CN1033975A - Process for preparation of light magnesia by leaching magnesite with ammonium salts - Google Patents
Process for preparation of light magnesia by leaching magnesite with ammonium salts Download PDFInfo
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- CN1033975A CN1033975A CN 88100206 CN88100206A CN1033975A CN 1033975 A CN1033975 A CN 1033975A CN 88100206 CN88100206 CN 88100206 CN 88100206 A CN88100206 A CN 88100206A CN 1033975 A CN1033975 A CN 1033975A
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- magnesium
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- magnesia
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Abstract
The present invention is, and to be raw material with the magnesia leach wherein magnesium oxide with ammonium salt aqueous solution, makes it change into the solubility magnesium salts and enter solution, realizes and separate impurities.There is ammonia to emit during the leaching reaction, after water absorbs, standby.In magnesium salt solution, add sal volatile and generate the magnesiumcarbonate precipitation, and mother liquor is ammonium salt solution just, therefore can return the leaching magnesia.Obtain light magnesium oxide and emit carbonic acid gas after the magnesiumcarbonate calcining, it is fed in the aforesaid standby ammoniacal liquor obtain, thereby realized the recycled of raw material as the precipitation agent sal volatile.
Description
The invention belongs in the inorganic chemical industry with the magnesia is the method for raw material production light magnesium oxide.
One of conventional production methods of light magnesium oxide is to decompose the magnesium basic carbonate that magnesium salts makes by soda ash, makes (" inorganic chemicals industry handbook, the first volume, 790 pages, volumes such as Tianjin chemical research institute, Chemical Industry Press, 1979, Beijing) through high-temperature calcination.Because soda ash is in short supply, price rises, and this method is subjected to certain limitation aborning.Abroad, have the reaction of ammonia and sal epsom to make the patent (SU906142(640615) of chemical fertilizer with ammonium sulfate magnesium double salt) report.The method that present domestic replacement soda ash is made raw material has bittern ammonium carbonate method (" inorganic chemicals industry ", the fourth phase in 1987) and magnesite ammonium carbonate method (" inorganic chemicals industry ", the fifth phase in 1985).This all is a method preferably, but that its weak point is a prepared using is abundant inadequately.With the magnesite ammonium carbonate method is example, and this method is to react with the vitriol oil and magnesite earlier, makes Adlerika, makes precipitation agent with volatile salt and adds in the solution, is settled out magnesiumcarbonate, again its calcining is obtained the light magnesium oxide finished product.This method only is about 60% in the raw material overall utilization of magnesium, and subsidiary material consume higher, account for 84% of raw and auxiliary material total expenses.The by product ammonium sulfate or the ammonium chloride of above-mentioned two kinds of methods can't fully reclaim, and higher because of reclaiming energy consumption, industrialization has little significance.
Purpose of the present invention just for provide a kind of without soda ash is provided, without sulfuric acid, nitric acid or hydrochloric acid, and can make full use of the method that starting material are produced light magnesium oxide.This method production cost is low, has realized nothing " three wastes " discharging basically.
