CN103864122A - Method for preparing magnesium hydroxide from phosphate tailings with high magnesium content - Google Patents
Method for preparing magnesium hydroxide from phosphate tailings with high magnesium content Download PDFInfo
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- CN103864122A CN103864122A CN201410085908.7A CN201410085908A CN103864122A CN 103864122 A CN103864122 A CN 103864122A CN 201410085908 A CN201410085908 A CN 201410085908A CN 103864122 A CN103864122 A CN 103864122A
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Abstract
The invention discloses a method for preparing magnesium hydroxide from phosphate tailings with high magnesium content. The method comprises the following steps: (1), calcining the phosphate tailings with high magnesium content at a temperature of 850-1100 DEG C to form calcined dolomite; (2), adding the calcined dolomite into an ammonium sulfate solution, dropwise adding concentrated sulfuric acid to control a pH value to be 6.0-6.5, keeping a temperature of a reaction system at 95-100 DEG C to react for 40-80 minutes and absorbing ammonia gas coming out of the reaction system through water to obtain ammonia water; (3), filtering after the reaction is completed to obtain filtrate and a filter cake; (4), mixing the filtrate of the step (3) with the ammonia water obtained in the step (2), introducing the ammonia gas or adding liquid ammonia or the ammonia water to control magnesium hydroxide to precipitate, filtering after the precipitation is completed, washing and drying the filter cake to obtain a magnesium hydroxide product, and collecting filtrate as a raw material solution of the ammonium sulfate solution in the step (2). The method is capable of turning waste into wealth and recycling waste phosphate tailings with high magnesium content for preparing the magnesium hydroxide, simple in process and significant in economic and environmental benefits.
Description
Technical field
The present invention relates to the high magnesium phosphorus of a kind of use mine tailing and prepare the method for magnesium hydroxide, belong to chemical technique field.
Background technology
The phosphorus ore great majority of China be in low-grade phosphorus ore, generally need to become high-grade phosphorus heading by floating and enriching could use.High magnesium phosphorus mine tailing is that Rock Phosphate (72Min BPL) obtains the byproduct after phosphorus concentrate by floating and enriching, and its main component is calcium magnesium phosphorus, wherein P
2o
5content is 3%-10%, and MgO content is being 15%-20%, and the content of CaO is 28%-42%, belongs to the low-phosphorous phosphorus ore of high magnesium.At present both at home and abroad the processing of phosphate rock floating mine tailing is mainly taked to build a dam to store up, it is seldom utilized.By-product phosphorus comprehensive utilization of tailing rate that China phosphorus ore industry is produced is low is only 7% left and right, and a large amount of phosphorus mine tailings can only be deposited in Tailings Dam for a long time, and the mine tailing that is discharged into mine tailing district also can cause serious impact to surrounding environment., become a potential safety hazard point.At present, the today day by day reducing in resource, mine tailing, as secondary resource, enjoys common people to pay close attention to.Therefore, rational exploitation and utilization phosphorite tailings can not only produce certain economic benefit, and the Implement of sustainable development strategy is had to great social effect.
Chinese patent application CN102674407A discloses a kind of method of utilizing high magnesium phosphorus mine tailing to produce light magnesium oxide, and Chinese patent application CN102653408A discloses a kind of method of utilizing high magnesium phosphorus mine tailing to produce Magnesium Carbonate Light 41-45.Chinese patent application CN102534253A discloses and has a kind ofly utilized high magnesium phosphorus mine tailing melting and reducing to prepare the method for MAGNESIUM METAL.These patents have all embodied the thinking that high magnesium phosphorus mine tailing is rationally utilized, but at present, also do not produce the report of the method for magnesium hydroxide with high magnesium phosphorus mine tailing.
