CN103011630A - Method of producing high-purity magnesium hydroxide and magnesium oxide by low-grade magnesite - Google Patents
Method of producing high-purity magnesium hydroxide and magnesium oxide by low-grade magnesite Download PDFInfo
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Abstract
The invention relates to the field of mineral resource processing technology, in particular to a method of producing high-purity magnesium hydroxide and magnesium oxide by low-grade magnesite. The method comprises the following steps: calcining low-grade magnesite in a calcining furnace at calcining temperature to obtain light-calcining magnesite ore and carbon dioxide, recovering the carbon dioxide, and crushing the calcined light-calcining magnesite ore. By utilizing a method of realizing leaching, purification and separation coupling of the low-grade magnesite and producing high-pruity magnesium hydroxide and magnesium oxide through recycling of ammonia-ammonium slat, the advantages of preparing high-purity products by adopting the traditional bittern-ammonia process can be fully achieved, the method is of green and cycling clean production technique method, no wastes are emitted in the whole process, resources can be comprehensively utilized, the utilization rate of the magnesite resource can be improved, strong acid is not consumed in the technique process, other constitutions are fully utilized, the pollution to the environment can be reduced, and the method provides a new approach for reasonably developing and utilizing the low-grade magnesite resources.
Description
Technical field
The present invention relates to the Mineral resources processing technique field, is that a kind of low-grade magnesite is produced high purity magnesium hydroxide and method of magnesium oxide.
Background technology
The main chemical compositions of magnesite is MgCO
3, main application is for the preparation of the magnesium series refractory material and contains the magnesium chemical.The magnesite resource reserves of China occupy first place, the world, maximum in the world magnesium products production and export State, because the product lower take primary raw materials and added value, that scientific and technological content is not high, therefore exists the low inferior problem of waste resource, contaminate environment and benefit as main.Magnesite is a kind of Nonrenewable resources, at present, because people carry out irrational development and use to it, causes the magnesite resource of China's high-quality day by day to reduce, MgCO in existing most of magnesite
3Content be lower than 90%(and be converted to MgO content and be lower than 42%), prospect allows of no optimist.Major impurity in the magnesite comprises CaO, Al
2O
3, SiO
2, Fe
2O
3Deng; foreign matter content is high will directly to cause the reduction of MgO content in the magnesite; and then cause the Quality Down of its derived product; the increase of production cost and the consequences such as destruction of ecotope; and do not meet the requirement of Sustainable development; therefore clean for low-grade magnesite; requiring of efficient and comprehensive utilization is extremely urgent; realize the rational exploitation and utilization of low-grade magnesite; make up the Chemical Manufacture novel process of clean and effective; can greatly save and protect the high-quality magnesite resource and eliminate environmental pollution, meet national Ecological Civilization Construction with green; circulation and intensive demand for development.
Number of patent application is that the Chinese patent literature of 201110428374.X is mentioned: magnesite is progressively carried out fragmentation, ore grinding, classification, ore dressing, dressing product calcining, useful component changes into that magnesium salts prepares high-purity magnesium oxide or Direct Electrolysis is MAGNESIUM METAL after the calcining, the preparation refractory materials.This patent can realize the comprehensive utilization of magnesite, but also seriation of product but exists flow process longer, the problems such as the higher and flotation agent pollution of beneficiation cost; Prepare in addition the magnesium salts consumption acids, easily produce acid waste water, form secondary pollution.
Number of patent application is that 201010563752.0 Chinese patent literature is mentioned: the MgO that the low-grade magnesite calcining is obtained grinds that powdered is molten by pulp, alkali, carbonization, acid is molten and multiple times of filtration, repeated drying, the repeatedly operation such as calcining, acquisition Al
2O
3, CaCO
3, MgO, SiO
2, Fe
2O
3Reach the products such as NaCl.This invention can be extracted useful component in the magnesite one by one, improves resource utilization; But this invention flow process is complicated, uses strong acid and strong base higher to equipment requirements, and operation is harsh, is difficult to carry out scale operation.
