CN101993098A - Method for preparing high-purity magnesium oxide from nesquehonite by carbon-ammonia recycle method - Google Patents
Method for preparing high-purity magnesium oxide from nesquehonite by carbon-ammonia recycle method Download PDFInfo
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- CN101993098A CN101993098A CN2010105621096A CN201010562109A CN101993098A CN 101993098 A CN101993098 A CN 101993098A CN 2010105621096 A CN2010105621096 A CN 2010105621096A CN 201010562109 A CN201010562109 A CN 201010562109A CN 101993098 A CN101993098 A CN 101993098A
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Abstract
The invention discloses a method for preparing high-purity magnesium oxide from nesquehonite by a carbon-ammonia recycle method, belonging to the field of chemical production of inorganic salts. The method comprises the following steps of: with brine magnesium chloride as a raw material, preparing a nesquehonite intermediate which has good crystalline form and is easy to filter by using the carbon-ammonia recycle method; further calcining to produce high-purity magnesium oxide and simultaneously realize the recycle of carbon dioxide and ammonia, wherein the carbon dioxide is generated in the process of calcining the nesquehonite, and the ammonia is obtained by evaporating the ammonium chloride mother liquid and used for depositing magnesium. The method has the advantages of fully solving the problem of greenhouse effect and environmental pollution caused by ammonium chloride emission in the process of producing magnesium oxide and realizing high-value utilization of sea salt magnesium chloride resources. The method disclosed in the invention has high operability and is easy for industrialized production.
Description
Technical field
The invention belongs to the chemical industry of inorganic salt production field, particularly a kind of method of producing high-purity magnesium oxide by carbon ammonium circulation method through magnesium carbonate trihydrate.
Background technology
China's bittern magnesium resource is abundant, and a large amount of magnesium mainly is to be present in seawater, salt lake saline and the well halogen with muriatic form.Bittern obtains being rich in magnesium chloride brine or magnesium chloride hydrate after carrying sodium, potassium.And utilize the magnesium oxide product that this magnesium resource can the production high added value.
High-purity magnesium oxide is as a kind of important inorganic chemical product, is widely used in softening agent that top coat, rubber, paint, the stopping composition of paper production, steel ball polishing agent, the glass reinforced plastic of siliconized plate uses etc.China's high-purity magnesium oxide needs annual demand gap about 90,000 tons, account for 90% of aggregate demand, and demand will enlarge further also.
What the domestic production high-purity magnesium oxide adopted at present is the light calcined magnesia that calcined magnesite makes, and the process electric smelting is condensed or heavily fired and get high-purity magnesium oxide again.This method can only be produced the magnesium oxide of content about 95%, seldom can reach MgO content at the high-purity magnesium oxide more than 98%, even produce high-purity magnesium oxide, energy input is also very big.
Utilize the bittern magnesium chloride to produce magnesian main technological route the direct breakdown method and the precipitator method are arranged.Direct breakdown method is very high for the purity requirement of bischofite raw material, calcination process temperature height, and byproduct hydrogen chloride gas has serious corrosion to production unit.The intermediate of the precipitator method mainly is magnesium hydroxide and magnesium basic carbonate.The magnesium hydroxide intermediate is easy to reunite, and strainability is poor, and the bath water amount that needs is big.And the preparation temperature height of magnesium basic carbonate intermediate, so energy consumption height.Given this, developing a kind of is raw material with the bittern magnesium chloride, it is good and be easy to filtering intermediate to obtain crystalline form at a lower temperature, this intermediate can obtain high-purity magnesium oxide at lower temperature lower calcination, and the method that by product can recycle, not only solve the Greenhouse effect problem that environmental pollution that the ammonium chloride mother liquor discharging causes and Carbon emission cause, and realized the higher value application of magnesium resource, produced tangible economic benefit.