Magnesium hydroxide is a kind of novel filled-type fire retardant, during by decomposes, discharge in conjunction with water, absorb a large amount of latent heat, reduce synthetic materials that it the fills surface temperature in flame, there is the polymer unwinds of inhibition and produced inflammable gas is carried out to cooling effect.Decomposing the magnesium oxide generating is again good refractory materials, also can help to improve the fire resistance of synthetic materials, and the water vapour that it is emitted simultaneously also can be used as a kind of smoke suppressant.Magnesium hydroxide be in generally acknowledged rubber and plastic industry, have fire-retardant, press down cigarette, fill the outstanding fire retardant of triple functions.Be widely used in the macromolecular materials such as rubber, chemical industry, building materials, plastics and electronics, unsaturated polyester and paint, coating.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of and utilizes high magnesium phosphorus mine tailing to prepare the method for magnesium hydroxide, and technique is simple, in good product quality, production process without the three wastes, environmental protection.
Technical scheme of the present invention is as follows: the high magnesium phosphorus of a kind of use mine tailing is prepared the method for magnesium hydroxide, comprises the following steps:
(1), high magnesium phosphorus mine tailing is calcined at 850-1100 DEG C, burn till forge white;
(2), forge white adding in ammoniumsulphate soln above-mentioned, drip vitriol oil control pH between 6.0-6.5, keep temperature of reaction system at 95-100 DEG C of reaction 40-80 minute, from reaction system, ammonia water out absorbs and obtains ammoniacal liquor;
(3), reacted rear filtration, obtain filtrate and filter cake,
(4), the filtrate of step (3) is mixed with the ammoniacal liquor obtaining in step (2), and pass into ammonia or add liquefied ammonia or ammoniacal liquor control magnesium hydrate precipitate, precipitate rear filtration, filter cake obtains magnesium hydroxide products through washing, being dried, and filtrate collection plays the stock liquid as the ammoniumsulphate soln of step (2).
As preferably: in step (2), described in forge magnesium oxide in white and the mol ratio of ammonium sulfate is 1:2.0-3.0.
In technique scheme: in step (2), drip when the vitriol oil, temperature of reaction system rises, in the time of temperature rise to 80 DEG C, should control the speed that drips the vitriol oil, the speed that reaction system is heated up is 0.1-1 DEG C/min.Be conducive to separating out and the recovery of ammonia of impurity.
In technique scheme: the concentration of described ammoniumsulphate soln is 2.0mol/L.
In technique scheme: the filter cake obtaining in step (3) is sent into ammonium phosphate plant and recycled.Filter cake main component is the impurity such as calcium monofluorophosphate, iron, calcium, aluminium, silicon.
In technique scheme: in step (4), the pH that controls reaction system during with ammoniacal liquor or liquid ammonia deposition magnesium hydroxide is 10.Be conducive to like this precipitation of magnesium hydroxide.
In technique scheme: in step (4), while adding ammonia or ammoniacal liquor or liquefied ammonia, should control reaction system temperature of reaction is 35-40 DEG C.
In technique scheme: P in described high magnesium phosphorus mine tailing
2o
5content is 3%-10%, and MgO content is 15%-20%.
Beneficial effect: tool of the present invention has the following advantages (1) the present invention, and to utilize industrial waste object height magnesium phosphorus mine tailing be raw material, saved resource.
(2) the present invention is in step (2), by controlling temperature and the pH value of reaction system, the impurity such as iron, calcium, aluminium, silicon are stayed in slag, by removing by filter, thereby in the time that next step precipitates, obtain the magnesium hydroxide that purity is high, the purity of the magnesium hydroxide of preparation is greater than 95%.
(3) the technology of the present invention can be applied to a large amount of processing of high magnesium phosphorus mine tailing, processes high magnesium phosphorus mine tailing a kind of effective means is provided for phosphorate rock mining and ore dressing.
(4) the invention solves the problem of high magnesium phosphorus mine tailing land occupation resource, environmental pollution, turn waste into wealth, there is good economic benefit and environment protection significance.