Number of patent application is that 200710000049.7 Chinese patent literature is mentioned a kind of method of utilizing low-grade magnesite to prepare nano-sized magnesium hydroxide, magnesium oxide after the high-temperature calcination and strong acid (sulfuric acid or nitric acid) reaction are made the soluble magnesium salts solution, by adding highly basic (sodium hydroxide or ammoniacal liquor), the control processing condition, through ageing, filtration, washing, drying, the step such as break up and make nanometric magnesium hydroxide, by-product sodium salt or ammonium salt.This invention only obtains magnesium products, and by-product sodium salt or ammonium salt are difficult to recycle, and the use of soda acid easily causes secondary pollution, in addition, because other component is utilized, causes resource utilization not high.
Number of patent application is that 200810010163.2 Chinese patent literatures are mentioned: the magnesia unslacked that the magnesite calcining is obtained carries out acidolysis and the removal of impurities of ammonium sulfate and the vitriol oil, obtain sal epsom, prepare respectively magnesium basic carbonate and magnesium hydroxide again behind neutralization and removing impurities by oxidation, magnesium basic carbonate is sintered into magnesium oxide.
Summary of the invention
The invention provides a kind of low-grade magnesite and produce high purity magnesium hydroxide and method of magnesium oxide, overcome the deficiency of above-mentioned prior art, it can effectively solve, and the magnesite resource utilization ratio is not high, technological process consumes strong acid, other component is underutilized and the problem of environmental pollution.
Technical scheme of the present invention realizes by following measures: low-grade magnesite is produced high purity magnesium hydroxide and method of magnesium oxide, carry out as follows: the first step, in calcining furnace, low-grade magnesite stone is calcined under calcining temperature, obtain the light-burned ore of magnesite and carbonic acid gas, with carbon dioxide recovery, the light-burned ore of the magnesite after this calcining is carried out fragmentation and is finely ground to the light burnt powder powder;
Second step, light burnt powder powder aquation is become the light burnt powder slurry, also stir at the enamel still internal reaction with the ammonium salt solution after the dissolving, generate solubility calcium-magnesium-containing salts solution, ammonia and leached mud, ammonia obtains ammoniacal liquor behind ammonia rectifying tower and ammonia condenser, after solubility calcium-magnesium-containing salts solution and the leached mud solid-liquid separation, add the water washing leached mud, washing water are cycled to used in light-burned efflorescence slurry;
The 3rd step, with second step gained solubility calcium-magnesium-containing salts solution and ammoniacal liquor and the first step gained carbon dioxide reaction, obtain calcium carbonate, pure magnesium salt solution and ammonium salt solution after filtration with after the solid-liquid separation, the ammoniacal liquor of pure magnesium salt solution and second step gained at the stainless steel cauldron internal reaction and stir, is generated magnesium hydroxide and contains the ammonium salt solution of free ammonia;
The 4th step, with obtaining moisture magnesium hydroxide after the combination operation of magnesium hydroxide process filtration washing, carry out obtaining high purity magnesium hydroxide after the drying, washing water are used for ammonium salt dissolving and the light-burned efflorescence slurry of second step after reclaiming free ammonia;
In the 5th step, the moisture magnesium hydroxide calcining of the 4th step gained is obtained high-purity magnesium oxide.
The below is the further optimization and/or improvements to the foregoing invention technical scheme:
MgCO in the low-grade magnesite in the above-mentioned the first step
3Content can be 75% to 90%, and calcining temperature is 900 ℃ to 1100 ℃, and the granularity that light burnt powder is levigate is that-200 orders are to+300 orders.
Light burnt powder slurry concentration in the above-mentioned second step can be 30% to 40%, and ammonium chloride concentration is 20% to 30%, and the temperature of reaction in enamel still is 100 ℃ to 120 ℃, and mixing speed is 80rpm to 100rpm, and the reaction times is 2h to 4h.
In above-mentioned the 3rd step, free ammonia is excess of ammonia and recycles, and the temperature in stainless steel cauldron is 70 ℃ to 90 ℃, mixing speed 80 rpm to 100rpm, and reaction and digestion time are 1.5h, the relative magnesium chloride of ammonia volume excessive 30% to 50%.