Summary of the invention
The purpose of this invention is to provide a kind of method of producing high-purity magnesium oxide by carbon ammonium circulation method through magnesium carbonate trihydrate, with the bittern magnesium chloride is raw material, by carbon ammonium circulation method, the preparation crystalline form is good and be easy to filtering magnesium carbonate trihydrate intermediate, produce high-purity magnesium oxide through further calcining, the ammonia recycle utilization after the carbonic acid gas that produces in the magnesium carbonate trihydrate of the realization calcining simultaneously process and the ammonium chloride mother liquor ammonia still process of heavy magnesium.
Technical scheme of the present invention is to utilize carbonic acid gas that magnesium carbonate trihydrate intermediate calcining produces and the ammonia after the ammonium chloride mother liquor ammonia still process as precipitation agent, react under lower temperature with the bittern magnesium chloride after purifying, it is good and be easy to filtering magnesium carbonate trihydrate intermediate to obtain crystalline form, obtain high-purity magnesium oxide, carbonic acid gas that calcining produces and the ammonia recycle utilization after the ammonium chloride mother liquor ammonia still process through further calcining.Ammonia, carbonic acid gas and magnesium chloride principle are as follows:
2NH
3+CO
2+H
2O＝(NH
4)
2CO
3
(NH
4)
2CO
3+MgCl
2+3H
2O＝MgCO
3·3H
2O↓+2NH
4Cl
Symbol: ↓ be that (precipitation) separated out in crystallization
The present invention utilizes ammonia after the ammonium chloride mother liquor ammonia still process that produces carbonic acid gas and heavy magnesium in the calcining magnesium carbonate trihydrate intermediate process as precipitation agent, with the bittern magnesium chloride is raw material, it is good and be easy to filtering magnesium carbonate trihydrate intermediate, the ammonia that whole technological process realizes and the recycle of carbonic acid gas to obtain crystalline form under lower temperature.Not only solve the Greenhouse effect problem that environmental pollution that the ammonium chloride mother liquor discharging causes and Carbon emission cause, and realized the higher value application of magnesium resource, produced tangible economic benefit.
The present invention is by carbon ammonium circulation method, is raw material with the bittern magnesium chloride, produces high-purity magnesium oxide through the magnesium carbonate trihydrate intermediate, and technology comprises crystallization, filtration washing, calcining, carbon dioxide recovery, the ammonium chloride mother liquor ammonia still process of magnesium carbonate trihydrate intermediate.Processing step is:
(1) preparation magnesium carbonate trihydrate intermediate
The bittern magnesium chloride is configured to the magnesium chloride solution that concentration is 0.5～4.5mol/L, adds in the reactive crystallization still, temperature is controlled at 20～40 ℃, feeds ammonia and carbonic acid gas in agitation condition downhill reaction crystallization kettle; The equivalence ratio of magnesium and ammonia is that 1: 2, ammonia flow are that 0.5～1.5 liter/minute, the flow of carbonic acid gas are 0.25～1.0 liter/minute; When density of magnesium chloride reaches 0～0.05mol/L in the solution, stop to feed in raw material, continue to stir 30～120 minutes.Solid after the filtration is the magnesium carbonate trihydrate intermediate; The filtrate that obtains after the filtration then is used as the raw material of ammonia still process; The purity of the magnesium carbonate trihydrate intermediate of producing is greater than 98.5%.
(2) magnesium carbonate trihydrate filters and washing
The magnesium carbonate trihydrate intermediate that (1) is obtained spends calcium ion water washing twice, and removing the mass ratio of calcium ion water and filter cake is 1.5: 1～3: 1, and the free water water ratio of the magnesium carbonate trihydrate that obtains after the filtration is 15%～25% (quality percentage composition).
(3) magnesium carbonate trihydrate calcining
The magnesium carbonate trihydrate that (2) are obtained places rotary calciner, and calcining temperature is 850～950 ℃, and calcining temperature is 0.5～2 hour, finally obtains high-purity magnesium oxide.The carbonic acid gas that produces in the calcination process through cooling, absorbs except that after the deammoniation, and compression is returned step (1) and is used to prepare the magnesium carbonate trihydrate intermediate, and the rate of recovery of carbonic acid gas is 70%～80%.
