WO2020155245A1 - 一种利用菱镁矿微波活化制备高活性氧化镁的方法 - Google Patents

一种利用菱镁矿微波活化制备高活性氧化镁的方法 Download PDF

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WO2020155245A1
WO2020155245A1 PCT/CN2019/076096 CN2019076096W WO2020155245A1 WO 2020155245 A1 WO2020155245 A1 WO 2020155245A1 CN 2019076096 W CN2019076096 W CN 2019076096W WO 2020155245 A1 WO2020155245 A1 WO 2020155245A1
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magnesium oxide
magnesite
activation
highly active
microwave
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French (fr)
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马北越
吴桦
任鑫明
刘朝阳
靳恩东
付高峰
于景坤
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东北大学
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    • C—CHEMISTRY; METALLURGY
    • C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2/00—Lime, magnesia or dolomite
    • C04B2/10—Preheating, burning calcining or cooling
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F5/00—Compounds of magnesium
    • C01F5/02—Magnesia
    • C01F5/06—Magnesia by thermal decomposition of magnesium compounds
    • C01F5/08—Magnesia by thermal decomposition of magnesium compounds by calcining magnesium hydroxide
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00—Physical properties of inorganic compounds
    • C01P2006/12—Surface area

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  • the invention belongs to the technical field of efficient utilization of metallurgical resources, and specifically relates to a method for preparing high-activity magnesium oxide by microwave activation of magnesite.
  • activated magnesium oxide is an important raw material for the preparation of electronic components, inks, and harmful gas adsorbents because of its high specific surface area. It is expected to become a high-end, high-temperature, corrosion-resistant magnesium product.
  • the preparation methods of active magnesium oxide mainly adopt ammonium salt method, carbonation method and acid leaching method.
  • the method has a relatively complicated reaction process and low recovery rate. Therefore, the search for a low-cost, high-efficiency method is of great significance to the production of activated magnesium oxide.
  • the purpose of the present invention is to overcome the shortcomings of the prior art and provide a method for preparing highly active magnesium oxide by microwave activation of magnesite.
  • the main steps of the method are as follows: firstly, the magnesite is lightly burned, hydrated, wet-milled, and filtered to obtain a magnesium hydroxide filtrate; secondly, after the filtrate is dried, microwave heating is performed to complete the activation and thermal decomposition at the same time Process; Finally, the specific surface area and activity test of the prepared magnesium oxide.
  • a method for preparing highly active magnesium oxide by microwave activation of magnesite is carried out in the following steps:
  • Step 1 Light heating + hydration + wet grinding + filtration
  • the magnesite raw material is calcined in a high-temperature furnace to obtain light-burned magnesia powder
  • microwave heating is performed to complete activation and thermal decomposition, wherein the microwave heating temperature is 500-700°C, and the heating time is 1 to 3 hours.
  • the high-temperature furnace is one of a shaft kiln, a boiling furnace, and a suspension furnace; the calcination temperature is 800-900°C, and the calcination time is 2-4h.
  • the ratio of the deionized water and the primary lightly burned magnesia powder according to the volume of the liquid to the mass of the solid is (3 ⁇ 4): 1, the unit is ml:g; the ball mill adopts vacuum Ball mill jar and ZrO 2 mill ball.
  • the drying temperature of the filtrate is 100-120°C, and the drying time is 20-24h.
  • step 2 highly active magnesium oxide to be prepared to test the activity obtained: specific surface area of high activity magnesium oxide prepared was 140.14 ⁇ 144.82m 2 ⁇ g -1, iodine absorption of 192.32 ⁇ 196.75mg ⁇ g - 1 .
  • the method for performing activity test on the prepared high-activity magnesium oxide is:
  • the iodine adsorption method is used to test the activity of magnesium oxide, and the iodine absorption value is used as an indicator of the activity of magnesium oxide.
  • the iodine adsorption method is: take 2g of active magnesium oxide and 100ml, 0.1mol ⁇ L -1 carbon tetrachloride solution into a 200ml glass bottle, and put it Shake vigorously for 30 minutes to allow the suspension to settle for 5 minutes; then absorb 20ml of the clear solution and place it in 50ml, 0.03mol ⁇ L -1 potassium iodide ethanol solution, and use 0.025mol ⁇ L -1 NaS 2 O 3 Standard solution titration.
  • the formula for the iodine absorption value is (25) ⁇ (127) ⁇ C ⁇ (V 1 -V 2 ), where C is the concentration of the NaS 2 O 3 standard solution, mol ⁇ L -1; V 1 NaS 20ml iodine titration of stock 2 O 3 consumption of standard solution volume, ml; V 2 is the iodine titration after contacting magnesium 20ml sample consumed the NaS 2 O 3 standard solution volume, ml; 127 1ml NaS 2 O 3 with a concentration of 0.5mol ⁇ L -1 is equivalent to the number of milligrams of iodine; 25 is the conversion formula for 1ml of iodine.
