CN101214980A - Method for producing large particles of heptahydrate magnesium sulfate and monohydrate magnesium sulfate from magnesium sulfate solution - Google Patents
Method for producing large particles of heptahydrate magnesium sulfate and monohydrate magnesium sulfate from magnesium sulfate solution Download PDFInfo
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- CN101214980A CN101214980A CNA2007101593324A CN200710159332A CN101214980A CN 101214980 A CN101214980 A CN 101214980A CN A2007101593324 A CNA2007101593324 A CN A2007101593324A CN 200710159332 A CN200710159332 A CN 200710159332A CN 101214980 A CN101214980 A CN 101214980A
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- magnesium sulfate
- magnesium
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- adlerika
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Abstract
The invention discloses a method for producing magnesium sulfate, which is a method for producing macroaggregated magnesium sulfate heptahydrate and magnesium sulfate mono-hydrate from magnesium sulfate solution, in particular to a method for producing macroaggregated magnesium sulfate heptahydrate and magnesium sulfate mono-hydrate by employing solid containing magnesium sulfite (the chemical name is MgSO3) to obtain solution containing magnesium sulfate after oxidation treatment. The method of the invention comprises high temperature oxidizing magnesium sulfite, adding acid to adjust pH value, filtering solution, negative pressure evaporating and high temperature heating or seeding cooling for producing magnesium sulfate heptahydrate. The invention is simple in method and easy in operation. The product of magnesium sulfate produced by the method is high in product quality, and the selling price is increased. The method sufficiently employs byproduct of desulphurization process with magnesium as raw material, thereby decreasing the investment of environmental equipment in the desulphurization process with magnesium and operation cost, also decreasing the production cost of magnesium sulfate industry and achieving the win-win purpose of social benefit and economic benefit. The problems that in the existing method the product quality is low and macroaggregated magnesium sulfate heptahydrate can not be produced are resolved.
Description
Technical field
What the present invention announced is the production method of sal epsom, specifically is meant to utilize to contain magnesium sulfite solid (chemical name MgSO
3) carry out the sulfur acid magnesium solution that obtains after the oxide treatment, and the method for producing macrobead magnesium sulfate heptahydrate and magnesium sulfate monohydrate.
Background technology
Existing industrial enterprise administers flue dust and adopts the magnesium oxide method flue gas desulfurization technique mostly, and the byproduct that produces after the desulfurization is the solid magnesium sulfite.But the running cost of this sulfur removal technology is very high.Enterprise all adopts with this co-production sal epsom by way of compensation for reducing the cost of environmental protection operation.And traditional sal epsom production method is after this solid magnesium sulfite is carried out oxide treatment, has just obtained Adlerika.And then with this solution simply cool off, crystallization, separation promptly obtained low-grade magnesium sulfate heptahydrate because the Application Areas of this low-grade sal epsom is narrow, market is low always, so can't form benefit all the time.This has also blocked the utilization and extention of magnesium oxide method flue gas desulfurization technique simultaneously.And the magnesium oxide method flue gas desulfurization technique, successful abroad utilization is for many years.So, the key of present domestic use magnesium oxide method flue gas desulfurization is the problem that solves running cost, and the key that addresses this problem is made higher-grade macrobead magnesium sulfate heptahydrate and the magnesium sulfate monohydrate that satisfies market demand with the byproduct-magnesium sulfite essence that produces in the magnesium oxide method flue gas desulfurization technique exactly.In addition because the existing sal epsom of producing all is the fine particle product, absorption moisture and problem such as occur hardening is very inconvenient when the user uses easily in storage and transportation.Therefore say that existing treatment process to magnesium sulfite exists a lot of not enough.
Summary of the invention
For addressing the above problem.The purpose of this invention is to provide a kind ofly with the byproduct magnesium sulfite that produces in the magnesium oxide method flue gas desulfurization technique, essence is made the macrobead magnesium sulfate heptahydrate that satisfies market demand and the method for high-quality magnesium sulfate monohydrate.To solve the problem that quality product that existing method exists is low and can not produce the macrobead product.
