• 专利附录
  • 专利说明
  • 权利要求
  • 类似技术
  • 同族专利
  • 引用文献
  • 法律状态
  • 优先权
    • 专利摘要:
    Anhydrous magnesium carbonate is obtained from magnesium salt solutions or from suspensions of sparingly soluble magnesium compounds, for example nesquehonite, magnesium hydroxide, and the like by mixing the solution or suspension with ammonium carbonate, alkali metal carbonate or carbon dioxide such that the MgO:CO2 molar ratio is </=2.0, after which the mixture is decomposed in an autoclave at a temperature of >/=110 DEG C. The anhydrous magnesium carbonate is separated off from the mother liquor, from which the ammonia is regenerated by addition of calcium hydroxide, alkali metal hydroxides or a calcined magnesium-containing raw material, which at the same time gives a magnesium salt solution.
    公开号:SU1704626A3
    申请号:SU884356277
    申请日:1988-08-05
    公开日:1992-01-07
    发明作者:Бумбалек Вацлав；Хорак Вацлав；Зурек Франтишек；Прокмшка Франтишек
    申请人:Устав Про Вызкум Руд (Инопредприятие)；
    IPC主号:
    专利说明:

    This invention relates to inorganic chemistry and produces dried magnesium carbonate.
    The aim of the invention is to reduce the content of bound water and moisture in the target product.
    Example 1. In a 5,000 ml autoclave, 2000 ml of a magnesium chloride solution of the following composition was added, MgCl21b7.7, 28.9, CaCl0.03, Fe 0.005, and 340 g of ammonium carbonate was added, resulting in the NgiCO molar ratio in the reaction mixture is set to
    1.0 After that, the reaction mixture with stirring is heated to a temperature of 180 ° C, the resulting pressure of 1.9 MNa. The duration of the reaction in the temperature range 110-180 ° C 135 minutes After cooling, the solid phase is filtered off and washed, and 8.1 g / dm3 of KgCl is found in the filtrate. The residue on the filter (lepegak) is subjected to the study of the microstructure, differential thermal analysis and chemical analysis. The content of magnesium carbonate in this product is 99.6 wt.%. Wash filtrate
    Vj o
    4 o
    eight

    s
    170
     warm pa compile 1 / g calcined n / m mlnenitl, goderzhrgo, May. /: NC 87, SLO, 3, (, 25.. Ammilcle removal aids by boiling and Hylrcrni to HOOO ml rlstpor contains 1 X g / dm 3 MgdljH 7.0 g / dm 3 SL (: 12.
    Example 2. In a 300 capacity autoclave (1 ml of water, 2000 ml of a sulphate millina solution with a concentration of 193 g / dm3 KgS (4 after which the solution is heated to 110 ° with stirring) (and then ammonia and dioxide are introduced into the reaction vessel). carbon, as a result of which the molar ratio is Mg: C реак in the reaction mixture is 0.84. Ammonia is metered at a molar ratio NHjt 1.80. The reaction mixture is heated to 155 ° C, the maximum pressure reached is 3.2. MIA, after stabilization the pressure is equal to 1.6 MIA. After cooling, the resulting solid phase is subjected to analysis, microstructure tour - PTG corresponds to the crystalline microstructure of the KgCO.
    IrimerZ. 200 (1 ml of magnesium nitrate solution containing, g / dm3: Mg (NO,) 2 441, Ca (N () j) 2 4.4, then 880 g of potash are added to an autoclave with a capacity of 500 L ml. the mixture, the molar ratio of MgO:: CO2 of which is 0.93, is heated to 1 U5 C under a pressure of 2.1 KPa and immediately removed from the reaction vessel. The solid phase contains 98.0 wt.X MgCO and 1.8 wt.X CaCOe The yield of magnesium is 98.2%.