In above-mentioned the 4th step, drying temperature can be 130 ℃ to 170 ℃, and the calcining temperature in the 5th step is 500 ℃ to 700 ℃, and ammonium salt is ammonium chloride or ammonium sulfate.
Above-mentioned the 4th the step in the filtration washing combination operation can comprise the original position countercurrent washing three times, pulping and washing once, original position is washed once.
The above-mentioned ammonium salt solution that gained in the 3rd step is contained free ammonia can pass through respectively the operations such as extraction, enrichment and condensation recovery and obtain ammoniacal liquor, and this ammoniacal liquor goes on foot the 3rd and reuses; The ammonium salt solution of gained is reused at second step.
Above-mentioned leached mud is the leached mud of iron content aluminium silico-calcium, and leached mud can be used for producing the addition material of magnesia oxychloride cement.
The present invention utilizes ammonia-ammonium salt cyclic regeneration to realize that low-grade magnesite leaches, purify, separation coupling is also produced high purity magnesium hydroxide and method of magnesium oxide, given full play to the advantage that traditional bittern-ammonia process prepares high purity product, the inventive method is a green, the cleaning manufacturing technique method of circulation, whole process does not have waste discharge, utilize resources synthetically, improved the magnesite resource utilization ratio, do not consume strong acid in the technological process, other component is fully used, and reduce the pollution to environment, for the rational exploitation and utilization of low-grade magnesite resource provides new way.
Description of drawings
Accompanying drawing 1 is process flow diagram of the present invention.
Embodiment
The present invention is not subjected to the restriction of following embodiment, can determine concrete embodiment according to technical scheme and the practical situation of invention.
The invention will be further described below in conjunction with embodiment:
Embodiment 1, and this low-grade magnesite prepares high purity magnesium hydroxide and method of magnesium oxide carries out in the steps below:
Get 1000g magnesite, 950 ℃ of lower calcining 3h(burning mistake rates are 47.5% in calcining furnace), reclaim the carbonic acid gas that calcining and decomposing goes out; The light-burned ore reduction of magnesite with after the calcining is finely ground to 200 order to 300 purpose light burnt powder powder; Add entry 980ml in the light burnt powder powder and stir, be mixed with concentration and be 35% light burnt powder slurry, get the ammonium chloride that quality is 1150g, add entry 2500ml and stirring and dissolving, be mixed with 25% ammonium chloride solution; Light burnt powder slurry and ammonium chloride solution react in the enamel still that stirs and heat, and temperature of reaction is 105 ℃, and the reaction times is 3h, the ammonia that generates in the reaction process, magnesium chloride and calcium chloride, and Ammonia recovery also is condensed into ammoniacal liquor; The carbonic acid gas that reclaims, ammoniacal liquor and calcium chloride generate calcium carbonate at the stainless steel cauldron internal reaction, after removing calcium carbonate, obtain magnesium chloride solution, in with the stainless steel cauldron that stirs and heat, generate magnesium hydroxide with ammoniacal liquor and magnesium chloride solution, temperature of reaction is 80 ℃, reaction and digestion time are 1.5h, and ammonia volume is excessive 30%, and the magnesium hydroxide of generation adopts 80 ℃ of hot washes, be specially the original position countercurrent washing three times, pulping and washing once, again original position washing once, the moisture magnesium hydroxide that obtains is at 130 ℃ of lower dry 3h, then at 600 ℃ of lower calcining 2h, obtain high-purity magnesium oxide, gained high purity magnesium hydroxide quality is 410g, and purity is 99.38%, gained high-purity magnesium oxide quality is 280g, and purity is 99. 17%.Ammonium chloride is technical grade, content〉99%.