Embodiment
Below in conjunction with embodiment, the invention will be further described:
Embodiment 1:
High magnesium phosphorus mine tailing composition: P
2o
5%:5.38%, MgO%:16.05%
Take high magnesium phosphorus mine tailing 100g calcines at 850 DEG C, obtain forging white 61.4g, under agitation by forging in the ammoniumsulphate soln of the white 0.5L2.0mol/L of adding (ammonium sulfate with magnesian mol than being 2.5:1), drip the industrial vitriol oil (mass concentration is 98%) and control pH value between 6.0-6.5, when dripping when the vitriol oil, temperature of reaction system raises, in the time of temperature rise to 80 DEG C left and right, control the speed that drips the vitriol oil, the speed that reaction system is heated up is 0.1-1 DEG C/min.Be conducive to ammonia overflow and precipitate separate out.Then keep temperature of reaction system at 95 DEG C, reaction 40min.The ammonia water overflowing absorbs and obtains ammoniacal liquor.Reacted rear filtration, and washed filter cake with water and wash, filtrate is heavy magnesium water, and filter cake is delivered to ammonium phosphate plant and recycled.Heavy magnesium water is mixed with ammoniacal liquor obtained above, and the temperature of controlling reaction is 35 DEG C, in 40 minutes, adds liquefied ammonia, controls pH10.0 left and right.By slip ageing, within several hours, extremely precipitation is complete, filters, and filter cake hot wash, dries and obtain magnesium hydroxide products, and product purity is 95.2%.Filtrate is forging the white raw materials recovery utilization as ammoniumsulphate soln while reacting with ammonium sulfate.
Case study on implementation 2
High magnesium phosphorus mine tailing composition: P2O5%:6.35%, MgO%:18.59%
Take high magnesium phosphorus mine tailing 100g calcines at 900 DEG C, obtain forging white 60.4g, under agitation by forging in the ammoniumsulphate soln of the white 0.46L2.0mol/L of adding (ammonium sulfate with magnesian mol than being 2.0:1), drip the industrial vitriol oil (mass concentration is 98%) and control pH value between 6.0-6.5, when dripping when the vitriol oil, temperature of reaction system raises, in the time of temperature rise to 80 DEG C left and right, control the speed that drips the vitriol oil, the speed that reaction system is heated up is 0.1-1 DEG C/min.Be conducive to ammonia overflow and precipitate separate out.Then keep temperature of reaction system at 100 DEG C, reaction 60min.The ammonia water overflowing absorbs and obtains ammoniacal liquor.Reacted rear filtration, and washed filter cake with water and wash, filtrate is heavy magnesium water, and filter cake is delivered to ammonium phosphate plant and recycled.Heavy magnesium water is mixed with ammoniacal liquor obtained above, and the temperature of controlling reaction is 40 DEG C, in 45 minutes, passes into ammonia, controls pH10.0 left and right.By slip ageing, within several hours, extremely precipitation is complete, filters, and filter cake hot wash, dries and obtain magnesium hydroxide products.Product purity is 96.1% filtrate forging the white raw materials recovery utilization as ammoniumsulphate soln while reacting with ammonium sulfate.
Case study on implementation 3
High magnesium phosphorus mine tailing composition: P2O5%:9.84%, MgO%:15.03%
Take high magnesium phosphorus mine tailing 100g calcines at 1100 DEG C, obtain forging white 65.3g, under agitation by forging in the ammoniumsulphate soln of the white 0.57L2.0mol/L of adding (ammonium sulfate with magnesian mol than being 3.0:1), drip the industrial vitriol oil (mass concentration is 98%) and control pH value between 6.0-6.5, when dripping when the vitriol oil, temperature of reaction system raises, in the time of temperature rise to 80 DEG C left and right, control the speed that drips the vitriol oil, the speed that reaction system is heated up is 0.1-1 DEG C/min.Be conducive to ammonia overflow and precipitate separate out.Then keep temperature of reaction system at 98 DEG C, reaction 80min.The ammonia water overflowing absorbs and obtains ammoniacal liquor.Reacted rear filtration, and washed filter cake with water and wash, filtrate is heavy magnesium water, and filter cake is delivered to ammonium phosphate plant and recycled.Heavy magnesium water is mixed with ammoniacal liquor obtained above, and the temperature of controlling reaction is 35 DEG C, adds ammoniacal liquor (mass concentration is 25-28%) in 45 minutes, controls pH10.0 left and right.By slip ageing, within several hours, extremely precipitation is complete, filters, and filter cake hot wash, dries and obtain magnesium hydroxide products.Product purity is 95.8 filtrates forging the white raw materials recovery utilization as ammoniumsulphate soln while reacting with ammonium sulfate.