    Example. Into an autoclave with a capacity of 5000 ml, 2000 ml of a suspension of Nkwekhonite KgCO in distilled water was introduced. The concentration of solids in the suspension is 130.0 g / dm3. The reaction mixture is heated without the addition of other reagents, the ratio of MgO: C (. The maximum temperature reached 180 ° C at a pressure of 1.6 Mia. After cooling, the pure MgCO-j was confirmed by analyzing the PTC microstructure, the MgU concentration in the filtrate was 0.13 g / dm 3
    Example A 50 ml autoclave (10 ml was injected with 2000 ml of a magnesium hydroxide suspension in distilled water with a concentration of 100 g of solid per 1 liter. At the same time, 200 g of two carbon monoxide were added to the reaction vessel, resulting in a MgO: CC 2 molar ratio em
    5 about 5
    with
    $ 0 -
    five
    0.75. After cooling the reaction mixture to a temperature of 155 ° C, the pressure reaches 1.8 MPa, and after cooling in a solid veil Gmdl, only degumming magnesium carbonate is confirmed. In the liquid phase, the MgO concentration is 0.22 g / dm 3.
    Try it on An industrial reactor with a capacity of 2.8 m3 equipped with a mixing mechanism at 155 ° C and a pressure of 1.2 Mla is injected with a solution of magnesium chloride containing {g, d / m3: MgCl2 L 158.2, CaC12 0.8, NH4Cl 28.0 , and ammonium carbonate solution with a concentration of 309 g / dm3. Dosing is carried out as follows: 50 ml of magnesium chloride solution and 20 l of ammonium carbonate solution are injected into the reactor through Yumin each time, which provides an α-MgO ratio of CO, approximately 1.3. The resulting suspension is subjected to filtration and washing, the solid pelvis contains 99.2 wt.% KgCOj, the residual concentration in the solution is 48.4 g / dm3 KgCl.
    Example 7. 2000 ml of magnesium chloride solution with a concentration of 142.8 g / dm3 MgCl2 are introduced into an autoclave (5000 ml) and 500 ml of NaOH solution (g / dm5 NaOH) and 260 g of crystalline NaHCOj are added with stirring, thereby setting the ratio : C Ј in the reaction mixture with a value of 0.97. The closed autoclave is then heated to 160 ° C and the pressure is 1.1 MJIa. After cooling, the resulting suspension is filtered and washed with suction. The weight of the wet sediment on the filter is 278 g with a water content of 5.96%. After drying, 252 g of anhydrous magnesium carbonate are obtained.
    Try on A suspension consisting of 375 g of magnesium hydroxide and 2.26 dm3 of solution (NHq., Having a concentration of 273 g / dm3 is placed in a 5000 ml autoclave, thus the molar ratio MgO: C02 in the reaction mixture is about 1.
    I
    The reaction mixture with stirring is heated in a closed space to 193 ° C, the corresponding pressure of 2.7 MPa. After recovery, the solid phase is filtered and washed. Humidity of a deposit on the filter 9,2Х. Dried product weighing 532 g contained on the X-ray definition of fine structure only one solid phase - dehydrated carbonate
    magni. The filter, n.chyuchl rinse water, was supplemented to a volume of 2.5 dm3; according to dialysis, magnesium is detected, having a concentration of 2.1 g / dm3, like MgO 87, P g / dm3 NHj. Hydromagnet n solid product U7, U7, „
    II p and mep 9 "In a 5000 ml autoclave, a suspension containing 375 g of MgCOH) and 2.20 dm3 of water is placed, then 510 g of solid MH4SOE are added.
    With stirring, the reaction mixture is heated in a closed space to 174 ° C, the corresponding pressure is 2.1 MPa. The solid fraction obtained by filtration contains 11.3% moisture, and the dry matter with a mass of 535 g corresponds to its composition to dehydrated MgCOj. The filtrate, including the wash water, was added to a volume of 2.5 dm1, the concentration of KgO in the solution was 2.48 g / cm3, and №C 44 g / dm3.