  • the method of the present invention for preparing high-activity magnesium oxide by microwave activation of magnesite realizes the high-efficiency and high-value-added utilization of magnesite, which is beneficial to reduce environmental pollution, and it is easy to produce high-activity magnesium oxide.
  • the method of the present invention for preparing highly active magnesium oxide by microwave activation of magnesite proposes microwave heating after drying the magnesium hydroxide slurry, which is a hydration product of magnesite, to complete the activation and thermal decomposition process at the same time, saving The process improves the production efficiency, and the operation is simple and easy to implement, which is convenient for industrial production.
  • Figure 1 is a process flow diagram of the method for preparing highly active magnesium oxide by microwave activation of magnesite according to the present invention.
  • the main component of magnesite used in the following embodiments is MgCO 3 , and its mass percentage is 47% MgO, 52% CO 2 , and the balance is oxide impurities of Si, Ca, Fe, and Al.
  • the iodine adsorption method used in the following examples is: take 2g of active magnesium oxide sample and 100ml, 0.1mol ⁇ L -1 carbon tetrachloride solution in a 200ml glass bottle, shake it vigorously for 30min to make the suspension Let stand and settle for 5 minutes; then draw 20ml of the clear solution, place it in 50ml, 0.03mol ⁇ L -1 of potassium iodide ethanol solution, and titrate with a NaS 2 O 3 standard solution with a concentration of 0.025mol ⁇ L -1 .
  • the formula for the iodine absorption value is (25) ⁇ (127) ⁇ C ⁇ (V 1 -V 2 ), where C is the concentration of NaS 2 O 3 standard solution, mol ⁇ L -1 ; V 1 is the titration of 20 ml of iodine 2 O 3 NaS stock standard solution consumed volume, ml; V 2 is the iodine titration of a sample after contacting magnesium 20ml consumed standard NaS 2 O 3 solution volume, ml; 127 to 1ml, concentration 0.5mol ⁇ L - 1 NaS 2 O 3 is equivalent to milligrams of iodine; 25 is the conversion formula for 1 ml of iodine.
  • Step 1 Light heating + hydration + wet grinding + filtration
  • the magnesite is calcined in a shaft kiln at 800°C for 2 hours to obtain light burnt magnesia powder;
  • the filtrate was first dried at 100°C for 24 hours, and then subjected to microwave treatment, heated to 500°C, and kept for 1 hour, and at the same time, the activation and thermal decomposition processes were completed to obtain highly active magnesium oxide.
  • the iodine adsorption method is used to test the activity of magnesium oxide, and the iodine absorption value is used as an indicator of the activity of magnesium oxide.
  • the specific surface area of activated magnesium oxide is 140.14m 2 ⁇ g -1 and the iodine absorption value is 192.32 mg ⁇ g -1 .
  • a method for preparing highly active magnesium oxide by microwave activation of magnesite is carried out in the following steps:
  • Step 1 Light heating + hydration + wet grinding + filtration
  • the filtrate was first dried at 120°C for 20 hours, and then subjected to microwave treatment, heated to 700°C, and kept for 1 hour, and the activation and thermal decomposition processes were completed at the same time to obtain highly active magnesium oxide.
  • the iodine adsorption method is used to test the activity of magnesium oxide, and the iodine absorption value is used as an indicator of the activity of magnesium oxide.
  • the specific surface area of activated magnesium oxide is 143.52m 2 ⁇ g -1
  • the iodine absorption value is 196.35 mg ⁇ g -1 .
  • a method for preparing highly active magnesium oxide by microwave activation of magnesite is carried out in the following steps:
  • Step 1 Light heating + hydration + wet grinding + filtration
  • the filtrate was first dried at 120°C for 24 hours, and then subjected to microwave treatment, heated to 500°C, and kept for 1 hour, and at the same time, the activation and thermal decomposition processes were completed to obtain highly active magnesium oxide.
  • the iodine adsorption method is used to test the activity of magnesium oxide, and the iodine absorption value is used as an indicator of the activity of magnesium oxide.
  • the specific surface area of activated magnesium oxide is 142.22m 2 ⁇ g -1 and the iodine absorption value is 193.15 mg ⁇ g -1 .
  • a method for preparing highly active magnesium oxide by microwave activation of magnesite is carried out in the following steps:
  • Step 1 Light heating + hydration + wet grinding + filtration
  • the filtrate was first dried at 120°C for 24 hours, and then subjected to microwave treatment, heated to 700°C, and kept for 3 hours, and the activation and thermal decomposition processes were completed at the same time to obtain highly active magnesium oxide.
  • the iodine adsorption method is used to test the activity of magnesium oxide, and the iodine absorption value is used as an indicator of the activity of magnesium oxide.
  • the specific surface area of activated magnesium oxide is 144.82m 2 ⁇ g -1
  • the iodine absorption value is 196.75 mg ⁇ g -1 .