The present invention seeks to be achieved by following technical solution.Its production process comprises the high temperature oxidation magnesium sulfite, adds acid accent pH value, solution filtration, negative pressure evaporation, high-temperature high-pressure heat or add the crystal seed cooling and produce the macrobead magnesium sulfate heptahydrate.
1, high temperature oxidation magnesium sulfite
At first the magnesium sulfite solid that contains that obtains in the magnesium oxide method flue gas desulfurization technique is rendered in the sal epsom circulating mother liquor, by the sal epsom circulating mother liquor it is dispersed into paste liquid, sal epsom circulating mother liquor and magnesium sulfite solid input ratio are; 100: 10～25, carry out secondary oxidation with being pumped into aeration tank again after waiting to disperse, its reaction equation is: MgSO
3+
1/
2O
2=MgSO
4Oxidation uses compressed-air actuated temperature to be 100-150 ℃ of warm air;
2, add sulfuric acid and transfer pH value
Owing to contain the part magnesium hydroxide in the magnesium sulfite, therefore the Adlerika that obtains after the oxidation need be carried out pH value and regulates, add sulfuric acid while moving, reach 6-7 until pH value.
3, solution filters
Adlerika after pH value regulated removes by filter the impurity in the solution.Make the saturated Adlerika of high temperature.
4, negative pressure evaporation
The high temperature saturated solution of magnesium sulfate is pumped into vacuum evaporator, carry out negative pressure evaporation.Remove redundant moisture, just obtained the sal epsom supersaturated solution.Negative pressure evaporation pressure is:
400mmHg-600mmHg; The evaporation termination boiling point is 85～95 ℃.
5, high-temperature high-pressure heat
According to the character of magnesium sulfate solution, if the sal epsom supersaturated solution is carried out high-temperature high-pressure heat again, a large amount of crystalline that will obtain magnesium sulfate monohydrate are separated out.The temperature of heating is 105～115 ℃.Feed pressure is 0.3～0.4mpa.Then the sulfuric acid monohydrate magnesium crystal of separating out is separated and promptly obtain high-quality magnesium sulfate monohydrate.
6, add crystal seed
According to the character of magnesium sulfate solution, the sal epsom supersaturated solution is added sal epsom crystal seed, the macrobead crystal that cools and just obtained magnesium sulfate heptahydrate.Specific practice is: the high temperature supersaturation Adlerika of method for preparing is pumped in the crystallizer, cool off earlier, stir, when feed temperature is reduced to 65～75 ℃, short grained sal epsom finished product is joined in the feed liquid.The add-on of short grained sal epsom finished product adds by every cubic metre of solution 10～20Kg.And then carry out cooling and stirring, the time of stirring is 4～6 hours.Stirring velocity is 30～40r/min.When liquid material temperature reaches 35～40 ℃, stop to stir and cooling.Then feed liquid is put into centrifugal separation equipment, carry out drying treatment again.Promptly make the macrobead magnesium sulfate crystals.The inventive method is simple, and is easy to implement.By the sal epsom quality product height that present method is made, foreign matter content is low, has improved selling price.Present method made full use of magnesium method sulfur removal technology byproduct---magnesium sulfite is done raw material, thereby the environmental protection equipment investment and the running cost of magnesium method sulfur removal technology have been reduced, and make environmental protection project can really form considerable economic, promptly reduced environmental protection running cost, reduce the production cost of sal epsom industry again, reached social benefit and economic benefit doulbe-sides' victory purpose.It is a kind of ideal sal epsom production method.
