CN104291353A - Method for preparation of 4A zeolite from lateritic nickel ore acid leaching residue - Google Patents
Method for preparation of 4A zeolite from lateritic nickel ore acid leaching residue Download PDFInfo
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- CN104291353A CN104291353A CN201310305197.5A CN201310305197A CN104291353A CN 104291353 A CN104291353 A CN 104291353A CN 201310305197 A CN201310305197 A CN 201310305197A CN 104291353 A CN104291353 A CN 104291353A
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- nickel ore
- acid leaching
- leaching residue
- zeolite
- red soil
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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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- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
Relating to the technical field of environment and materials, the invention provides a method for preparation of 4A zeolite from lateritic nickel ore acid leaching residue. The method comprises the steps of: subjecting lateritic nickel ore acid leaching residue and sodium hydroxide to alkali fusion reaction, dissolving the alkali fusion product in water and performing filtration to obtain filtrate, mixing the obtained filtrate with an aluminium source in certain proportion, and carrying out hydrothermal reaction, thus finally obtaining the 4A zeolite. The method provided by the invention has the characteristics of simple process, low cost and little slag, and has important practical significance for realizing high value-added comprehensive utilization of lateritic nickel ore acid leaching residue, thus being suitable for popularization and application.
Description
Technical field
The invention belongs to environment, field of material technology, be specifically related to a kind of with red soil nickel ore acid leaching residue for the method for 4A zeolite prepared by raw material.
Background technology
Nickel minerals mainly comprises the large class of nickel sulfide ore and red soil 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, nickelous sulfide resource is day by day exhausted, and the exploitation of low-grade red soil nickel ore cause global extensive concern.Red soil nickel ore be nickeliferous ore through long-term weathering, leaching is drenched, enrichment and the mixture that formed, has the advantages that lean ore is many, rich ore is few, store content is large, cost is low.Red soil nickel ore acid leaching residue is the solid waste after red soil nickel ore extracts nickel.Along with world's nickel resources demand continues to increase, the quantity discharged of red soil nickel ore acid leaching residue grows with each passing day.Under normal circumstances, the utilization ratio of red soil nickel ore acid leaching residue is lower, mainly air storage, occupies a large amount of soils, and serious environment pollution.Therefore the high value added utilization realizing red soil nickel ore acid leaching residue has important practical significance.
4A zeolite belongs to LTA type zeolite, and uniform pore diameter has very strong adsorption selectivity and cation exchange capacity (CEC), is widely used in gas sweetening and is separated, detergent builder, the aspect such as wastewater treatment.Business 4A zeolite mainly utilizes 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 red soil nickel ore acid leaching residue to synthesize 4A zeolite and not only can reduce the cost synthesizing 4A zeolite, and the high value added utilization of red soil nickel ore acid leaching residue can be realized, be with a wide range of applications.
Summary of the invention
Goal of the invention
The object of this invention is to provide a kind of with red soil nickel ore acid leaching residue for raw material prepares the method for 4A zeolite, the 4A zeolite that purity is high to prepare, gas adsorption separation performance is excellent, the low in raw material price that this technique uses, the quantity of slag is few, added value of product is high.
Advantage of the present invention and positively effect as follows:
The present invention is with red soil nickel ore acid leaching residue for silicon source, and adopt the hot legal system of alkali melt water for 4A zeolite, technique is simple, cost is low, has important practical significance to the high added value comprehensive utilization realizing red soil nickel ore acid leaching residue.
