CN86102539A - The no waste liquid manufacture method of Magnesium Carbonate Light 41-45 - Google Patents

The no waste liquid manufacture method of Magnesium Carbonate Light 41-45 Download PDF

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Publication number
CN86102539A
CN86102539A CN 86102539 CN86102539A CN86102539A CN 86102539 A CN86102539 A CN 86102539A CN 86102539 CN86102539 CN 86102539 CN 86102539 A CN86102539 A CN 86102539A CN 86102539 A CN86102539 A CN 86102539A
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China
Prior art keywords
reaction
magnesium
magnesiumcarbonate
ammonium
salt solution
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CN 86102539
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Chinese (zh)
Inventor
王关清
周友声
史祖余
王健生
刘艳芬
朱雅敏
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DUNHUANG CHENICAL PLANT SHANGHAI
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DUNHUANG CHENICAL PLANT SHANGHAI
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Publication of CN86102539A publication Critical patent/CN86102539A/en
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Abstract

The invention provides a kind of no waste liquid manufacture method that can be used as the Magnesium Carbonate Light 41-45 of light magnesium oxide raw material.The characteristics of this method are to produce magnesium salt solution with ammonium salt solution decomposition magnesia or magnesite breeze, then with itself and bicarbonate of ammonia with reclaim the ammoniacal liquor reaction and produce magnesiumcarbonate, ammonium salt-containing mother liquor behind byproduct of reaction ammoniacal liquor and the separation magnesiumcarbonate all recycles, so no discharging of waste liquid.

