in system in filtrate2)/n(Al2O3) add sodium metaaluminate for the amount of 1.5:1, gained suspension is transferred in reactor crystallization 24h at 70 DEG C, is cooled to room temperature, through filtering, washing, dry, final prepare 4A zeolite.
Embodiment 2
After lateritic nickel ore acid leaching residue is ground with sodium hydroxide, by sodium silicon mol ratio n (Na2O)/n(SiO2) for 1.4:1 mix homogeneously, at 550 DEG C of temperature, alkali melts reaction 3h, by water sodium mol ratio n (H2O)/n(Na2O), after adding water for the amount of 70:1, it is filtered obtaining filtrate.By silica alumina ratio n (SiO in system in filtrate2)/n(Al2O3) add sodium metaaluminate for the amount of 2:1, gained suspension is transferred in reactor crystallization 12h at 80 DEG C, is cooled to room temperature, through filtering, washing, dry, final prepare 4A zeolite.
Embodiment 3
After lateritic nickel ore acid leaching residue is ground with sodium hydroxide, by sodium silicon mol ratio n (Na2O)/n(SiO2) for 1.5:1 mix homogeneously, at 600 DEG C of temperature, alkali melts reaction 2h, by water sodium mol ratio n (H2O)/n(Na2O), after adding water for the amount of 90:1, it is filtered obtaining filtrate.By silica alumina ratio n (SiO in system in filtrate2)/n(Al2O3) add aluminium sesquioxide for the amount of 2:1, gained suspension is transferred in reactor crystallization 6h at 90 DEG C, is cooled to room temperature, through filtering, washing, dry, final prepare 4A zeolite.
Embodiment 4
After lateritic nickel ore acid leaching residue is ground with sodium hydroxide, by sodium silicon mol ratio n (Na2O)/n(SiO2) for 1.6:1 mix homogeneously, at 650 DEG C of temperature, alkali melts reaction 2h, by water sodium mol ratio n (H2O)/n(Na2O), after adding water for the amount of 110:1, it is filtered obtaining filtrate.By silica alumina ratio n (SiO in system in filtrate2)/n(Al2O3) add aluminium sesquioxide for the amount of 3:1, gained suspension is transferred in reactor crystallization 6h at 100 DEG C, is cooled to room temperature, through filtering, washing, dry, final prepare 4A zeolite.
Claims (4)
1. the method preparing 4A zeolite for raw material with lateritic nickel ore acid leaching residue, it is characterised in that comprise the following steps:
(1) after lateritic nickel ore acid leaching residue being ground with sodium hydroxide, by sodium silicon mol ratio n (Na2O)/n(SiO2) it is 1.2 ~ 1.6:1 mix homogeneously, at 450 ~ 650 DEG C of temperature, alkali melts reaction 2-4h, by water sodium mol ratio n (H2O)/n(Na2O) it is that the amount of 50 ~ 110:1 adds after water, is filtered obtaining filtrate；
(2) by silica alumina ratio n (SiO in system in the filtrate obtained to step (1)2)/n(Al2O3) it is that the amount of 1.5 ~ 3:1 adds aluminum source, gained suspension is transferred in reactor crystallization 6 ~ 24h at 70 ~ 100 DEG C, is cooled to room temperature, through filtering, washing, dry, final prepare 4A zeolite.
2. a kind of method preparing 4A zeolite for raw material with lateritic nickel ore acid leaching residue according to claim 1, it is characterized in that: the lateritic nickel ore acid leaching residue described in step (1) be lateritic nickel ore after sulphuric acid or ammonium sulfate roasting, gained roasting grog is through water logging, the filtering residue that is filtrated to get.
3. a kind of method preparing 4A zeolite for raw material with lateritic nickel ore acid leaching residue according to claim 1, it is characterised in that: the aluminum source described in step (2) is sodium metaaluminate or aluminium sesquioxide.
4. a kind of method preparing 4A zeolite for raw material with lateritic nickel ore acid leaching residue according to claim 1, it is characterised in that: the purity preparing 4A zeolite described in step (2) is more than 90%.
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| CN201310305197.5A CN104291353B (en) | 2013-07-20 | 2013-07-20 | A kind of method preparing 4A zeolite for raw material with lateritic nickel ore acid leaching residue |
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| CN104291353A CN104291353A (en) | 2015-01-21 |
| CN104291353B true CN104291353B (en) | 2016-07-06 |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105036151B (en) * | 2015-08-14 | 2017-12-15 | 商洛学院 | A kind of method that zeolite molecular sieve is produced using mine tailing |
| CN107055565B (en) * | 2017-05-31 | 2019-08-02 | 合肥工业大学 | A method of zeolite molecular sieve is prepared with opal attapulgite clay |
| CN108910909B (en) * | 2018-09-30 | 2020-04-03 | 芜湖格丰环保科技研究院有限公司 | Method for preparing ZSM-5 molecular sieve by using laterite-nickel ore smelting waste residues |
| CN109467101B (en) * | 2018-12-28 | 2020-11-27 | 北京科技大学 | Process method for preparing aluminum-silicon solution by dissolving laterite-nickel ore smelting slag |
| CN113461026B (en) * | 2021-07-09 | 2023-11-10 | 盐城工学院 | Preparation method and application of zeolite type dephosphorizing agent for high-salt waste liquid |
Citations (4)
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|---|---|---|---|---|
| JP2006232597A (en) * | 2005-02-24 | 2006-09-07 | Aomori Prefecture | Method for manufacturing artificial zeolite from smelting reduction slag |
| CN102139887A (en) * | 2011-02-25 | 2011-08-03 | 抚顺矿业集团有限责任公司 | Method for preparing 4A molecular sieve by oil shale waste residue |
| CN102167352A (en) * | 2011-03-14 | 2011-08-31 | 浙江师范大学 | Method for preparing 4A zeolite by kaolin alkali fusion one-step method |
| CN103073021A (en) * | 2013-01-11 | 2013-05-01 | 东北大学 | Method for preparing titanium silicalite ETS-10 with high-silicon industrial raw material |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2006232597A (en) * | 2005-02-24 | 2006-09-07 | Aomori Prefecture | Method for manufacturing artificial zeolite from smelting reduction slag |
| CN102139887A (en) * | 2011-02-25 | 2011-08-03 | 抚顺矿业集团有限责任公司 | Method for preparing 4A molecular sieve by oil shale waste residue |
| CN102167352A (en) * | 2011-03-14 | 2011-08-31 | 浙江师范大学 | Method for preparing 4A zeolite by kaolin alkali fusion one-step method |
| CN103073021A (en) * | 2013-01-11 | 2013-05-01 | 东北大学 | Method for preparing titanium silicalite ETS-10 with high-silicon industrial raw material |
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