CN105256151A - Method for extracting magnesium chloride from serpentine through ethyl alcohol - Google Patents
Method for extracting magnesium chloride from serpentine through ethyl alcohol Download PDFInfo
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- CN105256151A CN105256151A CN201510659926.6A CN201510659926A CN105256151A CN 105256151 A CN105256151 A CN 105256151A CN 201510659926 A CN201510659926 A CN 201510659926A CN 105256151 A CN105256151 A CN 105256151A
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- extraction
- serpentine
- solid
- magnesium chloride
- ethyl alcohol
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to a method for comprehensively utilizing serpentine resources, and belongs to the technical field of chemical engineering of ore rock refining and metal purification. According to the principle of the extraction process in wet metallurgy, ethyl alcohol is selected as an extraction agent, the extraction agent is used for carrying out solid-liquid extraction on metal chlorides generated through reactions under a certain condition, and therefore the metal chlorides are made to be separated from solid silicon dioxide. According to the method, serpentine powder and concentrated hydrochloric acid react in a semi-solid state under high-temperature and high-pressure conditions, and the solid-liquid ratio is 1: 1 to 3: 1; the leaching temperature is 100-200 DEG C, and the reaction time is 2-8 hours; after the complete reaction, the ethyl alcohol is used for extracting magnesium chloride generated by the reacting materials, and the extraction temperature is 25-45 DEG C; extraction is carried out for 10-30 min through magnetic stirring or ultrasonic oscillation, the rotating speed of a rotor is 500-1000 rpm, the ultrasonic frequency is 20-40 kHZ, and an ethanol solution rich in Mg2+ ions and silicon dioxide solid residues are obtained; and the ethanol solution is heated, evaporated and condensed, the ethyl alcohol is recycled, and solid magnesium chloride is obtained at the same time.
Description
Technical field
The present invention relates to the method for comprehensive utilization serpentine resource, belong to ore deposit rock extracting metals purification chemical technology field.
Background technology
China's serpentinite Mineral resources are very abundant, have the features such as mineral deposit is many, scale large, distribution is wide, quality condition is good.Serpentine is the layer silicate mineral be composited by silicon-oxy tetrahedron and hydrogen magnesium octahedron, and its Physicochemical formula is 3MgO2SiO
22H
2o, its main component is MgO and SiO
2, the composition be mingled with has CaO, Fe
2o
3, Al
2o
3; NiO etc.
Extraction mainly acid leaching process at present to the metal oxide in serpentine, and need to take wet processing to obtain various metal and non-metallic products from leaching feed liquid.The wet processing technique of serpentine acid leaching feed liquid, current main method has:
The precipitator method: the precipitator method mainly add lime, ammoniacal liquor, soda ash etc. in pickling liquor, generate the metallic compound of indissoluble, by regulating pH, by each metal ion species fractional precipitation in pickling liquor to obtain different metal product, or foreign ion collective is precipitated, only retain Mg in solution
2+method.Immersion liquid after purification again with precipitation agent with magnesium basic carbonate form precipitation magnesium, after filtration, washing, dry, calcine, pulverize to obtain magnesium oxide product.This method needs to consume a large amount of alkali, and precipitation process can lose magnesium with a small amount of magnesium hydrate precipitate simultaneously.In addition, this method can only obtain MgO, MgCO
3deng product, the basic raw material magnesium chloride that electrolytic process produces magnesium directly cannot be obtained.
Crystallization process: reclaim magnesium from acidleach filtrate, common crystallization process has condensing crystal method and crystallisation by cooling method.Condensing crystal makes solution supersaturation by the method for heating evaporation solvent, thus separate out solute crystals will; Crystallisation by cooling is then keep liquor capacity constant, and the saturation solubility reducing solute by reducing solution temperature separates out the method for solvent crystal.This method can prepare crude magnesium product, but the liquid stayed after crystallization is still containing more magnesium, and more acid, processes more difficult.If with the merging of acidleach filter cake washing lotion is back to use in acidleach, recycle, finally can cause the accumulation of impurity component, so that acidleach system impurity concentration increases, acidleach cannot circulate down.