Description

The no waste liquid manufacture method of Magnesium Carbonate Light 41-45
The present invention is a kind of method from magnesium-containing mineral manufacturing magnesiumcarbonate, particularly relates to ammonium salt solution and decomposes the Technology that magnesium-containing mineral is made magnesiumcarbonate.
The method that domestic present carbon ammonia method is produced magnesiumcarbonate, system's ammonium carbonate solution, bicarbonate of ammonia or bicarbonate of ammonia add ammoniacal liquor and get with containing magnesium solution (being generally bittern) reaction, can make in this way and look the big Magnesium Carbonate Light 41-45 of specific volume, but reaction by product ammonium salt solution recovery value is little, discharges then seriously polluted.(inorganic chemicals industry, 1982, № 6, P1)
The objective of the invention is to be to seek a kind of quality product and not only meet China's Magnesium Carbonate Light 41-45 standard (GB1612-79) but also can be used as the raw material of producing light magnesium oxide (HG1-324-77), do not produce the new production method of waste liquid again.
The present invention implements by following method is concrete, and accompanying drawing is seen in technical process.
1. leaching
With ammonium sulfate, ammonium nitrate or ammonium chloride salt solution and magnesia or magnesite breeze etc. contain the magnesium mineral aggregate, in reactor 1, mix, heating, temperature of reaction is controlled near the solution boiling point, after the reaction feed liquid is filtered, filtrate is magnesium salt solution, filtrate is delivered to reactor 2, the ammonia water of emitting in the reaction absorbs to form and reclaims ammoniacal liquor, these reclaim, and ammoniacal liquor is a part of uses acid to neutralize, and generates ammonium salt solution and returns the additional leaching of do reagent usefulness, and another part is delivered to reactor 2(referring to schema) the participation reaction.
When being raw material with ammonium sulfate and magnesia, its reaction equation is:
During reaction, the content of impurity mn ion is relevant in the ratio of ammonium salt and magnesia and magnesia transformation efficiency and the final leaching liquid, this value is big more, the magnesia transformation efficiency rises, but mn ion content increases in the leaching liquid, when magnesium oxide ratio was 1: 0.85～1.12 in ammonium salt and the magnesia raw material, the mn ion foreign matter content can meet the requirement of the standard HG1-324-77 of the Ministry of Chemical Industry light magnesium oxide raw material in the product magnesiumcarbonate.
2. reaction
Delivering to the above-mentioned filtrate of reactor 2 and the carbonate reaction of ammonium, in present method, is with bicarbonate of ammonia and recovery ammoniacal liquor, NH 4OH/NH 4HCO 3Mole ratio be 0～1.75: 1, when making leaching agent with ammonium sulfate, this reaction formula is
Mg ++Concentration is at 0.41～0.83mol/dm 3Between, NH 4HCO 3/ Mg ++Be 1～1.2: 1, temperature of reaction is controlled at 40-90 ℃.Gained precipitation is through washing, centrifugation, the drying and crushing lightweight magnesium basic carbonate that gets product.This magnesium basic carbonate is pulverized and is promptly got light magnesium oxide through roasting.
Compare with the carbon ammonia method that China adopts at present, because existing carbon ammonia method adopts the carbonate reaction of magnesium salt solution and ammonium, one ton of magnesiumcarbonate will produce 357.3 kilograms of NH + 4Absolute blowdown flow rate, if need 80 tons in water, produce waste water 80m in magnesiumcarbonate production per ton 3, on average contain ammonia nitrogen 4466.5mg/dm 3, surpass ammonia nitrogen emission standard 15mg/dm 3297.8 times, waste water per ton is received 1.45 yuan of effluent charge, 1 ton of magnesiumcarbonate of every production will be received 116 yuan of effluent charge, 1 ton of magnesium oxide of every production will be received 290 yuan of effluent charge.
The present invention applies mechanically owing to the ammonium salt solution closed cycle, so no discharging of waste liquid.And gained magnesiumcarbonate foreign matter content is low, and product can be produced the raw material of the light magnesium oxide that meets the Ministry of Chemical Industry's standard.
Following embodiment proposes in order better the present invention to be described, but this Fa Ming And is not subjected to the restriction of these embodiment.Following embodiment one～six, the leaching part, embodiment seven～nine, reactive moieties, embodiment ten is that mother liquor returns and makes use-case.
Embodiment one
Stirrer is being housed, the 2000cm of reflux cooler and thermometer 3In the there-necked flask, add 35.0 gram magnesia (containing MgO82.86%) and 1200cm 30.6mol/dm 3(NH 4) 2SO 4Solution is heated to boiling in oil bath, emit ammonia, keeps little boiling 3 hours, and cold filtration is analyzed Mg in the filtrate ++Concentration must contain Mg ++Concentration is 0.537mol/dm 3Solution 1005cm 3, Mn ++The impurity concentration trace, the Magnesium Carbonate Light 41-45 that this solution makes by the method for embodiment seven can make to meet the raw material of standard laid down by the ministries or commissions of the Central Government HG1-324-77 light magnesium oxide.
Embodiment two
The add-on of magnesia is 29.75 grams, and other condition is constant among the embodiment one, and gained magnesiumcarbonate and magnesium oxide all meet aforesaid standards.
Embodiment three
The add-on of magnesia is 39.2 grams, and other condition is constant in the example one, and gained magnesiumcarbonate and magnesium oxide meet aforesaid standards.
Embodiment four
Add the magnesia among 90 gram magnesite breezes (containing MgO 33%) the replacement embodiment one, all the other conditions are constant, must contain Mg ++Concentration is 0.05mol/dm 3Solution 1003cm 2Gained magnesiumcarbonate and magnesium oxide meet aforesaid standards.
Embodiment five
Add 1.2mol/dm 3NH 4Cl solution 1200cm 3Replace (the NH among the embodiment one 4) 2SO 4Solution, other condition is constant, must contain Mg ++Concentration is 0.52mol/dm 3Solution 998cm 3, gained magnesiumcarbonate and magnesium oxide meet aforesaid standards.
Embodiment six
Add 1.2mol/dm 3NH 4NO 3Solution 1200cm 3Replace (the NH among the embodiment one 4) 2SO 4Solution, other condition is constant, must contain Mg ++Concentration is 0.54mol/dm 3Solution 1000cm 3, gained magnesiumcarbonate and magnesium oxide meet aforesaid standards.
Embodiment seven
At 2000cm 3Add embodiment one gained MgSO in the beaker 4Solution (0.537mol/dm 3) 1005cm 3, add 98.04% technical grade NH 4HCO 352.2 restrain 20% ammoniacal liquor 68.6cm 3Warming while stirring to 70 ℃, filter, filter cake washes with water, and dewatered drying gets magnesium basic carbonate 40.21 grams, and quality meets GB1612-79, this magnesiumcarbonate roasting is got MgO16.89 gram (in 100%), meet the requirement of HG1-324-77 select quality, the mother liquor wash water reclaims and is used for leaching, no discharging of waste liquid.
Embodiment eight
At 2000cm 3Add MgSO in the beaker 4Solution (0.41mol/dm 3) 1000cm 3, add 98.04% technical grade NH 4HCO 366.1 gram does not add ammoniacal liquor, is warming up to 90 ℃, other is pressed embodiment seven and handles equally, gets magnesiumcarbonate 24.8 grams, gets MgO9.92 gram (in 100%) after the roasting, meets aforesaid standards, and the mother liquor wash water reclaims and is used for leaching no discharging of waste liquid.
Embodiment nine
At 2000cm 3Add MgSO in the beaker 4Solution (0.83mol/dm 3) 1000cm 3, add 98.04% technical grade NH 4HCO 366.9 gram adds 20% ammoniacal liquor 123cm 3, being warming up to 40 ℃, other is pressed embodiment seven and handles equally, gets magnesiumcarbonate 58.5 grams, gets MgO23.4 gram (100%) after the roasting, meets aforesaid standards, and the mother liquor wash water reclaims and is used for leaching no discharging of waste liquid.
Embodiment ten
Example seven mother liquors (are analyzed: Mg ++0.1023mol/dm 3, (NH 4) 2SO 40.676mol/dm 3) replace (NH in the example one in proportion 4) 2SO 4Solution, other condition is constant, must contain Mg ++Concentration 0.41mol/dm 3Solution 1000cm 3, add 98.04% technical grade NH 4HCO 365.4 gram adds 20% ammoniacal liquor 86cm 3, being warming up to 60 ℃, other is pressed embodiment seven and handles equally, gets magnesiumcarbonate 54.5 grams, gets magnesium oxide 21.8 grams (100%) after the roasting, meets aforesaid standards, still recyclable leaching, the no discharging of waste liquid of being used for of mother liquor and wash water.