(4) ammonium chloride mother liquor ammonia still process
The ammonium chloride mother liquor that (1) is obtained, add milk of lime, constantly stir, then solution is sent into ammonia still, under the condition of 200-203 ℃ of heating, ammonia is steamed, the ammonia that steams is through cooling, sends into to return step (1) after ammonia absorption tower absorbs and be used to prepare the magnesium carbonate trihydrate intermediate, and the waste liquid of ammonia still process is used to regulate the sal epsom type bittern in seawater salt lake.
The present invention utilizes ammonia and carbonic acid gas as precipitation agent, is raw material with the bittern magnesium chloride, and preparation magnesium carbonate trihydrate intermediate is further calcined the production high-purity magnesium oxide, the ammonia recycle utilization after carbonic acid gas that produces in the calcination process and the ammonium chloride mother liquor ammonia still process.This processing method is good in economic efficiency, non-environmental-pollution; The method that provides is easy, and is workable, is easy to realize industrialization.
Advantage of the present invention and active effect are:
(1) utilize carbon ammonium circulation method with bittern magnesium chloride magnesium chloride, good and be easy to filtering magnesium carbonate trihydrate intermediate through crystalline form, further high-purity magnesium oxide is produced in calcining, the ammonium chloride that has solved by-product in the meticulous magnesium products production process discharges the environmental pollution that causes, and the Greenhouse effect problem that Carbon emission causes in the calcination process.Thereby solved the higher value application problem of present bittern magnesium resource, promoted industrial chain value and improved ecotope.
(2) Zhi Bei magnesium oxide purity is more than 98.5%.
(3) adopted with ammonia and carbonic acid gas as precipitation agent, preparation is good and be easy to filtering magnesium carbonate trihydrate intermediate through crystalline form under lower temperature, further the method for high-purity magnesium oxide is produced in calcining, the energy consumption of the reactive crystallization of Jie Shenging greatly, and reduced the water consumption of washing.
(4) calcium chloride solution that obtains after ammonia still process of ammonium chloride mother liquor can be used to regulate the sal epsom type bittern in seawater salt lake, and environment is not had negative impact.
Description of drawings
Fig. 1 is a process flow diagram of the present invention.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is done and to explain
Embodiment 1
The concrete technical process of present embodiment sees also Fig. 1.
(1) preparation magnesium carbonate trihydrate intermediate
The bittern magnesium chloride is configured to the magnesium chloride solution that concentration is 0.5mol/L, adds in the reactive crystallization still, temperature is controlled at 20 ℃, feeds ammonia and carbonic acid gas in agitation condition downhill reaction crystallization kettle.The equivalence ratio of magnesium and ammonia is that 1: 2, ammonia flow are that 0.5 liter/minute, the flow of carbonic acid gas are 0.25 liter/minute.When density of magnesium chloride reaches 0.01mol/L in the solution, stop to feed in raw material, continue to stir 30 minutes.Solid after the filtration is the magnesium carbonate trihydrate intermediate.The filtrate that obtains after the filtration then is used as the raw material of ammonia still process.
(2) magnesium carbonate trihydrate filters and washing
The magnesium carbonate trihydrate intermediate that (1) is obtained spends calcium ion water washing twice, and removing the mass ratio of calcium ion water and filter cake is 1.5: 1, and the free water water ratio of the magnesium carbonate trihydrate that obtains after the filtration is 25%.
(3) magnesium carbonate trihydrate calcining
The magnesium carbonate trihydrate that (2) are obtained places rotary calciner, and calcining temperature is 850 ℃, and calcining temperature is 0.5 hour, finally obtains high-purity magnesium oxide.The carbonic acid gas that produces in the calcination process through cooling, absorbs except that after the deammoniation, and compression is returned step (1) and is used to prepare the magnesium carbonate trihydrate intermediate, and the rate of recovery of carbonic acid gas is 70%.