Description of drawings
Accompanying drawing is process flow sheet of the present invention (the attached apparatus and process schema that contains)
Embodiment
The production method of magnesium sulfate monohydrate
Get sal epsom circulating mother liquor 1000Kg, magnesium sulfite solid material 200Kg.Above two kinds of materials are rendered in the mixed reaction pond, disperseed and oxide treatment.Dispersion and oxidation adopt heat of compression air to carry out.Air themperature is 140 ℃, and the feed temperature in the aeration tank is 110 ℃.Then feed liquid is pumped into to regulate and carry out potential of hydrogen in the still and regulate, the mode of adjusting adopts and adds the vitriolic method and carry out, and stops to add acid when the pH value of feed liquid reaches 6.Be neutral solution with this pH value then, pump into and carry out the press filtration processing in the filter press device, thereby promptly obtain the saturated Adlerika of high temperature.Then the saturated Adlerika of this high temperature is pumped in the vacuum evaporator.Carry out negative pressure evaporation.Negative pressure still internal pressure is 550mmHg.The evaporation final temperature is 90 ℃.Thereby obtain the supersaturation Adlerika.This supersaturation Adlerika sent into carry out autoclaving in the autoclave, while stirring heating.When feed temperature is 110 ℃.The pressure of feed liquid stops heating during for 0.3mpa.The pulpous state crystal of magnesium sulfate monohydrate will be obtained.Carry out press filtration more at last, thereby drying makes high-quality sulfuric acid monohydrate magnesium products.
The production method of magnesium sulfate heptahydrate
Be that supersaturation Adlerika with above production sulfuric acid monohydrate magnesium method gained pumps in the crystallization kettle, begin simultaneously to stir, thereby make liquid cooling cooling.Treat to add crystal seed when temperature is reduced to 70 ℃, promptly add the small-particle magnesium sulfate crystals.The add-on of crystal seed is to add 20Kg in the supersaturated solution per ton.Continue cooling after adding crystal seed, be 5 hours cooling time.The speed that stirs in process of cooling is 35r/min.Cooled feed temperature is 40 ℃.Promptly obtain the magnesium sulfate heptahydrate slurry.After again the magnesium sulfate heptahydrate slip that obtains being carried out centrifugation, drying.Just obtained macrobead magnesium sulfate heptahydrate product.
Claims (4)
1. produce the method for macrobead magnesium sulfate heptahydrate with Adlerika, it is characterized in that its operation is the high temperature oxidation magnesium sulfite, add acid accent pH value, solution filtration, negative pressure evaporation and add the crystal seed cooling.
2. method according to claim 1, it is characterized in that sal epsom circulating mother liquor and magnesium sulfite solid input ratio are: 100: 10～25, carry out secondary oxidation with being pumped into aeration tank again after waiting to disperse, oxidation uses compressed-air actuated temperature to be 100-150 ℃ of warm air, with the Adlerika that obtains after the oxidation, carrying out pH value regulates, add sulfuric acid while moving, reach 6-7 until pH value, Adlerika after pH value regulated removes by filter the impurity in the solution, make the saturated Adlerika of high temperature, the high temperature saturated solution of magnesium sulfate is pumped into vacuum evaporator, carry out negative pressure evaporation, obtain the sal epsom supersaturated solution, negative pressure evaporation pressure is: 400mmHg-600mmHg; The evaporation termination boiling point is 85～95 ℃, supersaturated solution behind the negative pressure evaporation is pumped in the crystallization kettle, begin simultaneously to stir, thereby make liquid cooling cooling, treat to add when temperature reaches 70 ℃ crystal seed, it is the small-particle magnesium sulfate crystals, the add-on of crystal seed is to add 20Kg in the supersaturated solution per ton, continue cooling after adding crystal seed, be 5 hours cooling time, the speed that stirs in process of cooling is 35r/min, and cooled feed temperature is 40 ℃, and the magnesium sulfate heptahydrate slip that obtains is carried out centrifugation, drying.
