CN104843748A - Low-grade magnesite and low-grade magnesite tailing comprehensive recycling use method - Google Patents
Low-grade magnesite and low-grade magnesite tailing comprehensive recycling use method Download PDFInfo
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- CN104843748A CN104843748A CN201410051735.7A CN201410051735A CN104843748A CN 104843748 A CN104843748 A CN 104843748A CN 201410051735 A CN201410051735 A CN 201410051735A CN 104843748 A CN104843748 A CN 104843748A
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- grade magnesite
- magnesium sulfate
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Abstract
The invention discloses a low-grade magnesite comprehensive recycling use method including the following steps: (1) low-grade magnesite or low-grade magnesite tailing is crushed into a finely crushed ore sample; (2) part of the finely crushed ore sample of the step (1) is reacted with sulfuric acid to obtain CO2 gas and magnesium sulfate heptahydrate solution; and the rest of the ore sample of the step (1) is heated, decomposed and hydrated at high temperature, the CO2 gas is introduced into a hydration fluid for carbonization, and by pyrolysis of the carbonized product, magnesium oxide is obtained. In the process of preparation of high purity magnesium oxide, no chemical is added, in the process of carbonization, the CO2 gas produced in preparation of magnesium sulfate is used for realization of a high efficient technological process, by use of the production process, the efficient utilization of the low-grade magnesite can be realized, and the process is relatively simple, efficient and environmentally friendly.
Description
Technical field
The present invention be more particularly directed to a kind of low-grade magnesite and tailings comprehensive recycling novel process thereof, belong to mineral processing and metallurgical technology field.
Background technology
In the Mineral resources of China proven reserve, magnesite proven reserve 2.89 × 10
9t, accounts for 30.1% of world's proven reserve, occupies first place in the world.Although China's magnesite ore quality majority is excellent, can the select quality ore of calcination of high-purity magnesia but only have few of ore deposits to have, and the most all degree of low-grade magnesite (being less than 90% by content meter) different containing detrimental impurity, can not, directly as high-grade raw material, make its market value low.It is mostly raw material preliminary working product that current China produces with the magnesian of outlet, differs tens times with the benefit of expensive goods.And for the process of low-grade magnesite, be all generally abandon do not adopt or store up placement, therefore develop extremely urgent to low-grade magnesite, the demand in market also requires that China's magnesium products must high added value and functionalization simultaneously.In prior art, flotation, heat choosing are mainly contained for the process of low-grade magnesite.Purification by floatation magnesite also exists technical process complexity, invests the shortcomings such as large, and to the ferric oxide existed with class matter homophase in rhombspar, calcite and the separation difficulty of calcium oxide.It is high to there is energy consumption in heat choosing, the shortcomings such as minerals separation purification is not thorough, cause its enforcement to there is not practicality.
Summary of the invention
The invention provides a kind of low-grade magnesite and tailings comprehensive recycling novel process thereof, it is not high that the method can solve current low-grade magnesite resource utilization, other components are underutilized, and mine tailing bulk deposition land occupation and the problem of contaminate environment.
A kind of low-grade magnesite comprehensive reutilization method provided by the invention, comprises the steps:
(1) low-grade magnesite or its mine tailing are milled to sample ore fineness and are no more than 200 orders;
(2) by the levigate sample ore of part in step (1) and sulfuric acid reaction, gas CO is obtained
2with magnesium sulfate heptahydrate solution; By all the other sample ore thermal degradation of step (1) and high temperature aquation, and by gas CO
2pass in hydrating fluid and carry out carbonization, the product after carbonization obtains magnesium oxide through pyrolysis.
Preferably, be the carbonic acid gas that levigate sample ore and sulfuric acid reaction obtain for the carbonic acid gas of carbonization in described step (2).
Preferably, CO
2collection adopt draining water gathering of gas law.