The first step of the inventive method is the preparation magnesium salt solution.Key problem in technology is to prepare magnesium salt solution without the vitriol oil, hydrochloric acid or nitric acid, but replaces the vitriol oil, hydrochloric acid or nitric acid to prepare magnesium salt solution with the aqueous solution of ammonium chloride, ammonium sulfate, ammonium nitrate or their mixture.We call the ammonium salt decomposition agent to ammonium chloride, ammonium sulfate, ammonium nitrate or their mixture.With magnesia is raw material, and magnesia makes with magnesite light-burned (roasting below 1000 ℃), its major ingredient be magnesium oxide (MgO) content more than 80%, also have calcium oxide (CaO), aluminium sesquioxide (Al
2O
3), ferric oxide (Fe
2O
3) and silicon-dioxide (SiO
2) wait impurity.Leaching is reflected under the normal pressure, carries out in the Steel Vessel that a band stirs.Earlier with 100 purpose magnesias, add in the carbonating mother liquor that produces when the present invention second goes on foot the magnesium salt solution carbonation reaction, size mixing and add a part of ammonium salt decomposition agent 90～95 ℃ of reacting by heating one hour, add the ammonium salt decomposition agent again, continue reaction leaching one hour, after measured, at this moment the rate of decomposition of magnesia reaches more than 95%.Magnesium oxide in the leaching reaction in the magnesia is converted into magnesium chloride, sal epsom or magnesium nitrate and enters in the leaching liquid, the ammonia water that generates in the reaction absorbs, the carbon dioxide reaction that produces during with the present invention's the 3rd step calcining magnesiumcarbonate generates sal volatile, makes the precipitation agent of magnesium salt solution for the present invention second step and uses.Because leaching liquid is subacidity, so silicon-dioxide exists with solid phase in leaching process all the time, do not enter magnesium salt solution.Calcium also enters magnesium salt solution hardly.Aluminium sesquioxide and ferric oxide are mainly with ironic hydroxide (Fe(OH)
3) and aluminium hydroxide (Al(OH)
3) form exist, reaction is during near terminal point, magnesium salt solution is near neutral (about PH=6.5), only need standing sedimentation this moment after, filtering separation just can be removed impurity.The analysis revealed magnesium salt solution need not to do the preparation that special processing just can be used for light magnesium oxide.And entered magnesium salt solution with magnesite ammonium carbonate method impurity such as iron, aluminium, manganese when adding sulfuric acid reaction, therefore solution also will could prepare light magnesium oxide through impurity removal process, so not adding sulfuric acid, hydrochloric acid or nitric acid has not only guaranteed quality product, has simplified technology, has shortened Production Flow Chart, saved starting material, and solved sulfuric acid, hydrochloric acid or nitric acid equipment and Corrosion of Pipeline problem.Its major ingredient of filter residue that the leaching back is left can not produce environment and pollute as above-mentioned, therefore can concentrate the stacking processing.
Second step of the inventive method is the preparation of Magnesium Carbonate Light 41-45.Be mixed with sal volatile and the first step with carbonated aqueous ammonia or ammoniacal liquor with an amount of bicarbonate of ammonia and reclaim the sal volatile that obtains and add in the magnesium salt solution that the first step makes as precipitation agent and carry out carbonation reaction, generate the basic carbonate magnesium precipitate.Centrifugal or suction filtration separates.Isolating mother liquor mainly contains ammonium chloride, ammonium sulfate or ammonium nitrate, and this is required ammonium salt decomposition agent in the first step leaching reaction just, so reusable edible.The magnesium basic carbonate that precipitin reaction generates promptly obtains Magnesium Carbonate Light 41-45 with hot wash, oven dry.Contain a certain amount of ammonium chloride, ammonium sulfate or ammonium nitrate in the initial wash water, return the first step as the magnesia usefulness of sizing mixing.
The 3rd step of the inventive method is the preparation of light magnesium oxide.To send into calcining furnace after the Magnesium Carbonate Light 41-45 drying and crushing in calcining below 1000 ℃.Magnesium Carbonate Light 41-45 decomposes generation carbonic acid gas and finished light magnesium oxide.Leach the ammoniacal liquor reaction of reclaiming when reacting with the first step after the carbon dioxide recovery, obtain sal volatile, as the precipitation agent of the second step carbonation reaction." waste water " that produces in the production process like this, " waste gas " all carried out the boundless and indistinct of circulation cover lame pour throw hide the that coughs herd dislike the capable y offspring of clock happy buy the clear Yin of the fat of neighing to the greatest extent S the region between the heart and the diaphragm pay study carefully a kind of bamboo alkali Х ū and allow the very small of mirror mire sleep to look 0% and bring up to 80%, the raw and auxiliary material total expenses has reduced about 1/3.