Claims (8)
1. a method of preparing magnesium hydroxide with high magnesium phosphorus mine tailing, is characterized in that: comprise the following steps:
(1), high magnesium phosphorus mine tailing is calcined at 850-1100 DEG C, burn till forge white;
(2), forge white adding in ammoniumsulphate soln above-mentioned, drip vitriol oil control pH between 6.0-6.5, keep temperature of reaction system at 95-100 DEG C of reaction 40-80 minute, from reaction system, ammonia water out absorbs and obtains ammoniacal liquor;
(3), reacted rear filtration, obtain filtrate and filter cake,
(4), the filtrate of step (3) is mixed with the ammoniacal liquor obtaining in step (2), and pass into ammonia or add liquefied ammonia or ammoniacal liquor control magnesium hydrate precipitate, precipitate rear filtration, filter cake obtains magnesium hydroxide products through washing, being dried, and filtrate collection is as the stock liquid of the ammoniumsulphate soln of step (2).
2. the method for preparing according to claim 1 magnesium hydroxide with high magnesium phosphorus mine tailing, is characterized in that: in step (2), described in forge magnesium oxide in white and the mol ratio of ammonium sulfate is 1:2.0-3.0.
3. prepare according to claim 1 the method for magnesium hydroxide with high magnesium phosphorus mine tailing, it is characterized in that: in step (2), while dripping the vitriol oil, temperature of reaction system rises, in the time of temperature rise to 80 DEG C, should control the speed that drips the vitriol oil, the speed that reaction system is heated up is 0.1-1 DEG C/min.
4. according to the method for preparing magnesium hydroxide described in claim 1-3 any one with high magnesium phosphorus mine tailing, it is characterized in that: the filter cake obtaining in step (3) is sent into ammonium phosphate plant and recycled.
5. according to the method for preparing magnesium hydroxide described in claim 1-3 any one with high magnesium phosphorus mine tailing, it is characterized in that: the concentration of described ammoniumsulphate soln is 2.0mol/L.
6. according to the method for preparing magnesium hydroxide described in right pressure ball 1 with high magnesium phosphorus mine tailing, it is characterized in that: in step (4), the pH that controls reaction system during with ammonia or ammoniacal liquor or liquid ammonia deposition magnesium hydroxide is 10.
7. according to the method for preparing magnesium hydroxide described in claim 1 or 6 with high magnesium phosphorus mine tailing, it is characterized in that: in step (4), while adding ammonia or ammoniacal liquor or liquefied ammonia, should control reaction system temperature of reaction is 35-40 DEG C.
8. the method for preparing according to claim 1 magnesium hydroxide with high magnesium phosphorus mine tailing, is characterized in that: P in described high magnesium phosphorus mine tailing
2o
5content is 3%-10%, and MgO content is 15%-20%.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104071813A (en) * | 2014-07-08 | 2014-10-01 | 中国科学院青海盐湖研究所 | Method for preparing magnesium hydroxide |
| CN104387121A (en) * | 2014-11-10 | 2015-03-04 | 瓮福（集团）有限责任公司 | Method for preparing phosphorus-magnesium fertilizer |
| CN104445299A (en) * | 2014-10-30 | 2015-03-25 | 瓮福（集团）有限责任公司 | Method for preparing high-purity magnesium hydroxide |
| CN104528780A (en) * | 2014-12-25 | 2015-04-22 | 武汉工程大学 | Method for preparing in-situ modified nano-magnesium hydroxide by taking phosphate tailings as raw materials |
| CN104528778A (en) * | 2014-12-25 | 2015-04-22 | 武汉工程大学 | Process for producing in-situ modified nano-magnesium hydroxide by taking phosphate tailings as raw materials |
