CN105460961B - A kind of method that nodeless mesh aqueous carbonate magnesium is prepared using heavy magnesium water - Google Patents

A kind of method that nodeless mesh aqueous carbonate magnesium is prepared using heavy magnesium water Download PDF

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Publication number
CN105460961B
CN105460961B CN201610023080.1A CN201610023080A CN105460961B CN 105460961 B CN105460961 B CN 105460961B CN 201610023080 A CN201610023080 A CN 201610023080A CN 105460961 B CN105460961 B CN 105460961B
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magnesium
water
precipitating reagent
temperature drying
heavy
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CN105460961A (en
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宋丽英
胡泽铭
胡晓波
胡庆福
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Noncommissioned Officer Academy of Army Medical University
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00Compounds of magnesium
    • C01F5/24Magnesium carbonates

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
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  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention discloses a kind of method that nodeless mesh aqueous carbonate magnesium is prepared using heavy magnesium water:Comprise the following steps:(1)A certain amount of precipitating reagent is added into heavy magnesium water at normal temperatures, generates the carbonic acid magnesium precipitate suspension containing the crystallization water;(2)Above-mentioned suspension is separated by filtration, collects filter cake, filtrate storage, comprehensive utilization;(3)Filter cake carries out low temperature drying, drying temperature is controlled at 70 ~ 150 DEG C through secondary drying first in containing carbon dioxide atmosphere, more than 90% Free water is removed, is then fed into high temperature drying, drying temperature is controlled at 150 ~ 300 DEG C, remaining Free water and the crystallization water are removed, nodeless mesh aqueous carbonate magnesium products are made.The method investment cost of the present invention is low, overcomes the high disadvantage of carbonizatin method energy consumption, and relatively lightweight magnesium carbonate production effects of energy saving and emission reduction is notable, there is provided fire retardant new product.