Embodiment 2, and this low-grade magnesite prepares high purity magnesium hydroxide and method of magnesium oxide carries out in the steps below:
Get 1000g magnesite, 1000 ℃ of lower calcining 3h(burning mistake rates are 49.8% in calcining furnace), reclaim the carbonic acid gas that calcining and decomposing goes out, with the light-burned ore reduction of magnesite after the calcining, be finely ground to-200 purpose light burnt powder powder, add entry 1000ml in the light burnt powder powder and stir, be mixed with concentration and be 35% light burnt powder slurry; Get the ammonium chloride that quality is 1200g; Add entry 3800ml, stirring and dissolving is mixed with 20% ammonium chloride solution; Light burnt powder slurry and ammonium chloride solution react in the enamel still that stirs and heat, and temperature of reaction is 110 ℃, and the reaction times is 3h, generates ammonia, magnesium chloride and calcium chloride in the reaction process, and Ammonia recovery also is condensed into ammoniacal liquor; The carbonic acid gas that reclaims, ammoniacal liquor and calcium chloride generate calcium carbonate at the stainless steel cauldron internal reaction, after removing calcium carbonate, obtain magnesium chloride solution, in with the stainless steel cauldron that stirs and heat, generate magnesium hydroxide with ammoniacal liquor and magnesium chloride solution, temperature of reaction is 85 ℃, reaction and digestion time are 1.5h, ammonia volume is excessive 40%, and the magnesium hydroxide of generation adopts 85 ℃ of hot washes, is specially the original position countercurrent washing three times, pulping and washing once, original position is washed once again, and then the moisture magnesium hydroxide that obtains obtains high-purity magnesium oxide at 650 ℃ of lower calcining 2h at 140 ℃ of lower dry 2h, the high purity magnesium hydroxide quality is 418g, purity is 99.53%, and calcining obtains high-purity magnesium oxide 286g, and purity is 99. 25%.Ammonium chloride is technical grade, content〉99%.
Embodiment 3, and this low-grade magnesite prepares high purity magnesium hydroxide and method of magnesium oxide carries out in the steps below:
Get 1000g magnesite, 900 ℃ to 1100 ℃ lower calcining 3h(burning mistake rates are 49.8% in calcining furnace), reclaim the carbonic acid gas that calcining and decomposing goes out, with the light-burned ore reduction of magnesite after the calcining, be finely ground to-200 orders to+300 purpose light burnt powder powder; Add entry 1000ml in the light burnt powder powder and stir, be mixed with concentration and be 30% to 40% light burnt powder slurry; Get the ammonium chloride that quality is 1200g, add entry 3800ml, stirring and dissolving is mixed with 20% to 30% ammonium chloride solution; Light burnt powder slurry and ammonium chloride solution carry out in the enamel still that stirs and heat, and temperature of reaction is 100 ℃ to 120 ℃, and the reaction times is 2h to 4h, the ammonia that generates in the reaction process, magnesium chloride and calcium chloride, and Ammonia recovery also is condensed into ammoniacal liquor; The carbonic acid gas that reclaims, ammoniacal liquor and calcium chloride generate calcium carbonate in stainless steel cauldron, after removing calcium carbonate, obtain magnesium chloride solution, in with the stainless steel cauldron that stirs and heat, generate magnesium hydroxide with ammoniacal liquor and magnesium chloride solution, temperature of reaction is 70 ℃ to 90 ℃, reaction and digestion time are 1.5h, ammonia volume excessive 30% to 50%, the magnesium hydroxide that generates adopts 70 ℃ to 90 ℃ hot washes, be specially the original position countercurrent washing three times, pulping and washing once, original position washing is once again, the moisture magnesium hydroxide that obtains is at 120 ℃ to 150 ℃ lower dry 2h, then obtain high-purity magnesium oxide at 500 ℃ to 700 ℃ lower calcining 2h, gained high purity magnesium hydroxide purity is 99.38% to 99.53%, and gained high-purity magnesium oxide purity is 99. 17% to 99. 25%.Ammonium chloride is technical grade, content〉99%.
In the present invention: % is per-cent, expression be mass percent, composition and the content of magnesite are as shown in table 1.
The present invention has larger adaptability, and technical characterictic can carry out necessary adjustment according to practical situation among the embodiment, to reach best effect.