The present invention applies mechanically after 8 times in Recycling Mother Solution, and the every by analysis index of the light magnesium oxide of producing is as follows: content of magnesia is 94.49%; Calcining weightless 1.65%; Calcium oxide 0.91%; Hydrochloric acid insoluble substance 0.059%; Look 12 milliliters of specific volumes/gram; Every indexs such as vitriol, muriate, iron, manganese, screenings all reach industrial first grade quality standard among the chemical industry ministerial standard HGI-324-77.
All main raw material(s)s of the present invention and power charge are by the existing market calculation of price, and the factory cost of light magnesium oxide per ton is about 2050 yuan.
Method of the present invention both can be produced light magnesium oxide, can produce Magnesium Carbonate Light 41-45 again.
One of embodiments of the invention:
With fineness is 100 purpose magnesias, 20.0 grams, in the mother liquor that reclaims when adding 30 times of magnesium salts carbonation reactions to inventory, furnishing slurry in the sealing Steel Vessel that band stirs, 85～95 ℃ of thermal degradation reactions 1 hour, and then add ammonium salt decomposition agent 8 gram (ammonium chloride: ammonium sulfate: ammonium nitrate is 30: 2: 2), re-leaching is 1 hour under the temperature of about 95 ℃ of maintenances, until till verifying decomposition fully, cooling, sedimentation, filter, filter residue is concentrated to stack and is handled, promptly obtain comparatively purified magnesium salt solution 350ml, being converted to content of magnesia is every liter 45 gram, and the pH value of solution is about 6.5.Have partly ammonia overflow from magnesium salt solution in the reaction, water absorbs, and the carbonic acid gas effect that produces during with calcining magnesiumcarbonate generates sal volatile, uses as the precipitation agent of magnesium salt solution.In the 350ml magnesium salt solution that obtains, add the 350ml precipitation agent; For the ease of stirring, be converted to magnesian concentration in the reaction system and should be controlled at 10～30 grams per liters; The reaction end temperature is controlled at about 65 ℃, and the reaction times is 30 minutes.In the time of need replenishing as precipitation agent, be equipped with an amount of bicarbonate of ammonia, make sal volatile and make precipitation agent with carbonated aqueous ammonia or ammoniacal liquor.In the precipitation agent consumption of volatile salt with magnesium salt solution in the ratio of mole number of magnesium salts be 1.0～1.1 to be advisable.With about 60 ℃ hot wash basic carbonate magnesium precipitate, up to chlorion and sulfate radical (SO
2- 4) ionic content less than controlling index till.The washing water in early stage can return and be used for magnesia and size mixing.Wet magnesiumcarbonate 196 grams are sent into oven dry is crushed to below 100 orders with Universalpulverizer to moisture less than below 2% in the drying room, send into the calcining furnace decomposing and calcining, calcining temperature is 900 ℃, 2 hours time, obtains light magnesium oxide finished product 13.5 grams at last.The carbonic acid gas that calcining and decomposing produces obtains volatile salt with leaching the ammoniacal liquor reaction that generates when reacting after cooling off, make the precipitation agent of magnesium salt solution carbonation reaction and use.
Claims (6)
1, a kind of is the method for raw material production light magnesium oxide with the magnesia, it is characterized in that making wherein magnesium oxide change the solubility magnesium salts into ammonium salt decomposition agent leaching magnesia enters the aqueous solution and separate with other impurity.The soluble magnesium salts solution adds precipitation agent and carries out carbonation reaction, generates magnesiumcarbonate, after filtering, wash, dry, pulverizing its calcining is obtained light magnesium oxide.
2, the method for claim 1, it is characterized in that the ammonium salt decomposition agent is the aqueous solution by ammonium chloride, ammonium sulfate, ammonium nitrate or their mixture, and magnesium salt solution carries out the mother liquor that obtains behind the carbonation reaction, just ammonium salt decomposition agent, therefore the leaching magnesia of applying mechanically capable of circulation.