Preferably, after described carbonization, the pH value of liquid controls to be 7 ~ 8, when after carbonization, liquid controls within the scope of this pH, the utilization ratio of reaction efficiency and each component comparatively passes into the carbonic acid gas carbonization better effects if of other amounts, and can the rate of recovery of controlled oxidization magnesium 70% ~ 90%.During carbonization, the speed of the gas passed into should be determined according to the concentration of reaction vessel and reaction solution, those skilled in the art can select as required flexibly, such as the speed of 1 ~ 20mL/s is taked to pass into for small-sized container, solid in the carbodiimide solution obtained is the product treating pyrolysis, it can wash after filtration, then carries out corresponding pyrolysis step.
Preferably, described method also comprises: described Adlerika is through purifying treatment, and purifying treatment condition is regulate pH to be about 1 ~ 3 blowing air, deironing.
Preferred, described method also comprises, and the magnesium sulfate heptahydrate after purification obtains magnesium sulfate heptahydrate crystal through crystallization, and in crystallisation process, temperature controls at 50 ~ 70 DEG C, ensures the purity obtaining product.The magnesium sulfate heptahydrate crystal prepared according to method of the present invention, purity is more than 98.00%, and the rate of recovery is 70 ~ 90%.
Preferably, in described step (2), the thermal degradation temperature of sample ore is 700 ~ 1000 DEG C, preferred 700-900 DEG C, and the temperature of high temperature aquation controls at 60 ~ 90 DEG C.
Preferably, in described step (2), the pyrolysis of carbonized product comprises once decomposes and secondary pyrolysis, and a described decomposition temperature controls to be 60 ~ 90 DEG C, and the time of decomposition can control at 2 ~ 5h, and the solid product obtained is magnesiumcarbonate, and it is for secondary pyrolysis; Described secondary pyrolysis temperature is 700 ~ 1000 DEG C, and the time can control at 2 ~ 4h, and the product after twice decomposition is high-purity magnesium oxide.
According to high-purity magnesium oxide prepared by method of the present invention, purity is more than 99.7%, and the rate of recovery is 70% ~ 90%.
The present invention prepares in the process of high-purity magnesium oxide and does not add any chemical agent, and in carbonization process, make use of the gas CO preparing magnesium sulfate and produce
2, achieve the high efficiency of technical process.Adopt this kind of production technique, can realize the efficiency utilization of low-grade magnesite, present invention process is relatively simple, high-efficiency environment friendly.
Accompanying drawing explanation
The method schematic diagram that Fig. 1, low-grade magnesite and tailings comprehensive thereof are recycled.
Embodiment
Embodiment 1: somewhere, Shandong magnesite main chemical compositions formula: MgO82.20%, SiO
27.62%, CaO4.23%, Fe
2o
32.58%, Al
2o
32.41%.Mineral composition: be mainly magnesite, gangue mineral is mainly quartz etc.
See Fig. 1, the method that low-grade magnesite and tailings comprehensive thereof are recycled comprises:
(1) by sample ore after ore grinding, get the sample ore 100g of-200 orders 100%, react 120min with 50ml sulfuric acid at 90 DEG C, collect CO
2, obtain magnesium sulfate liquid, by magnesium sulfate liquid filtering, controlling filtrate temperature is 50 DEG C, and obtain magnesium sulfate heptahydrate, purity is 98.51%, and the rate of recovery is 75%;
(2) the sample ore 100g of-200 orders 100% is taken, control temperature 800 DEG C in rotary kiln, reaction 120min, take out sample ore, aquation 90min in the water-bath of 80 DEG C, by hydrating fluid carbonization at normal temperatures and pressures, the pH of regulator solution, makes it drop to less than 8, filters, filtrate is heated 120min in the water-bath of 80 DEG C, filters, obtain filter cake, dry, in the retort furnace of 800 DEG C, pyrolysis 2h, obtains magnesium oxide, purity is 99.80%, and the rate of recovery is 79%.