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Abstract

一种利用菱镁矿微波活化制备高活性氧化镁的方法，属于冶金资源高效利用技术领域。具体制备方法为：首先，将菱镁矿进行轻烧、水化、湿磨、过滤处理，获得氢氧化镁滤液；其次，将滤液干燥后，再进行微波加热，同时完成活化和热分解过程；最后，对制备的氧化镁进行比表面积和活性测试。该方法提出对菱镁矿的水化产物氢氧化镁料浆干燥后进行微波处理，同时完成活化和热分解过程，节省工序，提高生产效率。

Description

一种利用菱镁矿微波活化制备高活性氧化镁的方法 技术领域：
本发明属于冶金资源高效利用技术领域，具体涉及一种利用菱镁矿微波活化制备高活性氧化镁的方法。
背景技术：
我国的菱镁矿资源很丰富，但大多数镁质产品为中低端产品，资源浪费严重。因此，开发高端镁制品是研究的重点和热点。其中，活性氧化镁因具有较高的比表面积，是制备电子元件、油墨、有害气体吸附剂的重要原料，有望成为高温、耐腐蚀的镁质高端产品。
目前，活性氧化镁的制备方法主要采用铵盐法、碳酸化法和酸浸法。其方法反应过程较为复杂，回收利用率较低。因此，寻求低成本、高效率的方法对活性氧化镁的生产具有重要的意义。
发明内容：
本发明的目的是克服上述现有技术存在的不足，提供一种利用菱镁矿微波活化制备高活性氧化镁的方法。该方法的主要工序如下：首先，将菱镁矿进行轻烧、水化、湿磨、过滤处理，获得氢氧化镁滤液；其次，将滤液干燥后，再进行微波加热，同时完成活化和热分解过程；最后，对制备的氧化镁进行比表面积和活性测试。
为实现上述目的，本发明采用以下技术方案：
一种利用菱镁矿微波活化制备高活性氧化镁的方法，按以下步骤进行：
步骤1：轻烧+水化+湿磨+过滤
(1)将菱镁矿原料置于高温炉中煅烧，获得轻烧氧化镁粉；
(2)将轻烧氧化镁粉和去离子水置于球磨机中，以200～300r·min -1转速单向运行10～15h，同时完成水化和湿磨处理，形成球磨后料浆；
(3)将球磨后料浆过滤，取滤液；
步骤2：干燥+活化+热分解
滤液先经干燥后，进行微波加热，完成活化和热分解，其中，所述的微波加热温度为500～700℃，加热时间为1～3h。
所述的步骤1(1)中，所述高温炉为竖窑、沸腾炉、悬浮炉中的一种；煅烧温度为800～900℃，煅烧时间为2～4h。
所述的步骤1(2)中，所述的去离子水与一次轻烧氧化镁粉按液体积与固体质量比为(3～4)： 1，单位ml:g；所述的球磨采用真空球磨罐和ZrO 2磨球。
所述的步骤2中，滤液干燥温度为100～120℃，干燥时间为20～24h。
所述的步骤2中，对制备的高活性氧化镁进行活性测试得：制备的高活性氧化镁的比表面积为140.14～144.82m 2·g -1，吸碘值为192.32～196.75mg·g -1。
所述的步骤2中，对制备的高活性氧化镁进行活性测试的方法为：
(1)利用比表面积分析仪，采用氮吸附法测试分解后试样的比表面积；
(2)采用碘吸附法测试氧化镁的活性，以吸碘值作为氧化镁活性的指标。
所述的步骤2(2)中，所述的碘吸附法为：取2g的活性氧化镁制样和100ml、0.1mol·L -1的四氯化碳溶液置于200ml玻璃瓶中，将其剧烈震荡30min，使悬浮液静置沉降5min；然后吸取20ml的清澈溶液，置于50ml、0.03mol·L -1的碘化钾的乙醇溶液中，用浓度为0.025mol·L -1的NaS 2O 3标准溶液滴定。
所述的步骤2(2)中，所述的吸碘值公式为(25)×(127)×C×(V 1-V 2)，其中C为NaS 2O 3标准溶液的浓度，mol·L -1；V 1为滴定20ml碘原液消耗的NaS 2O 3标准溶液体积，ml；V 2为滴定20ml接触氧化镁样品后的碘液所消耗的NaS 2O 3标准溶液体积，ml；127为1ml、浓度为0.5mol·L -1的NaS 2O 3相当于碘的毫克数；25为1ml碘的换算公式。
本发明的有益效果：
1.本发明的一种利用菱镁矿微波活化制备高活性氧化镁的方法，实现了菱镁矿高效高附加值利用，利于减少对环境产生的污染，且易制得高活性的氧化镁。
2.本发明的一种利用菱镁矿微波活化制备高活性氧化镁的方法，提出对菱镁矿的水化产物氢氧化镁料浆干燥后进行微波加热，同时完成活化和热分解过程，节省工序，提高生产效率，且操作简单易行，便于工业化生产。
附图说明：
图1是本发明的利用菱镁矿微波活化制备高活性氧化镁的方法工艺流程图。
具体实施方式：竖窑、沸腾炉、悬浮炉
下面结合实施例对本发明作进一步的详细说明。