Solvent extration: solvent extraction is the effective ways of a kind of separation from solution, enrichment, extraction useful matter, it utilizes the difference of solute between two kinds of mutual exclusive liquid phases to distribute the object reaching separation and enrichment.Magnesium has less ionic radius in aqueous, has larger hydration energy, comparatively easily reacts with multiple extraction agent.From bittern, extract magnesium with phosphodiester, the magnesium chloride of acquisition and magnesium sulfate can reach high-grade pure product.
Summary of the invention
Main or based on pickling process for the current comprehensive utilization to serpentine, produce a large amount of pickling liquors and cause the problem of the cost up of the difficult and subsequent metal extraction of waste liquid and be unfavorable for the problem that large-scale production utilizes.According to hydrometallurgy and chemical principle, react in the semi-solid state under taking concentrated hydrochloric acid and serpentine breeze High Temperature High Pressure, with ethanol, extracting and separating solid silica is carried out to the magnesium chloride wherein generated, extraction efficiency was carried by stirring or ultrasonic method, finally ethanol is steamed reuse and obtain acidity lower solid metal magnesium chloride residue, be convenient to the purification of subsequent metal.
A method for magnesium chloride in alcohol extraction serpentine, is characterized in that having following technological process and step:
A) serpentine ore is ground to form powdered granule;
B) be placed in autoclave by the powdered granule of (a) gained, add concentrated hydrochloric acid and airtight acid-leaching reaction with certain solid-to-liquid ratio, acidleach temperature controls at 100 ~ 200 DEG C, 2 ~ 8 hours reaction times, and the mass ratio of serpentine and concentrated hydrochloric acid is 1:1 ~ 3:1;
C) by molten in dehydrated alcohol for the reaction mass after reacting completely, temperature controls at 25 DEG C ~ 45 DEG C, filters with after rotor speed to be the magnetic agitation of 500 ~ 1000rpm or ultrasonic frequency the be sonic oscillation extraction 10 ~ 30min of 20 ~ 40kHZ;
D) the muriate ethanolic soln after (c) being filtered is 78 ~ 85 DEG C of distillations, and ethanol steams reuse, obtains the solid metal chlorides that composition is mainly magnesium chloride.
The present invention's ethanol extracts the magnesium chloride reacting generation under High Temperature High Pressure, and due to volatility and the lower boiling of ethanol, lower temperature can steam by ethanol, and can reach the object of reuse, saves consumption and the raw materials cost of the energy.In addition, the lower solid magnesium chloride of acidity will be obtained after ethanol evaporate to dryness, the generation of no acidic waste liquid and be conducive to the purification of follow-up metal, reduce alkali consumption.
Embodiment
After now embodiments of the invention being described in.
embodiment 1
Technological process and the step of the present embodiment are described below:
The serpentine breeze of serpentine gained after pulverizing attrition process process in serpentinite ore deposit will be picked up from, cross 100 mesh sieves, serpentine breeze and concentrated hydrochloric acid are mixed in autoclave and heat, solid-liquid weight ratio is 2:1, it is 200 DEG C that temperature controls, and the reaction times is 2 hours.The magnesium chloride generated after reaction is present in the reaction mass of semi-solid state, carries out liquid-solid extraction, reach 93% to the percentage extraction of magnesium chloride under temperature 45 C with dehydrated alcohol to magnesium chloride.
embodiment 2
Technological process and the step of the present embodiment are described below:
The serpentine breeze of serpentine gained after pulverizing attrition process process in serpentinite ore deposit will be picked up from, cross 100 mesh sieves, serpentine breeze and concentrated hydrochloric acid are mixed in autoclave and heat, solid-liquid weight ratio is 2:1, it is 200 DEG C that temperature controls, and the reaction times is 2 hours.The magnesium chloride generated after reaction is present in the reaction mass of semi-solid state, at room temperature with dehydrated alcohol, liquid-solid extraction is carried out to magnesium chloride, accelerate extraction process by magnetic agitation, rotor speed 500rpm, churning time 20min, reaches 98% to the percentage extraction of magnesium chloride.