Embodiment
The present invention proposes a kind of with red soil nickel ore acid leaching residue for the method for 4A zeolite prepared by raw material, it is characterized in that:
The method step is as follows:
(1) after red soil nickel ore acid leaching residue and sodium hydroxide being ground, by sodium silicon mol ratio n (Na
2o)/n (SiO
2) be that 1.2 ~ 1.6:1 mixes, at 450 ~ 650 DEG C of temperature, alkali melts reaction 2 ~ 4h, by water sodium mol ratio n (H
2o)/n (Na
2o) be, after the amount of 50 ~ 110:1 adds water, carry out filtration and obtain filtrate;
The chemical reaction related to is:
SiO
2+2NaOH?=?Na
2SiO
3+H
2O。
(2) by silica alumina ratio n (SiO in system in the filtrate obtained to step (1)
2)/n (Al
2o
3) be that the amount of 1.5 ~ 3:1 adds aluminium source, gained suspension to be transferred in reactor crystallization 6 ~ 24 h at 70 ~ 100 DEG C, be cooled to room temperature, after filtration, washing, dry, final obtained 4A zeolite.
The chemical reaction related to is:
Na
2siO
3+ NaOH+NaAlO
2+ H
2o → 4A zeolite.
Red soil nickel ore acid leaching residue described in step (1) is after red soil nickel ore and sulfuric acid or ammonium sulfate roasting, gained roasting grog through water logging, filter the filter residue obtained.
Aluminium 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 red soil nickel ore acid leaching residue and sodium hydroxide are ground, by sodium silicon mol ratio n (Na
2o)/n (SiO
2) for 1.6:1 mixes, at 450 DEG C of temperature, alkali melts reaction 4h, by water sodium mol ratio n (H
2o)/n (Na
2o) for after the amount of 110:1 adds water, carry out filtration and obtain filtrate.By silica alumina ratio n (SiO in system in filtrate
2)/n (Al
2o
3) for the amount of 1.5:1 adds sodium metaaluminate, gained suspension to be transferred in reactor crystallization 24 h at 70 DEG C, be cooled to room temperature, after filtration, washing, dry, final obtained 4A zeolite.
embodiment 2
After red soil nickel ore acid leaching residue and sodium hydroxide are ground, by sodium silicon mol ratio n (Na
2o)/n (SiO
2) for 1.4:1 mixes, at 550 DEG C of temperature, alkali melts reaction 3h, by water sodium mol ratio n (H
2o)/n (Na
2o) for after the amount of 70:1 adds water, carry out filtration and obtain filtrate.By silica alumina ratio n (SiO in system in filtrate
2)/n (Al
2o
3) for the amount of 2:1 adds sodium metaaluminate, gained suspension to be transferred in reactor crystallization 12h at 80 DEG C, be cooled to room temperature, after filtration, washing, dry, final obtained 4A zeolite.
embodiment 3
After red soil nickel ore acid leaching residue and sodium hydroxide are ground, by sodium silicon mol ratio n (Na
2o)/n (SiO
2) for 1.5:1 mixes, at 600 DEG C of temperature, alkali melts reaction 2h, by water sodium mol ratio n (H
2o)/n (Na
2o) for after the amount of 90:1 adds water, carry out filtration and obtain filtrate.By silica alumina ratio n (SiO in system in filtrate
2)/n (Al
2o
3) for the amount of 2:1 adds aluminium sesquioxide, gained suspension to be transferred in reactor crystallization 6h at 90 DEG C, be cooled to room temperature, after filtration, washing, dry, final obtained 4A zeolite.
embodiment 4
After red soil nickel ore acid leaching residue and sodium hydroxide are ground, by sodium silicon mol ratio n (Na
2o)/n (SiO
2) for 1.6:1 mixes, at 650 DEG C of temperature, alkali melts reaction 2h, by water sodium mol ratio n (H
2o)/n (Na
2o) for after the amount of 110:1 adds water, carry out filtration and obtain filtrate.By silica alumina ratio n (SiO in system in filtrate
2)/n (Al
2o
3) for the amount of 3:1 adds aluminium sesquioxide, gained suspension to be transferred in reactor crystallization 6h at 100 DEG C, be cooled to room temperature, after filtration, washing, dry, final obtained 4A zeolite.