3, the method for claim 1 is characterized in that the aqueous solution of the precipitation agent volatile salt of magnesium salt solution, and its typical concentrations is 0.25～5 mole.During with ammonium salt decomposition agent aqueous solution leaching magnesia, have ammonia to produce, water absorbs the back and generates ammoniacal liquor, and calcining has during magnesiumcarbonate carbon dioxide to produce, obtain the aqueous solution of volatile salt behind the feeding ammoniacal liquor, this is the precipitation agent of magnesium salt solution just, therefore also capable of circulation applying mechanically.Also can control ammonia (NH with carbonated aqueous ammonia or ammoniacal liquor and bicarbonate of ammonia reaction
3) excessive 0～10% prepare precipitation agent.
4, the method for claim 1 is characterized in that leaching temperature at 80～100 ℃, should remain on when magnesium salt concentrations is converted to magnesium oxide in the leaching liquid between 20～100 grams per liters, and the ammonium salt leaching agent can add step by step during leaching.
5, the method for claim 1, the temperature that it is characterized in that the magnesium salt solution carbonation reaction in precipitation agent consumption and the magnesium salt solution are converted to magnesium salts the ratio of magnesian mole number between 1: 1～1.1: 1 in 40～70 ℃.
6, the method for claim 1 is characterized in that the magnesiumcarbonate precipitate and separate, and washing back is 140 ℃ ± 10 ℃ oven dry down, can obtain Magnesium Carbonate Light 41-45 after being crushed to 100 orders.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88100206 CN1033975A (en) | 1988-01-06 | 1988-01-06 | Process for preparation of light magnesia by leaching magnesite with ammonium salts |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 88100206 CN1033975A (en) | 1988-01-06 | 1988-01-06 | Process for preparation of light magnesia by leaching magnesite with ammonium salts |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1033975A true CN1033975A (en) | 1989-07-19 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 88100206 Pending CN1033975A (en) | 1988-01-06 | 1988-01-06 | Process for preparation of light magnesia by leaching magnesite with ammonium salts |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102392143A (en) * | 2011-10-28 | 2012-03-28 | 东北大学 | Recycling method of magnesium in silicate nickel oxide ore |
| CN102627302A (en) * | 2011-11-29 | 2012-08-08 | 中国矿业大学(北京) | Serpentine processing and utilization method |
| CN102745724A (en) * | 2012-06-26 | 2012-10-24 | 沈阳化工大学 | Method for producing high-purity magnesium oxide by using light calcined powder as raw material |
| CN103011630A (en) * | 2012-12-26 | 2013-04-03 | 新疆蓝天镁业股份有限公司 | Method of producing high-purity magnesium hydroxide and magnesium oxide by low-grade magnesite |
| CN105347703A (en) * | 2015-12-03 | 2016-02-24 | 龙岩紫云化学科技有限公司 | Calcium magnesium carbonate salt mine decomposition method |
-
1988
- 1988-01-06 CN CN 88100206 patent/CN1033975A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102392143A (en) * | 2011-10-28 | 2012-03-28 | 东北大学 | Recycling method of magnesium in silicate nickel oxide ore |
| CN102392143B (en) * | 2011-10-28 | 2013-08-21 | 东北大学 | Recycling method of magnesium in silicate nickel oxide ore |
| CN102627302A (en) * | 2011-11-29 | 2012-08-08 | 中国矿业大学(北京) | Serpentine processing and utilization method |
| CN102745724A (en) * | 2012-06-26 | 2012-10-24 | 沈阳化工大学 | Method for producing high-purity magnesium oxide by using light calcined powder as raw material |
| CN103011630A (en) * | 2012-12-26 | 2013-04-03 | 新疆蓝天镁业股份有限公司 | Method of producing high-purity magnesium hydroxide and magnesium oxide by low-grade magnesite |
| CN103011630B (en) * | 2012-12-26 | 2015-09-09 | 新疆蓝天镁业股份有限公司 | Low-grade magnesite produces high purity magnesium hydroxide and method of magnesium oxide |
| CN105347703A (en) * | 2015-12-03 | 2016-02-24 | 龙岩紫云化学科技有限公司 | Calcium magnesium carbonate salt mine decomposition method |
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