(4) ammonium chloride mother liquor ammonia still process
The ammonium chloride mother liquor that (1) is obtained, add milk of lime, constantly stir, then solution is sent into ammonia still, under the condition of 203 ℃ of heating, ammonia is steamed, the ammonia that steams is through cooling, sends into to return step (1) after ammonia absorption tower absorbs and be used to prepare the magnesium carbonate trihydrate intermediate, and the waste liquid of ammonia still process is used to regulate the sal epsom type bittern in seawater salt lake.
The concrete technical process of present embodiment sees also Fig. 1.
(1) preparation magnesium carbonate trihydrate intermediate
The bittern magnesium chloride is configured to the magnesium chloride solution that concentration is 4.5mol/L, adds in the reactive crystallization still, temperature is controlled at 40 ℃, feeds ammonia and carbonic acid gas in agitation condition downhill reaction crystallization kettle.The equivalence ratio of magnesium and ammonia is that 1: 2, ammonia flow are that 1.5 liters/minute, the flow of carbonic acid gas are 1.0 liters/minute.When density of magnesium chloride reaches 0.05mol/L in the solution, stop to feed in raw material, continue to stir 120 minutes.Solid after the filtration is the magnesium carbonate trihydrate intermediate.The filtrate that obtains after the filtration then is used as the raw material of ammonia still process.
(2) magnesium carbonate trihydrate filters and washing
The magnesium carbonate trihydrate intermediate that (1) is obtained spends calcium ion water washing twice, and removing the mass ratio of calcium ion water and filter cake is 3: 1, and the free water water ratio of the magnesium carbonate trihydrate that obtains after the filtration is 15%.
(3) magnesium carbonate trihydrate calcining
The magnesium carbonate trihydrate that (2) are obtained places rotary calciner, and calcining temperature is 950 ℃, and calcining temperature is 2 hours, finally obtains high-purity magnesium oxide.The carbonic acid gas that produces in the calcination process through cooling, absorbs except that after the deammoniation, and compression is returned step (1) and is used to prepare the magnesium carbonate trihydrate intermediate, and the rate of recovery of carbonic acid gas is 80%.
(4) ammonium chloride mother liquor ammonia still process
The ammonium chloride mother liquor that (1) is obtained, add milk of lime, constantly stir, then solution is sent into ammonia still, under the condition of 203 ℃ of heating, ammonia is steamed, the ammonia that steams is through cooling, sends into to return step (1) after ammonia absorption tower absorbs and be used to prepare the magnesium carbonate trihydrate intermediate, and the waste liquid of ammonia still process is used to regulate the sal epsom type bittern in seawater salt lake.
Embodiment 3
The concrete technical process of present embodiment sees also Fig. 1.
(1) preparation magnesium carbonate trihydrate intermediate
The bittern magnesium chloride is configured to the magnesium chloride solution that concentration is 3mol/L, adds in the reactive crystallization still, temperature is controlled at 30 ℃, feeds ammonia and carbonic acid gas in agitation condition downhill reaction crystallization kettle.The equivalence ratio of magnesium and ammonia is that 1: 2, ammonia flow are that 1.0 liters/minute, the flow of carbonic acid gas are 0.75 liter/minute.When density of magnesium chloride reaches 0mol/L in the solution, stop to feed in raw material, continue to stir 90 minutes.Solid after the filtration is the magnesium carbonate trihydrate intermediate.The filtrate that obtains after the filtration then is used as the raw material of ammonia still process.
(2) magnesium carbonate trihydrate filters and washing
The magnesium carbonate trihydrate intermediate that (1) is obtained spends calcium ion water washing twice, and removing the mass ratio of calcium ion water and filter cake is 2: 1, and the free water water ratio of the magnesium carbonate trihydrate that obtains after the filtration is 20%.