以下实施例中采用的菱镁矿的主要组分为MgCO 3，其质量百分比为47％MgO，52％CO 2，余量为Si、Ca、Fe、Al的氧化物杂质。
以下实施例中采用的碘吸附法为：取2g的活性氧化镁制样和100ml、0.1mol·L -1的四氯化碳溶液置于200ml玻璃瓶中，将其剧烈震荡30min，使悬浮液静置沉降5min；然后吸取20ml的清澈溶液，置于50ml、0.03mol·L -1的碘化钾的乙醇溶液中，用浓度为0.025mol·L -1的NaS 2O 3标准溶液滴定。
所述的吸碘值公式为(25)×(127)×C×(V 1-V 2)，其中C为NaS 2O 3标准溶液的浓度，mol·L -1；V 1为滴定20ml碘原液消耗的NaS 2O 3标准溶液体积，ml；V 2为滴定20ml接触氧化镁样品后的碘液所消耗的NaS 2O 3标准溶液体积，ml；127为1ml、浓度为0.5mol·L -1的NaS 2O 3相当于碘的毫克数；25为1ml碘的换算公式。
实施例1
一种利用菱镁矿微波活化制备高活性氧化镁的方法，其工艺流程图如图1所示，按以下步骤进行：
步骤1：轻烧+水化+湿磨+过滤
(1)将菱镁矿置于800℃竖窑中煅烧2h，获得轻烧氧化镁粉；
(2)将1000g的轻烧氧化镁粉和3倍的，即3000ml去离子水，即置于行星式球磨机中，以300r·min -1转速单向运行10h，同时完成水化和湿磨处理；
(3)将球磨后料浆过滤，取滤液。
步骤2：干燥+活化+热分解
将滤液先在100℃下干燥24h，再进行微波处理，加热至500℃，并保温1h，同时完成活化和热分解过程，制得高活性氧化镁。
步骤3：活性测试
(1)利用比表面积分析仪，采用氮吸附法测试分解后试样的比表面积；
(2)采用碘吸附法测试氧化镁的活性，以吸碘值作为氧化镁活性的指标。
经检测，活性氧化镁的比表面积为140.14m 2·g -1，吸碘值为192.32mg·g -1。
实施例2
一种利用菱镁矿微波活化制备高活性氧化镁的方法，按以下步骤进行：
步骤1：轻烧+水化+湿磨+过滤
(1)将菱镁矿置于850℃沸腾炉中煅烧2h，获得轻烧氧化镁粉；
(2)将1000g的轻烧氧化镁粉和4倍的，即4000ml去离子水置于行星式球磨机中，以200r·min -1转速单向运行15h，同时完成水化和湿磨处理；
(3)将球磨后料浆过滤，取滤液。
步骤2：干燥+活化+热分解
将滤液先在120℃下干燥20h，再进行微波处理，加热至700℃，并保温1h，同时完成活化和热分解过程，制得高活性氧化镁。
步骤3：活性测试
(1)利用比表面积分析仪，采用氮吸附法测试分解后试样的比表面积；
(2)采用碘吸附法测试氧化镁的活性，以吸碘值作为氧化镁活性的指标。
经检测，活性氧化镁的比表面积为143.52m 2·g -1，吸碘值为196.35mg·g -1。
实施例3
一种利用菱镁矿微波活化制备高活性氧化镁的方法，按以下步骤进行：
步骤1：轻烧+水化+湿磨+过滤
(1)将菱镁矿置于900℃悬浮炉中煅烧4h，获得轻烧氧化镁粉；
(2)将1000g的轻烧氧化镁粉和3倍的，即3000ml去离子水置于行星式球磨机中，以200r·min -1转速单向运行10h，同时完成水化和湿磨处理；
(3)将球磨后料浆过滤，取滤液。
步骤2：干燥+活化+热分解
将滤液先在120℃下干燥24h，再进行微波处理，加热至500℃，并保温1h，同时完成活化和热分解过程，制得高活性氧化镁。
步骤3：活性测试
(1)利用比表面积分析仪，采用氮吸附法测试分解后试样的比表面积；
(2)采用碘吸附法测试氧化镁的活性，以吸碘值作为氧化镁活性的指标。
经检测，活性氧化镁的比表面积为142.22m 2·g -1，吸碘值为193.15mg·g -1。
实施例4
一种利用菱镁矿微波活化制备高活性氧化镁的方法，按以下步骤进行：
步骤1：轻烧+水化+湿磨+过滤
(1)将菱镁矿置于850℃悬浮炉中煅烧3h，获得轻烧氧化镁粉；
(2)将1000g的轻烧氧化镁粉和4倍的，即4000ml去离子水置于行星式球磨机中，以300r·min -1转速单向运行15h，同时完成水化和湿磨处理；
(3)将球磨后料浆过滤，取滤液。
步骤2：干燥+活化+热分解
将滤液先在120℃下干燥24h，再进行微波处理，加热至700℃，并保温3h，同时完成活化和热分解过程，制得高活性氧化镁。
步骤3：活性测试
(1)利用比表面积分析仪，采用氮吸附法测试分解后试样的比表面积；
(2)采用碘吸附法测试氧化镁的活性，以吸碘值作为氧化镁活性的指标。
经检测，活性氧化镁的比表面积为144.82m 2·g -1，吸碘值为196.75mg·g -1。