3. produce the method for magnesium sulfate monohydrate with Adlerika, it is characterized in that its operation is the high temperature oxidation magnesium sulfite, add acid accent pH value, solution filtration, negative pressure evaporation and high-temperature high-pressure heat.
4. method according to claim 3, it is characterized in that sal epsom circulating mother liquor and magnesium sulfite solid input ratio are: 100: 10～25, carry out secondary oxidation with being pumped into aeration tank again after waiting to disperse, oxidation uses compressed-air actuated temperature to be 100-150 ℃ of warm air, with the Adlerika that obtains after the oxidation, carrying out pH value regulates, add sulfuric acid while moving, reach 6-7 until pH value, Adlerika after pH value regulated removes by filter the impurity in the solution, make the saturated Adlerika of high temperature, the high temperature saturated solution of magnesium sulfate is pumped into vacuum evaporator, carry out negative pressure evaporation, obtain the sal epsom supersaturated solution, negative pressure evaporation pressure is: 400mmHg-600mmHg; The evaporation termination boiling point is 85～95 ℃, the sal epsom supersaturated solution is carried out high-temperature high-pressure heat again, and a large amount of crystalline that obtain magnesium sulfate monohydrate are separated out, and the temperature of heating is 105～115 ℃, feed pressure is 0.3～0.4mpa, then the sulfuric acid monohydrate magnesium crystal of separating out is separated.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101593324A CN101214980A (en) | 2007-12-29 | 2007-12-29 | Method for producing large particles of heptahydrate magnesium sulfate and monohydrate magnesium sulfate from magnesium sulfate solution |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101593324A CN101214980A (en) | 2007-12-29 | 2007-12-29 | Method for producing large particles of heptahydrate magnesium sulfate and monohydrate magnesium sulfate from magnesium sulfate solution |
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| CN101214980A true CN101214980A (en) | 2008-07-09 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014075232A1 (en) * | 2012-11-14 | 2014-05-22 | 中节能六合天融环保科技有限公司 | Method for producing magnesium sulfate heptahydrate and magnesium sulfate monohydrate using magnesium-method desulphurization slurry |
| CN110451548A (en) * | 2019-09-23 | 2019-11-15 | 山西北化关铝化工有限公司 | Spherical narrow granularity barium nitrate of one kind and preparation method thereof |
| CN110759366A (en) * | 2019-10-29 | 2020-02-07 | 莱州龙鹏化工有限公司 | Preparation method of magnesium sulfate |
| CN110790290A (en) * | 2019-12-18 | 2020-02-14 | 河南省睿博环境工程技术有限公司 | Method for producing high-purity magnesium sulfate from magnesium-method desulfurization waste residues |
| CN115159579A (en) * | 2022-08-01 | 2022-10-11 | 贵州金瑞新材料有限责任公司 | Method for deeply separating calcium and magnesium impurities in manganese sulfate |
-
2007
- 2007-12-29 CN CNA2007101593324A patent/CN101214980A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2014075232A1 (en) * | 2012-11-14 | 2014-05-22 | 中节能六合天融环保科技有限公司 | Method for producing magnesium sulfate heptahydrate and magnesium sulfate monohydrate using magnesium-method desulphurization slurry |
| CN110451548A (en) * | 2019-09-23 | 2019-11-15 | 山西北化关铝化工有限公司 | Spherical narrow granularity barium nitrate of one kind and preparation method thereof |
| CN110759366A (en) * | 2019-10-29 | 2020-02-07 | 莱州龙鹏化工有限公司 | Preparation method of magnesium sulfate |
| CN110790290A (en) * | 2019-12-18 | 2020-02-14 | 河南省睿博环境工程技术有限公司 | Method for producing high-purity magnesium sulfate from magnesium-method desulfurization waste residues |
| CN115159579A (en) * | 2022-08-01 | 2022-10-11 | 贵州金瑞新材料有限责任公司 | Method for deeply separating calcium and magnesium impurities in manganese sulfate |
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Open date: 20080709 |