(3) magnesium carbonate trihydrate calcining
The magnesium carbonate trihydrate that (2) are obtained places rotary calciner, and calcining temperature is 900 ℃, and calcining temperature is 1.5 hours, finally obtains high-purity magnesium oxide.The carbonic acid gas that produces in the calcination process through cooling, absorbs except that after the deammoniation, and compression is returned step (1) and is used to prepare the magnesium carbonate trihydrate intermediate, and the rate of recovery of carbonic acid gas is 75%.
(4) ammonium chloride mother liquor ammonia still process
The ammonium chloride mother liquor that (1) is obtained, add milk of lime, constantly stir, then solution is sent into ammonia still, under the condition of 203 ℃ of heating, ammonia is steamed, the ammonia that steams is through cooling, sends into to return step (1) after ammonia absorption tower absorbs and be used to prepare the magnesium carbonate trihydrate intermediate, and the waste liquid of ammonia still process is used to regulate the sal epsom type bittern in seawater salt lake.
Claims (3)
1. one kind is passed through the method that carbon ammonium circulation method is produced high-purity magnesium oxide through magnesium carbonate trihydrate, it is characterized in that processing step is:
(1) preparation magnesium carbonate trihydrate intermediate
The bittern magnesium chloride is configured to the magnesium chloride solution that concentration is 0.5～4.5mol/L, adds in the reactive crystallization still, temperature is controlled at 20～40 ℃, feeds ammonia and carbonic acid gas in agitation condition downhill reaction crystallization kettle; The equivalence ratio of magnesium and ammonia is that 1: 2, ammonia flow are that 0.5～1.5 liter/minute, the flow of carbonic acid gas are 0.25～1.0 liter/minute; When density of magnesium chloride reaches 0～0.05mol/L in the solution, stop to feed in raw material, continue to stir 30～120 minutes; Solid after the filtration is the magnesium carbonate trihydrate intermediate; The filtrate that obtains after the filtration then is used as the raw material of ammonia still process; The purity of the magnesium carbonate trihydrate intermediate of producing is greater than 98.5%;
(2) magnesium carbonate trihydrate filters and washing
The magnesium carbonate trihydrate intermediate that (1) is obtained spends calcium ion water washing twice, and removing the mass ratio of calcium ion water and filter cake is 1.5: 1～3: 1, and the free water water ratio of the magnesium carbonate trihydrate that obtains after the filtration is 15 quality %～25 quality %;
(3) magnesium carbonate trihydrate calcining and carbon dioxide recovery
The magnesium carbonate trihydrate that (2) are obtained places rotary calciner, and calcining temperature is 850-950 ℃, and calcining temperature is 0.5～2 hour, finally obtains high-purity magnesium oxide; The carbonic acid gas that produces in the calcination process through cooling, absorbs except that after the deammoniation, and compression is returned step (1) and is used to prepare the magnesium carbonate trihydrate intermediate, and the rate of recovery of carbonic acid gas is 70%～80%;
(4) ammonium chloride mother liquor ammonia still process
The ammonium chloride mother liquor that (1) is obtained, add milk of lime, constantly stir, then solution is sent into ammonia still, under the condition of 200-203 ℃ of heating, ammonia is steamed, the ammonia that steams is through cooling, sends into to return step (1) after ammonia absorption tower absorbs and be used to prepare the magnesium carbonate trihydrate intermediate, and the waste liquid of ammonia still process is used to regulate the sal epsom type bittern in seawater salt lake.
2. method according to claim 1 is characterized in that: the purity of the magnesium carbonate trihydrate intermediate of production is greater than 98.5%.
3. method according to claim 1 is characterized in that: the purity of the high-purity magnesium oxide of production is greater than 98.5%.