embodiment 3
Technological process and the step of the present embodiment are described below:
The serpentine breeze of serpentine gained after pulverizing attrition process process in serpentinite ore deposit will be picked up from, cross 100 mesh sieves, serpentine breeze and concentrated hydrochloric acid are mixed in autoclave and heat, solid-liquid weight ratio is 2:1, it is 200 DEG C that temperature controls, and the reaction times is 2 hours.The magnesium chloride generated after reaction is present in the reaction mass of semi-solid state, at room temperature carry out liquid-solid extraction with dehydrated alcohol to magnesium chloride, accelerate extraction process by sonic oscillation, ultrasonic frequency is 40kHZ, ultrasonic time 20min, reaches 100% to the percentage extraction of magnesium chloride.
Claims (1)
1., by a method for the magnesium chloride in alcohol extraction serpentine, it is characterized in that there is following technological process and step:
A) serpentine ore is ground to form powdered granule;
B) be placed in autoclave by the powdered granule of (a) gained, add concentrated hydrochloric acid and airtight acid-leaching reaction with certain solid-to-liquid ratio, acidleach temperature controls at 100 ~ 200 DEG C, 2 ~ 8 hours reaction times, and the mass ratio of serpentine and concentrated hydrochloric acid is 1:1 ~ 3:1;
C) by molten in dehydrated alcohol for the reaction mass after reacting completely, temperature controls at 25 DEG C ~ 45 DEG C, filters with after rotor speed to be the magnetic agitation of 500 ~ 1000rpm or ultrasonic frequency the be sonic oscillation extraction 10 ~ 30min of 20 ~ 40kHZ;
D) the muriate ethanolic soln after (c) being filtered is 78 ~ 85 DEG C of distillations, and ethanol steams reuse, obtains the solid metal chlorides that composition is mainly magnesium chloride.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510659926.6A CN105256151B (en) | 2015-10-14 | 2015-10-14 | The method that the magnesium chloride in serpentine is extracted with ethanol |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510659926.6A CN105256151B (en) | 2015-10-14 | 2015-10-14 | The method that the magnesium chloride in serpentine is extracted with ethanol |
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| Publication Number | Publication Date |
|---|---|
| CN105256151A true CN105256151A (en) | 2016-01-20 |
| CN105256151B CN105256151B (en) | 2017-07-21 |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2381994A (en) * | 1941-11-21 | 1945-08-14 | Kellogg M W Co | Production of anhydrous magnesium chloride |
| CN1603235A (en) * | 2004-11-01 | 2005-04-06 | 北京中信国安盟固利新材料技术研究院有限公司 | Method for preparing anhydrous magnesium chloride |
| CN1827804A (en) * | 2006-03-30 | 2006-09-06 | 上海大学 | Method for comprehensively utilizing serpentine resource |
| CN1911799A (en) * | 2006-09-01 | 2007-02-14 | 上海大学 | Method of preparing nanometer SiO2 from ophiolite |
-
2015
- 2015-10-14 CN CN201510659926.6A patent/CN105256151B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2381994A (en) * | 1941-11-21 | 1945-08-14 | Kellogg M W Co | Production of anhydrous magnesium chloride |
| CN1603235A (en) * | 2004-11-01 | 2005-04-06 | 北京中信国安盟固利新材料技术研究院有限公司 | Method for preparing anhydrous magnesium chloride |
| CN1827804A (en) * | 2006-03-30 | 2006-09-06 | 上海大学 | Method for comprehensively utilizing serpentine resource |
| CN1911799A (en) * | 2006-09-01 | 2007-02-14 | 上海大学 | Method of preparing nanometer SiO2 from ophiolite |
Non-Patent Citations (2)
| Title |
|---|
| 李新义等: "高纯无水氯化镁的制备及制镁工艺", 《化学工业与工程》 * |
| 马芬兰，包温姬: "高纯无水氯化镁的制备及制镁工艺探究", 《化工管理》 * |
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|---|---|
| CN105256151B (en) | 2017-07-21 |
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