| CN105984890A (en) * | 2015-02-26 | 2016-10-05 | 宝山钢铁股份有限公司 | Method for producing flame retardant grade magnesium hydrate from oriented silicon steel magnesium oxide waste |
| CN109400959A (en) * | 2018-11-09 | 2019-03-01 | 中国地质大学（武汉） | A kind of metal organic frame package flame retardant of magnesium hydroxide and preparation method thereof |
| CN111116175A (en) * | 2019-12-24 | 2020-05-08 | 湖北冶金地质研究所(中南冶金地质研究所) | Method for producing refractory material for cement kiln by using calcium magnesium phosphate ore tailings |
| CN111302372A (en) * | 2019-12-31 | 2020-06-19 | 黔南民族师范学院 | Method for separating and extracting magnesium and calcium from phosphate tailings treated by secondary ammonium salt |
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| CN101215108A (en) * | 2008-01-18 | 2008-07-09 | 沈阳化工学院 | Method for producing series function magnesium chemical products by using magnesite |
| CN101525144A (en) * | 2009-04-08 | 2009-09-09 | 辽宁红豆杉技术发展有限公司 | Method for preparing uniform granular magnesium hydrate by one-step reaction with ammonia bubbling method |
| CN102557086A (en) * | 2012-02-18 | 2012-07-11 | 贵州大学 | Method for recovering phosphorus from phosphorite tailings and preparing light magnesium oxide |
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Patent Citations (3)
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| CN101215108A (en) * | 2008-01-18 | 2008-07-09 | 沈阳化工学院 | Method for producing series function magnesium chemical products by using magnesite |
| CN101525144A (en) * | 2009-04-08 | 2009-09-09 | 辽宁红豆杉技术发展有限公司 | Method for preparing uniform granular magnesium hydrate by one-step reaction with ammonia bubbling method |
| CN102557086A (en) * | 2012-02-18 | 2012-07-11 | 贵州大学 | Method for recovering phosphorus from phosphorite tailings and preparing light magnesium oxide |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104071813A (en) * | 2014-07-08 | 2014-10-01 | 中国科学院青海盐湖研究所 | Method for preparing magnesium hydroxide |
| CN104445299A (en) * | 2014-10-30 | 2015-03-25 | 瓮福（集团）有限责任公司 | Method for preparing high-purity magnesium hydroxide |
| CN104387121A (en) * | 2014-11-10 | 2015-03-04 | 瓮福（集团）有限责任公司 | Method for preparing phosphorus-magnesium fertilizer |
| CN104387121B (en) * | 2014-11-10 | 2017-03-08 | 瓮福（集团）有限责任公司 | A kind of method preparing phosphorus fertiliser containing magnesium |
| CN104528780A (en) * | 2014-12-25 | 2015-04-22 | 武汉工程大学 | Method for preparing in-situ modified nano-magnesium hydroxide by taking phosphate tailings as raw materials |
| CN104528778A (en) * | 2014-12-25 | 2015-04-22 | 武汉工程大学 | Process for producing in-situ modified nano-magnesium hydroxide by taking phosphate tailings as raw materials |
| CN105984890A (en) * | 2015-02-26 | 2016-10-05 | 宝山钢铁股份有限公司 | Method for producing flame retardant grade magnesium hydrate from oriented silicon steel magnesium oxide waste |
| CN105984890B (en) * | 2015-02-26 | 2017-11-28 | 宝山钢铁股份有限公司 | The method that orientation silicon steel magnesia discarded object produces flame-proof magnesium hydroxide |
| CN109400959A (en) * | 2018-11-09 | 2019-03-01 | 中国地质大学（武汉） | A kind of metal organic frame package flame retardant of magnesium hydroxide and preparation method thereof |
| CN109400959B (en) * | 2018-11-09 | 2019-12-17 | 中国地质大学（武汉） | Magnesium hydroxide flame retardant wrapped by metal organic framework and preparation method thereof |
| CN111116175A (en) * | 2019-12-24 | 2020-05-08 | 湖北冶金地质研究所(中南冶金地质研究所) | Method for producing refractory material for cement kiln by using calcium magnesium phosphate ore tailings |
| CN111302372A (en) * | 2019-12-31 | 2020-06-19 | 黔南民族师范学院 | Method for separating and extracting magnesium and calcium from phosphate tailings treated by secondary ammonium salt |
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