Claims (4)
1. with red soil nickel ore acid leaching residue for the method for 4A zeolite prepared by raw material, it is characterized in that comprising the following steps:
(1) after red soil nickel ore acid leaching residue and sodium hydroxide being ground, by sodium silicon mol ratio n (Na
2o)/n (SiO
2) be that 1.2 ~ 1.6:1 mixes, at 450 ~ 650 DEG C of temperature, alkali melts reaction 2-4h, by water sodium mol ratio n (H
2o)/n (Na
2o) be, after the amount of 50 ~ 110:1 adds water, carry out filtration and obtain filtrate;
(2) by silica alumina ratio n (SiO in system in the filtrate obtained to step (1)
2)/n (Al
2o
3) be that the amount of 1.5 ~ 3:1 adds aluminium source, gained suspension to be transferred in reactor crystallization 6 ~ 24 h at 70 ~ 100 DEG C, be cooled to room temperature, after filtration, washing, dry, final obtained 4A zeolite.
2. according to claim 1 a kind of with red soil nickel ore acid leaching residue for the method for 4A zeolite prepared by raw material, it is characterized in that: the red soil nickel ore acid leaching residue described in step (1) be red soil nickel ore after sulfuric acid or ammonium sulfate roasting, gained roasting grog through water logging, filter the filter residue that obtains.
3. according to claim 1 a kind of with red soil nickel ore acid leaching residue for the method for 4A zeolite prepared by raw material, it is characterized in that: the aluminium source described in step (2) is sodium metaaluminate or aluminium sesquioxide.
4. according to claim 1 a kind of with red soil nickel ore acid leaching residue for the method for 4A zeolite prepared by raw material, it is characterized in that: the purity of the preparation 4A zeolite described in step (2) is more than 90%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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 |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| 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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104291353A true CN104291353A (en) | 2015-01-21 |
| CN104291353B CN104291353B (en) | 2016-07-06 |
Family
ID=52311347
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310305197.5A Expired - Fee Related 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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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105036151A (en) * | 2015-08-14 | 2015-11-11 | 商洛学院 | Methodof producing zeolite molecular sieve by utilizing tailings |
| CN107055565A (en) * | 2017-05-31 | 2017-08-18 | 合肥工业大学 | A kind of method that zeolite molecular sieve is prepared with opal attapulgite clay |
| CN108910909A (en) * | 2018-09-30 | 2018-11-30 | 芜湖格丰环保科技研究院有限公司 | A method of ZSM-5 molecular sieve is produced using smelting laterite-nickel ores waste residue |
| CN109467101A (en) * | 2018-12-28 | 2019-03-15 | 北京科技大学 | A kind of process preparing aluminium silicon solution using smelting laterite-nickel ores slag dissolution |
| CN113461026A (en) * | 2021-07-09 | 2021-10-01 | 盐城工学院 | Preparation method and application of zeolite type phosphorus removal agent for high-salt waste liquid |
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 |
-
2013
- 2013-07-20 CN CN201310305197.5A patent/CN104291353B/en not_active Expired - Fee Related
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 |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105036151A (en) * | 2015-08-14 | 2015-11-11 | 商洛学院 | Methodof producing zeolite molecular sieve by utilizing tailings |
| 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 |
| CN107055565A (en) * | 2017-05-31 | 2017-08-18 | 合肥工业大学 | A kind of method that zeolite molecular sieve is prepared with opal attapulgite clay |
| 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 |
| CN108910909A (en) * | 2018-09-30 | 2018-11-30 | 芜湖格丰环保科技研究院有限公司 | A method of ZSM-5 molecular sieve is produced using smelting laterite-nickel ores waste residue |
| CN109467101A (en) * | 2018-12-28 | 2019-03-15 | 北京科技大学 | A kind of process preparing aluminium silicon solution using smelting laterite-nickel ores slag dissolution |
| CN113461026A (en) * | 2021-07-09 | 2021-10-01 | 盐城工学院 | Preparation method and application of zeolite type phosphorus removal agent for high-salt waste liquid |
| 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 |
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|---|---|
| CN104291353B (en) | 2016-07-06 |
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Granted publication date: 20160706 Termination date: 20170720 |