Description

A kind of method that nodeless mesh aqueous carbonate magnesium is prepared using heavy magnesium water
Technical field
It is particularly a kind of to be carbonized using dolomite carbonizatin method, magnesite the present invention relates to a kind of method for preparing magnesium carbonate The method that heavy magnesium water in method technique prepares nodeless mesh aqueous carbonate magnesium, belongs to technical field of preparation for inorganic material.
Background technology
" the carbonic acid magnesium products " for using and selling on domestic and international market at present, in addition to magnisite carbonic acid magnesium products, Artificial synthesized " magnesium carbonate " product is hydrated basic magnesium carbonate:xMgCO3·yMg(OH)2·zH2O, wherein x=1 ~ 4, y=0 ~ 1, z=0 ~ 8.Have according to the literature as form existing for the hydrate of magnesium carbonate:MgCO3·H2O、MgCO3·3H2O、MgCO3· 2H2O and basic magnesium carbonate:4MgCO3·Mg(OH)2·8H2O、4MgCO3·Mg(OH)2·6H2O、4MgCO3·Mg(OH)2· 5H2O、4MgCO3·Mg(OH)2·4H2O、4MgCO3·Mg(OH)2·7H2O;3MgCO3·Mg(OH)2·3H2O、3MgCO3·Mg (OH)2·4H2The forms such as O.When sell product in 4MgCO3·Mg(OH)2·4H2Based on O products.
The preparation method of industrial hydrated basic magnesium carbonate is roughly divided into:(1)MgCl2Or MgSO4Method of Soda;(2)MgCl2 Or MgSO4Sodium bicarbonate method or ammonium bicarbonate method;(3)Carbonizatin method, it is divided into dolomite carbonizatin method, magnesite(Light-magnesite powder)Carbon Change method, asbestos tailings carbonizatin method, bittern(Bischofite)Lime or dolomite ash carbonizatin method etc.;(4)Double decomposition etc..Above method In due to technological reaction system property determine can not or be difficult to produce nodeless mesh aqueous carbonate magnesium products.Hydrated basic magnesium carbonate is again Claim light magnesium carbonate, relative density is small, light and loose, can be used as the excellent filler and reinforcing agent of rubber.Because it has Have do not burn with quality it is light the characteristics of, available for adiabatic, resistant to elevated temperatures fire-retardant heat-insulation material, it can also be used to manufacture glass system The household chemicals such as product, magnesium salts, pigment, paint, fireproof coating, printing-ink, ceramics, cosmetics, toothpaste and pharmaceutical products, food Grade light magnesium carbonate can be used for flour additive, it may also be used for drier, carrier, anti-caking agent etc..With entering for epoch Step, is also continued to develop to magnesium carbonate demand.Not only demand light magnesium carbonate, the heavier magnesium carbonate of some industry requirements, such as mould Expect industry.As fire retardant in use, needing the higher product of processing temperature.In recent years, nodeless mesh aqueous carbonate magnesium is prepared and drawn Play domestic and international scientific and technological circle's concern.Patent CN1362371A provides one kind and high purity magnesium oxide or carbonic acid is prepared in circulatory mediator The method of magnesium, the aqueous carbonate ammonium of intermediate products four is prepared by raw material of industrial hex-ammoniate, magnesium sulfate, magnesium nitrate and ammonium carbonate solution Magnesium double salt precipitation, filtered, low temperature thermal decomposition prepare nodeless mesh aqueous carbonate magnesium.Dalian University Of Communications Wang Jing et al. is proposed with chlorination Magnesium is raw material, and urea is precipitating reagent, and under conditions of sodium citrate makees surfactant, Carbon Dioxide is prepared using hydro-thermal method Magnesium powder body, industrialized production is not implemented.
The content of the invention
It is an object of the invention to provide a kind of method that nodeless mesh aqueous carbonate magnesium is prepared using heavy magnesium water, its raw material sources Extensively, it is easily achieved industrialized production.
The method of the present invention is using heavy magnesium water as primary raw material.In dolomite carbonizatin method or magnesite carbonizatin method production industry water Close in basic magnesium carbonate technique, the filtrate that carbodiimide solution filters to isolate, referred to as heavy magnesium water, dissolving magnesium bicarbonate is contained in heavy magnesium water Weak solution, in terms of MgO, 4 ~ 10g/L of content.
Specifically, a kind of method that nodeless mesh aqueous carbonate magnesium is prepared using heavy magnesium water of the present invention, is comprised the following steps:
(1)Precipitating reagent is added into heavy magnesium water, the addition of precipitating reagent is 0.4 ~ 1.2 of MgO molal quantities in heavy magnesium water Times, precipitating reagent is reacted with the magnesium bicarbonate in heavy magnesium water, generates hydrated basic magnesium carbonate precipitated product suspension;
Precipitating reagent used is:Ammoniacal liquor, sodium hydroxide, potassium hydroxide, magnesium hydroxide, magnesia, light-magnesite powder, wherein One or more of mixtures;
(2)Suspension is filtered, carries out separation of solid and liquid, collects filter cake, filtrate comprehensive utilization;
(3)By step(2)Gained filter cake is sent into the secondary drying system of low temperature drying and high temperature drying composition, wherein, it is low Temperature drying is carried out in carbon dioxide atmosphere, 70 ~ 150 DEG C of temperature of control, and more than 90% freely in low temperature drying stage removing filter cake Moisture content;High temperature drying system is sent into containing the magnesium carbonate of less than 10% free moisture content and whole crystallizations water, controls temperature 150 ~ 300 DEG C, nodeless mesh aqueous carbonate magnesium products are made.
The method of the present invention, step(3)In, carbon dioxide mass concentration 10% ~ 60%, can be purification containing CO2 gases Mixture has CO2 mixed gas etc. in boiler flue or cleaned air after the kiln gas of various calcining kilns or purification afterwards.Low temperature Dry and high temperature drying phases-time is respectively 2 ~ 6 h.
The method of the present invention, secondary drying equipment, low temperature drying optional drying box in the lab are optional in industrial production With box drier, band drier, chain laminar drying machine, tunnel-kiln type dry kiln etc.;High temperature drying is optional in the lab Drier is made by oneself with stainless steel tube, and rotary dryer, Rotatingandflashstreamingdrier, strong drying machine, gas can be selected in industrial production Flow drying machine etc..
What the present invention obtained has the beneficial effect that:The method investment cost of the present invention is low, overcomes carbonizatin method energy consumption High disadvantage, production process effects of energy saving and emission reduction is notable, and fire retardant new product is provided for market.
Embodiment
Following examples are used to illustrate the present invention.
Embodiment 1
The heavy magnesium water 1000mL of the MgO containing 6g/L is added in reactor, temperature is 30 DEG C, is 2mol/L ammoniacal liquor by concentration 150mL is slowly added in reactor heavy magnesium water, opens mixer, and rotating speed control is stirred in 50 ~ 60 turns/min, stirring 3h, stopping, Cooling 3h, observation precipitation are staticly settled, and is filtered, adds 500mL mashing washings to filter every time with distilled water 2 times, filter cake is sent Drying box, low temperature drying 3h is carried out at 120 DEG C, wherein Free water is containing about 5%;It is placed on again in stainless steel tube, in 200 DEG C of perseverances Warm 2h, Carbon Dioxide magnesium products 11.5g, the magnesium rate of recovery 92% is made.Filtrate and wash water are separately stored in filtrate receiver and wash water groove, Digestion and carbonization water can be used as.
Embodiment 2
The heavy magnesium water 1000mL into the MgO containing 7g/L is contained in reactor, temperature is 40 DEG C, is 2mol/L NaOH by concentration Solution 180mL is slowly added in reactor heavy magnesium water, opens mixer, and rotating speed controls in 50 ~ 60 turns/min, stirs 2.5h, stop Only stir, staticly settle cooling 2.5h, observation precipitation, and filtered, add 500mL mashing washings to filter 2 every time with distilled water Secondary, filter cake send drying box, carries out low temperature drying 3.5h at 110 DEG C, wherein Free water is containing about 6%;It is placed on again in stainless steel tube In 190 DEG C of constant temperature 2.5h, Carbon Dioxide magnesium products 13.5g, the magnesium rate of recovery 91.84% is made.Filtrate and wash water are separately stored in filter Liquid bath and digestive shelf, comprehensive utilization.
Embodiment 3
The heavy magnesium water 1000mL into the MgO containing 8g/L is contained in reactor, temperature is 50 DEG C, is 1mol/L Mg by concentration (OH) 2 suspension 100mL are slowly added in reactor heavy magnesium water, open mixer, rotating speed control is in 50 ~ 60 turns/min, stirring 2h, stop stirring, staticly settle cooling 2h, filter, filter cake send drying box, in 105 DEG C, 30% CO2Low temperature drying 3h under atmosphere, Wherein Free water is containing about less than 6%;It is placed on again in stainless steel tube in 200 DEG C of constant temperature 2h, Carbon Dioxide magnesium products is made 28.9g, the magnesium rate of recovery 96.94%.