The composition of table 1 magnesite and content
| Composition | MgCO 3 | CaCO 3 | Fe 2O 3 | SiO 2 | Al 2O 3 |
| Content/% | 75 to 90 | 13 to 18 | 1.5 to 2.8 | 3.5 to 6.0 | 0.8 to 1.2 |
As follows at the main chemical reactions equation that embodiment 1, embodiment 2 and embodiment 3 relate to:
MgCO
3→ MgO+CO
2↑, this reaction process needs heating.
CaCO
3→ CaO+CO
2↑, this reaction process needs heating.
4FeO+O
2→ 2Fe
2O
3, this reaction process needs heating.
MgO+2NH
4Cl/(NH
4)
2SO
4→MgCl
2/MgSO
4+2NH
3↑+H
2O
CaO+2NH
4Cl/(NH
4)
2SO
4→CaCl
2/CaSO
4+2NH
3↑+H
2O
CaCl
2+2NH
3+CO
2+H
2O→CaCO
3↓+2NH
4Cl
MgCl
2/MgSO
4+2NH
3+2CO
2+2H
2O→Mg(HCO
3)
2↓+2NH
4Cl/(NH
4)
2SO
4
MgCl
2/MgSO
4+2NH
3+2H
2O→Mg(OH)
2↓+2NH
4Cl/(NH4)
2SO
4
Claims (10)
1. low-grade magnesite is produced high purity magnesium hydroxide and method of magnesium oxide, it is characterized in that carrying out as follows: the first step, in calcining furnace, low-grade magnesite stone is calcined under calcining temperature, obtain the light-burned ore of magnesite and carbonic acid gas, with carbon dioxide recovery, the light-burned ore of the magnesite after this calcining is carried out fragmentation and is finely ground to the light burnt powder powder; Second step, light burnt powder powder aquation is become the light burnt powder slurry, also stir at the enamel still internal reaction with the ammonium salt solution after the dissolving, generate solubility calcium-magnesium-containing salts solution, ammonia and leached mud, ammonia obtains ammoniacal liquor behind ammonia rectifying tower and ammonia condenser, after solubility calcium-magnesium-containing salts solution and the leached mud solid-liquid separation, add the water washing leached mud, washing water are cycled to used in light-burned efflorescence slurry; The 3rd step, with second step gained solubility calcium-magnesium-containing salts solution and ammoniacal liquor and the first step gained carbon dioxide reaction, obtain calcium carbonate, pure magnesium salt solution and ammonium salt solution after filtration with after the solid-liquid separation, the ammoniacal liquor of pure magnesium salt solution and second step gained at the stainless steel cauldron internal reaction and stir, is generated magnesium hydroxide and contains the ammonium salt solution of free ammonia; The 4th step, with obtaining moisture magnesium hydroxide after the combination operation of magnesium hydroxide process filtration washing, carry out obtaining high purity magnesium hydroxide after the drying, washing water are used for ammonium salt dissolving and the light-burned efflorescence slurry of second step after reclaiming free ammonia; In the 5th step, the moisture magnesium hydroxide calcining of the 4th step gained is obtained high-purity magnesium oxide.
2. low-grade magnesite according to claim 1 is produced high purity magnesium hydroxide and method of magnesium oxide, it is characterized in that MgCO in the low-grade magnesite in the first step
3Content is 75% to 90%, and calcining temperature is 900 ℃ to 1100 ℃, and the granularity that light burnt powder is levigate is that-200 orders are to+300 orders.
3. low-grade magnesite according to claim 2 is produced high purity magnesium hydroxide and method of magnesium oxide, it is characterized in that the light burnt powder slurry concentration in the second step is 30% to 40%, ammonium chloride concentration is 20% to 30%, temperature of reaction in enamel still is 100 ℃ to 120 ℃, mixing speed is 80rpm to 100rpm, and the reaction times is 2h to 4h.
4. low-grade magnesite according to claim 3 is produced high purity magnesium hydroxide and method of magnesium oxide, it is characterized in that in the 3rd step, free ammonia is excess of ammonia and recycles, temperature in stainless steel cauldron is 70 ℃ to 90 ℃, mixing speed 80 rpm to 100rpm, reaction and digestion time are 1.5h, the relative magnesium chloride of ammonia volume excessive 30% to 50%.