This routine result of implementation is: the final magnesium sulfate grade obtained is 98.51%, and the rate of recovery is 75%; The magnesium oxide purity obtained is 99.80%, and the rate of recovery is 79%.
Embodiment 2: In A Certain Place of Xinjiang magnesite main chemical compositions formula: MgO80.96%, SiO
21.89%, CaO7.78%, Fe
2o
30.53%, Al
2o
31.62%.Mineral composition: be mainly magnesite, gangue mineral is mainly calcium carbonate etc.
(1) by sample ore after grinding machine ore grinding, get the sample ore 100g of-200 orders 100%, react 90min with 70ml sulfuric acid at 80 DEG C, collect CO
2, obtain magnesium sulfate liquid, by magnesium sulfate liquid filtering, controlling filtrate temperature is 60 DEG C, and obtain magnesium sulfate heptahydrate, purity is 98.87%, and the rate of recovery is 72%;
(2) the sample ore 100g of-200 orders 100% is taken, control temperature 750 DEG C in rotary kiln, reaction 120min, take out sample ore, aquation 90min in the water-bath of 80 DEG C, by hydrating fluid carbonization at normal temperatures and pressures, the pH of regulator solution, to less than 7, filters, filtrate is heated 90min in the water-bath of 80 DEG C, filter, obtain filter cake, dry, pyrolysis 2h in the retort furnace of 1000 DEG C, obtain magnesium oxide, purity is 99.92%, and the rate of recovery is 71%.
This routine result of implementation is: the final magnesium sulfate grade obtained is 98.87%, and the rate of recovery is 72%; The magnesium oxide purity obtained is 99.92%, and the rate of recovery is 71%.
Embodiment 3: somewhere, Anshan Brick With Magnesite Purified By Flotation mine tailing main chemical compositions formula: MgO78.69%, SiO
29.84%, CaO3.97%, Fe
2o
33.36%, Al
2o
32.92%.Mineral composition: be mainly magnesite, gangue mineral is mainly quartz etc.
(1) by mine tailing sample ore after grinding machine ore grinding, get the sample ore 100g of-200 orders 100%, react 90min with 60ml sulfuric acid at 80 DEG C, collect CO
2, obtain magnesium sulfate liquid, by magnesium sulfate liquid filtering, controlling filtrate temperature is 55 DEG C, and obtain magnesium sulfate heptahydrate, purity is 98.45%.The rate of recovery is 78%;
(2) the sample ore 100g of-200 orders 100% is taken, control temperature 1000 DEG C in rotary kiln, reaction 90min, take out sample ore, aquation 90min in the water-bath of 90 DEG C, by hydrating fluid carbonization at normal temperatures and pressures, the pH of regulator solution, to less than 7.5, filters, filtrate is heated 100min in the water-bath of 80 DEG C, filter, obtain filter cake, dry, pyrolysis 3h in the retort furnace of 800 DEG C, obtain magnesium oxide, purity is 99.87%, and the rate of recovery is 74%.
This routine result of implementation is: the final magnesium sulfate grade obtained is 98.45%, and the rate of recovery is 78%; The magnesium oxide purity obtained is 99.87%, and the rate of recovery is 74%.
Claims (8)
1. a method for low-grade magnesite and tailings comprehensive recycling thereof, comprises the steps:
(1) low-grade magnesite or its mine tailing are pulverized, obtain levigate sample ore;
(2) by the levigate sample ore of part in step (1) and sulfuric acid reaction, CO is obtained
2gas and magnesium sulfate heptahydrate solution; By all the other sample ore thermal degradation of step (1) and high temperature aquation, and by CO
2gas passes in hydrating fluid and carries out carbonization, and the product after carbonization obtains magnesium oxide through pyrolysis.
2. method according to claim 1, is characterized in that, for the CO of carbonization in step (2)
2for the CO that levigate sample ore and sulfuric acid reaction obtain
2.