Claims (3)

  1. A kind of 1. method that nodeless mesh aqueous carbonate magnesium is prepared using heavy magnesium water, it is characterised in that comprise the following steps:
    (1)Precipitating reagent is added into heavy magnesium water, the addition of precipitating reagent is 0.4 ~ 1.2 times of MgO molal quantities in heavy magnesium water, is sunk Shallow lake agent is reacted with the magnesium bicarbonate in heavy magnesium water, generates hydrated basic magnesium carbonate precipitated product suspension;
    Precipitating reagent used is the mixture of first kind precipitating reagent and the second class precipitating reagent, and wherein first kind precipitating reagent is ammoniacal liquor, hydrogen One or more in sodium oxide molybdena, potassium hydroxide, the second class precipitating reagent are in magnesium hydroxide, magnesia, light-magnesite powder It is one or more;
    (2)Suspension is filtered, carries out separation of solid and liquid, collects filter cake, filtrate comprehensive utilization;
    (3)By step(2)Gained filter cake is sent into the secondary drying system being made up of low temperature drying and high temperature drying, wherein, low temperature Drying is carried out in carbon dioxide atmosphere, controls 70 ~ 150 DEG C of temperature, and the low temperature drying stage removes more than 90% Free water in filter cake Part;High temperature drying system is sent into containing the magnesium carbonate of less than 10% free moisture content and whole crystallizations water, controls 150 ~ 300 DEG C of temperature, Nodeless mesh aqueous carbonate magnesium products are made.
  2. 2. according to the method for claim 1, it is characterised in that step(3)In, carbon dioxide mass concentration 10% ~ 60%, contain There is CO2Gas is that mixture has CO in boiler flue or cleaned air after the kiln gas of various calcining kilns or purification after purification2It is mixed Close gas.
  3. 3. according to the method for claim 1, it is characterised in that low temperature drying stage and high temperature drying phases-time are respectively 2 ~6h。
CN201610023080.1A 2016-01-14 2016-01-14 A kind of method that nodeless mesh aqueous carbonate magnesium is prepared using heavy magnesium water Expired - Fee Related CN105460961B (en)

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CN105883865B (en) * 2016-04-13 2017-11-14 北京化工大学 A kind of environment-friendly preparation technology of high pure and ultra-fine anhydrous magnesium carbonate
CN106745110B (en) * 2016-11-30 2018-02-27 营口市荣兴达科技实业有限公司 A variety of crystal formation high purity magnesium carbonates and preparation method thereof
CN108773848B (en) * 2018-08-23 2020-03-31 淄博美盛化工有限公司 Device and method for preparing heavy magnesium carbonate from heavy magnesium water
CN113735238A (en) * 2021-10-28 2021-12-03 中国人民解放军陆军军医大学士官学校 Process for co-producing magnesium carbonate series products by seawater desalination device

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DE1442761A1 (en) * 1963-12-07 1969-01-23 Licencia Talalmanyokat Method and device for carrying out reactions between gases and liquids or suspensions under pressure
CN1410351A (en) * 2001-10-08 2003-04-16 中国科学院过程工程研究所 Method of preparing light magnesium carbonate from heavy magnesium water
CN1186256C (en) * 2002-06-14 2005-01-26 中国科学院过程工程研究所 Process for preparing magnesium carbonate whisker
CN101327942A (en) * 2008-07-29 2008-12-24 国家海洋局天津海水淡化与综合利用研究所 Method for preparing light magnesium carbonate and magnesium oxide from dolomite sea water bittern
CN102079533B (en) * 2010-12-03 2012-10-10 桐柏兴源化工有限公司 Method for preparing basic magnesium carbonate and high purity magnesium oxide with trona
CN103979584B (en) * 2014-06-03 2016-01-13 李广凡 A kind of boric sludge is for Magnesium Carbonate Light 41-45 technique

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