Claims (5)

  1. 一种利用菱镁矿微波活化制备高活性氧化镁的方法，其特征在于，按以下步骤进行：
    步骤1：轻烧+水化+湿磨+过滤
    (1)将菱镁矿原料置于高温炉中煅烧，获得轻烧氧化镁粉；
    (2)将轻烧氧化镁粉和去离子水置于球磨机中，以200～300r·min -1转速单向运行10～15h，同时完成水化和湿磨处理，形成球磨后料浆；
    (3)将球磨后料浆过滤，取滤液；
    步骤2：干燥+活化+热分解
    滤液先经干燥后，进行微波加热，完成活化和热分解，其中，所述的微波加热温度为500～700℃，加热时间为1～3h。
  2. 根据权利要求1所述的一种利用菱镁矿微波活化制备高活性氧化镁的方法，其特征在于，所述的步骤1(1)中，所述高温炉为竖窑、沸腾炉、悬浮炉中的一种；煅烧温度为800～900℃，煅烧时间为2～4h。
  3. 根据权利要求1所述的一种利用菱镁矿微波活化制备高活性氧化镁的方法，其特征在于，所述的步骤1(2)中，所述的去离子水与一次轻烧氧化镁粉按液体积与固体质量比为(3～4)：1，单位ml:g；所述的球磨采用真空球磨罐和ZrO 2磨球。
  4. 根据权利要求1所述的一种利用菱镁矿微波活化制备高活性氧化镁的方法，其特征在于，所述的步骤2中，滤液干燥温度为100～120℃，干燥时间为20～24h。
  5. 根据权利要求1所述的一种利用菱镁矿微波活化制备高活性氧化镁的方法，其特征在于，所述的步骤2中，对制备的高活性氧化镁进行活性测试得：制备的高活性氧化镁的比表面积为140.14～144.82m 2·g -1，吸碘值为192.32～196.75mg·g -1。
PCT/CN2019/076096 2019-02-01 2019-02-26 一种利用菱镁矿微波活化制备高活性氧化镁的方法 WO2020155245A1 (zh)

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