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Cited By (10)
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|---|---|---|---|---|
| CN102198954A (en) * | 2011-04-22 | 2011-09-28 | 辽宁中大超导材料有限公司 | Impurity control method for sintered body magnesium oxide target |
| CN102502722A (en) * | 2011-10-28 | 2012-06-20 | 中国科学院过程工程研究所 | Preparation method of high-purity magnesium oxide |
| CN102815775A (en) * | 2012-07-24 | 2012-12-12 | 浙江省天正设计工程有限公司 | Treating process and equipment for high concentration magnesium salt waste water |
| CN105540625A (en) * | 2016-01-25 | 2016-05-04 | 化工部长沙设计研究院 | Method for preparing anhydrous magnesium carbonate through magnesium-containing mother solution |
| CN105668595A (en) * | 2016-04-15 | 2016-06-15 | 国家海洋局天津海水淡化与综合利用研究所 | Method for preparing high-purity magnesium oxide from sodium carbonate industry steaming ammonia gas and salt preparing bittern |
| CN106219489A (en) * | 2016-07-15 | 2016-12-14 | 天津大学 | The processing method of produced waste water during being prepared ferrum oxide by steel mill's pickle liquor |
| CN106477602A (en) * | 2016-10-13 | 2017-03-08 | 青海百事特镁业有限公司 | A kind of preparation technology of high-purity low oxychloride magnesium |
| WO2018018137A1 (en) * | 2016-07-27 | 2018-02-01 | Institut National De La Recherche Scientifique | Production of low carbon footprint magnesia |
| CN109019644A (en) * | 2018-08-20 | 2018-12-18 | 镇江裕太防爆电加热器有限公司 | A kind of magnesium tube material production equipment for high temperature heater (HTH) |
| CN111115892A (en) * | 2018-11-01 | 2020-05-08 | 烟台安诺其精细化工有限公司 | Method for treating diallyl product production wastewater |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102198954A (en) * | 2011-04-22 | 2011-09-28 | 辽宁中大超导材料有限公司 | Impurity control method for sintered body magnesium oxide target |
| CN102502722A (en) * | 2011-10-28 | 2012-06-20 | 中国科学院过程工程研究所 | Preparation method of high-purity magnesium oxide |
| CN102815775A (en) * | 2012-07-24 | 2012-12-12 | 浙江省天正设计工程有限公司 | Treating process and equipment for high concentration magnesium salt waste water |
| CN105540625A (en) * | 2016-01-25 | 2016-05-04 | 化工部长沙设计研究院 | Method for preparing anhydrous magnesium carbonate through magnesium-containing mother solution |
| CN105540625B (en) * | 2016-01-25 | 2017-04-26 | 化工部长沙设计研究院 | Method for preparing anhydrous magnesium carbonate through magnesium-containing mother solution |
| CN105668595A (en) * | 2016-04-15 | 2016-06-15 | 国家海洋局天津海水淡化与综合利用研究所 | Method for preparing high-purity magnesium oxide from sodium carbonate industry steaming ammonia gas and salt preparing bittern |
| CN106219489A (en) * | 2016-07-15 | 2016-12-14 | 天津大学 | The processing method of produced waste water during being prepared ferrum oxide by steel mill's pickle liquor |
| WO2018018137A1 (en) * | 2016-07-27 | 2018-02-01 | Institut National De La Recherche Scientifique | Production of low carbon footprint magnesia |
| US11401168B2 (en) | 2016-07-27 | 2022-08-02 | Institut National De La Recherche Scientifique | Production of low carbon footprint magnesia |
| CN106477602A (en) * | 2016-10-13 | 2017-03-08 | 青海百事特镁业有限公司 | A kind of preparation technology of high-purity low oxychloride magnesium |
| CN109019644A (en) * | 2018-08-20 | 2018-12-18 | 镇江裕太防爆电加热器有限公司 | A kind of magnesium tube material production equipment for high temperature heater (HTH) |
| CN111115892A (en) * | 2018-11-01 | 2020-05-08 | 烟台安诺其精细化工有限公司 | Method for treating diallyl product production wastewater |
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Application publication date: 20110330 |