According to claim 1 and 2 or 3 or 4 described low-grade magnesites produce high purity magnesium hydroxide and method of magnesium oxide, it is characterized in that in the 4th step, drying temperature is 130 ℃ to 170 ℃, and the calcining temperature in the 5th step is 500 ℃ to 700 ℃, and ammonium salt is ammonium chloride or ammonium sulfate.
According to claim 1 and 2 or 3 or 4 described low-grade magnesites produce high purity magnesium hydroxide and method of magnesium oxide, it is characterized in that the filtration washing combination operation in the 4th step comprises the original position countercurrent washing three times, pulping and washing once, original position is washed once.
7. low-grade magnesite according to claim 5 is produced high purity magnesium hydroxide and method of magnesium oxide, it is characterized in that the filtration washing combination operation in the 4th step comprises the original position countercurrent washing three times, pulping and washing once, original position is washed once.
According to claim 1 and 2 or 3 or 4 described low-grade magnesites produce high purity magnesium hydroxide and method of magnesium oxide, it is characterized in that the ammonium salt solution that gained in the 3rd step is contained free ammonia obtains ammoniacal liquor through operations such as extraction, enrichment and condensation recovery respectively, this ammoniacal liquor was reused in the 3rd step; The ammonium salt solution of gained is reused at second step.
9. low-grade magnesite according to claim 7 is produced high purity magnesium hydroxide and method of magnesium oxide, it is characterized in that the ammonium salt solution that gained in the 3rd step is contained free ammonia obtains ammoniacal liquor through operations such as extraction, enrichment and condensation recovery respectively, this ammoniacal liquor was reused in the 3rd step; The ammonium salt solution of gained is reused at second step.
10. low-grade magnesite according to claim 9 is produced high purity magnesium hydroxide and method of magnesium oxide, it is characterized in that leached mud is the leached mud of iron content aluminium silico-calcium, and leached mud is for the production of the addition material of magnesia oxychloride cement.
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103241751A (en) * | 2013-04-27 | 2013-08-14 | 陕西师范大学 | Preparation method for high-purity magnesium oxide |
| CN104445300A (en) * | 2014-11-14 | 2015-03-25 | 黔南民族师范学院 | Method of preparing magnesium hydroxide and calcium carbonate and separating out phosphorus ores by taking phosphate tailings as raw materials through ammonia circulation process |
| CN105924023A (en) * | 2016-04-25 | 2016-09-07 | 辽宁洁镁科技有限公司 | Preparation method for magnesium oxide raw material and magnesium hydroxide with low particle size by using low-grade magnesite |
| CN106044806A (en) * | 2016-06-06 | 2016-10-26 | 辽宁洁镁科技有限公司 | Method for preparing magnesium hydroxide from magnesite and magnesium hydroxide prepared with method |
| CN106745103A (en) * | 2016-12-19 | 2017-05-31 | 张旭 | The method that magnesite prepares magnesia or magnesia and fibrous magnesium hydroxide |
| CN107902925A (en) * | 2017-11-14 | 2018-04-13 | 大连智讯科技有限公司 | The method of light magnesium oxide is smelted using magnesite |
| CN110028089A (en) * | 2019-03-18 | 2019-07-19 | 辽宁工程技术大学 | A kind of serpentine tailing prepares method of magnesium oxide |
| CN112320826A (en) * | 2020-10-29 | 2021-02-05 | 刘峰 | Method for jointly preparing high-purity magnesium oxide and refined ammonium sulfate by using low-grade magnesite |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107902925A (en) * | 2017-11-14 | 2018-04-13 | 大连智讯科技有限公司 | The method of light magnesium oxide is smelted using magnesite |
| CN110028089A (en) * | 2019-03-18 | 2019-07-19 | 辽宁工程技术大学 | A kind of serpentine tailing prepares method of magnesium oxide |
| CN112320826A (en) * | 2020-10-29 | 2021-02-05 | 刘峰 | Method for jointly preparing high-purity magnesium oxide and refined ammonium sulfate by using low-grade magnesite |
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