    Example 10. A suspension of magnesium hydroxide in water with a concentration of 100 grams of solids per 1 liter and 865 grams of sodium hydrogencarbonate is placed in a 5000 ml autoclave, resulting in a molar ratio of MgOtCO of 0.5. The reaction mixture with stirring heated in an enclosed space of up to 175 ° C with a pressure of 1.3 MPa. After filtering and washing the solid phase, according to X-ray analysis of the fine structure, consists of dehydrated magnesium carbonate, dry weight is 428 g.
    The proposed method allows to obtain magnesium-free magnesium iodide with a moisture content of less than 10 /, while by a known method a product with a moisture content of 16.4% by weight is obtained
    权利要求:
    Claims (2)
    [1]
    1. A method of producing a dried magnesium carbonate from magnesium and carbonate-containing raw materials by heating, followed by separating the product from the mother liquor and washing the target product, characterized in that, in order to reduce the content of bound water and moisture in the target product, by contacting magnesium salts or magnesium hydroxide in water with carbon dioxide, or with ammonium carbonate, or with ammonium bicarbonate, obtained by reacting carbon dioxide and ammonia, or with alkali carbonate o metal, or with an alkali metal bicarbonate, taken in a mixture with sodium hydroxide at a molar ratio of MgO: CO in the reaction mixture not more than 1.3, at 155-195 ° C. for a contact time of 135 minutes.
    [2]
    2. Pop-up method 1, characterized in that the mother liquor and the wash water are decomposed by calcined magnesite to produce ammonia and return it to the contacting stage,
    Compiled by K.Naumova Editor N.Gunko tekhred L.KravchukKorrektor S.Shevkun
    Order 72
    Circulation
    VNIIPI State Committee for Inventions and Discoveries at the State Committee on Science and Technology of the USSR 113035, Moscow, Zh-35, Raushsk nab. 4/5
    Subscription v
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    同族专利:
    公开号 | 公开日
    EP0302514A2|1989-02-08|
    CS583787A1|1989-03-14|
    EP0302514A3|1990-05-09|
    BR8803890A|1989-02-21|
    JPH01133919A|1989-05-26|
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    引用文献:
    公开号 | 申请日 | 公开日 | 申请人 | 专利标题
    RU2533143C1|2013-03-26|2014-11-20|Геннадий Георгиевич Волокитин|Method of obtaining ultradispersive powders of carbonates|FR789670A|1934-05-19|1935-11-04|Soc Gen Magnesium|Process for obtaining anhydrous magnesium carbonate from dolomite or limestone|
    US2131524A|1934-05-19|1938-09-27|Magnesium Dev Corp|Process for the production of anhydrous magnesium carbonate|
    JPS5480298A|1977-12-09|1979-06-26|Toyo Soda Mfg Co Ltd|Production of magnesium orthocarbonate crystals|
    DE2847205C2|1978-10-30|1984-11-08|Vereinigte Aluminium-Werke AG, 1000 Berlin und 5300 Bonn|Process for the production of a paper filler and / or coating pigment|
    SU779308A1|1978-11-16|1980-11-15|Предприятие П/Я А-3732|Method of producing hydrated magnesium carbonate|KR100587914B1|2005-04-19|2006-06-08|한국전력공사|Method of preparing magnesium carbonate by supercritical fluid reaction proces|
    JP4944466B2|2006-03-22|2012-05-30|宇部マテリアルズ株式会社|Anhydrous magnesium carbonate powder and method for producing the same|
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    CN102718235A|2012-06-27|2012-10-10|辽宁工程技术大学|Method for preparing magnesium carbonate trihydrate crystal whiskers by adopting basic magnesium carbonate tetrahydrate|
    CN105883865B|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|
    CN105883867B|2016-06-24|2017-07-18|中国科学院地球化学研究所|A kind of method for preparing anhydrous magnesium carbonate at high temperature under high pressure|
    CN108238617B|2018-03-22|2020-02-21|河北科技大学|Method for producing anhydrous magnesium carbonate by carbonization method and anhydrous magnesium carbonate|
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    法律状态:
    优先权:
    申请号 | 申请日 | 专利标题
    CS875837A|CS265971B1|1987-08-06|1987-08-06|Process for preparing anhydrous magnesium carbonate|
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