Claims (10)

1, a kind ofly prepare the method for magnesiumcarbonate, it is characterized in that from magnesium-containing mineral:
1.1 decompose magnesium-containing mineral with ammonium salt solution, the preparation magnesium salt solution,
1.2 with the carbonate and the reaction of above-mentioned magnesium salt solution of ammonium, produce magnesiumcarbonate,
1.3 after absorbing, reaction by product ammonia water recycles,
1.4 the ammonium salt-containing mother liquor behind the separation magnesiumcarbonate recycles.
2, according to the method for claim 1.1, it is characterized in that described ammonium salt solution is an ammonium sulfate, ammonium chloride or ammonium nitrate, described magnesium-containing mineral are magnesia, magnesite breeze.
3,, it is characterized in that temperature of reaction is near the solution boiling point according to the method for claim 2..
4,, it is characterized in that the magnesium oxide mole ratio is 1: 0.85～1.12 in described ammonium salt and the magnesia according to the method for claim 2..
5,, it is characterized in that the carbonate of described ammonium contains bicarbonate of ammonia and reaction recovery ammoniacal liquor according to the method for claim 1.2.
6,, it is characterized in that the Mg that reacts according to the method for claim 1.2 ++Concentration is 0.41～0.83mol/dm 3Between.
7,, it is characterized in that the NH that reacts according to the method for claim 1.2 4HCO 3With Mg ++Mole ratio be 1～1.2: 1.
8,, it is characterized in that the NH that reacts according to the method for claim 1.2 4OH/NH 4HCO 3Mole ratio be 0～1.75: 1.
9,, it is characterized in that temperature of reaction is at 40～90 ℃ according to the method for claim 1.2.
10, according to the method for claim 1.2, it is characterized in that Mg ++Concentration is 0.41mol/dm 3NH 4HCO 3/ Mg ++=1.2: 1, NH 4OH/NH 4HCO 3=1.15: 1, temperature of reaction is 50-70 ℃.
CN 86102539 1986-10-15 1986-10-15 The no waste liquid manufacture method of Magnesium Carbonate Light 41-45 Pending CN86102539A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1051748C (en) * 1996-07-15 2000-04-26 国家建筑材料工业局地质研究所 Preparation of ultra-light magnesium oxide using blocky shepardite
CN101993097B (en) * 2009-08-25 2012-08-22 中国科学院过程工程研究所 Method for producing magnesium oxide with co-production of ammonium chloride by taking magnesium carbonate hydrate as intermediate
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
CN104843756A (en) * 2015-03-26 2015-08-19 龙岩紫云化学科技有限公司 Decomposition method of carbonatite
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

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1051748C (en) * 1996-07-15 2000-04-26 国家建筑材料工业局地质研究所 Preparation of ultra-light magnesium oxide using blocky shepardite
CN101993097B (en) * 2009-08-25 2012-08-22 中国科学院过程工程研究所 Method for producing magnesium oxide with co-production of ammonium chloride by taking magnesium carbonate hydrate as intermediate
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
CN104843756A (en) * 2015-03-26 2015-08-19 龙岩紫云化学科技有限公司 Decomposition method of carbonatite
CN104843756B (en) * 2015-03-26 2017-05-31 龙岩紫云化学科技有限公司 A kind of decomposition method of carbonate mine
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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