3. method according to claim 1 and 2, is characterized in that, in step (2), after carbonization, the pH value of liquid is 7-8.
4. method according to claim 1 and 2, is characterized in that, the CO that levigate sample ore and sulfuric acid reaction generate
2collection adopt draining water gathering of gas law.
5. method according to claim 1, is characterized in that, described method also comprises: described Adlerika is through purifying treatment, and purifying treatment condition is regulate pH to be 1 ~ 3 blowing air, deironing, the magnesium sulfate heptahydrate solution after being purified.
6. method according to claim 5, is characterized in that, the magnesium sulfate heptahydrate solution after purification obtains magnesium sulfate heptahydrate crystal through crystallization, and in crystallisation process, temperature controls at 50 ~ 70 DEG C.
7. method according to claim 1, is characterized in that, in described step (2), the thermal degradation temperature of levigate sample ore is 700 ~ 1000 DEG C, and the temperature of high temperature aquation controls at 60 ~ 90 DEG C.
8. method according to claim 1, is characterized in that, in described step (2), the pyrolysis of carbonized product comprises once decomposes and secondary pyrolysis, and a described decomposition temperature is 60 ~ 90 DEG C, and described secondary pyrolysis temperature is 700 ~ 1000 DEG C.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109970071A (en) * | 2019-05-06 | 2019-07-05 | 辽宁科技大学 | A kind of acid system purifies the production method of low-grade talcum |
| CN111892072A (en) * | 2020-08-05 | 2020-11-06 | 辽宁辰昊镁业有限公司 | Method for preparing magnesium sulfate from magnesite tailings |
Citations (4)
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|---|---|---|---|---|
| CN101104521A (en) * | 2007-06-05 | 2008-01-16 | 昆明贵金属研究所 | Method for treating magnesium sulfate waste liquid and coproducing active magnesium chloride |
| CN101941723A (en) * | 2010-09-08 | 2011-01-12 | 沈阳化工大学 | Method for producing high-activity nano magnesia by utilizing low-grade magnesite |
| CN102030487A (en) * | 2009-09-28 | 2011-04-27 | 王全祥 | New process for preparing high-purity magnesium oxide by normal temperature carbonization and low temperature pyrolysis |
| CN102285674A (en) * | 2010-12-30 | 2011-12-21 | 新疆蓝天伟业科技开发有限公司 | Method for comprehensively utilizing low-grade magnesite |
-
2014
- 2014-02-14 CN CN201410051735.7A patent/CN104843748A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101104521A (en) * | 2007-06-05 | 2008-01-16 | 昆明贵金属研究所 | Method for treating magnesium sulfate waste liquid and coproducing active magnesium chloride |
| CN102030487A (en) * | 2009-09-28 | 2011-04-27 | 王全祥 | New process for preparing high-purity magnesium oxide by normal temperature carbonization and low temperature pyrolysis |
| CN101941723A (en) * | 2010-09-08 | 2011-01-12 | 沈阳化工大学 | Method for producing high-activity nano magnesia by utilizing low-grade magnesite |
| CN102285674A (en) * | 2010-12-30 | 2011-12-21 | 新疆蓝天伟业科技开发有限公司 | Method for comprehensively utilizing low-grade magnesite |
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| 林晓萍: "菱镁矿生产高纯氧化镁工艺研究", 《硅谷》 * |
| 白晶: "由低品位菱镁矿制备高纯氢氧化镁的工艺研究", 《中国优秀硕士学位全文数据库 工程科技I辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109970071A (en) * | 2019-05-06 | 2019-07-05 | 辽宁科技大学 | A kind of acid system purifies the production method of low-grade talcum |
| CN111892072A (en) * | 2020-08-05 | 2020-11-06 | 辽宁辰昊镁业有限公司 | Method for preparing magnesium sulfate from magnesite tailings |
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Application publication date: 20150819 |
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