WO2020155243A1 - Method for preparing high-density magnesia from magnesite by means of spark plasma sintering - Google Patents

Method for preparing high-density magnesia from magnesite by means of spark plasma sintering Download PDF

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WO2020155243A1
WO2020155243A1 PCT/CN2019/076094 CN2019076094W WO2020155243A1 WO 2020155243 A1 WO2020155243 A1 WO 2020155243A1 CN 2019076094 W CN2019076094 W CN 2019076094W WO 2020155243 A1 WO2020155243 A1 WO 2020155243A1
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magnesia
spark plasma
plasma sintering
magnesite
powder
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PCT/CN2019/076094
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French (fr)
Chinese (zh)
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马北越
任鑫明
靳恩东
刘朝阳
付高峰
于景坤
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东北大学
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2/00Lime, magnesia or dolomite
    • C04B2/10Preheating, burning calcining or cooling
    • C04B2/102Preheating, burning calcining or cooling of magnesia, e.g. dead burning
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2/00Lime, magnesia or dolomite
    • C04B2/10Preheating, burning calcining or cooling
    • C04B2/12Preheating, burning calcining or cooling in shaft or vertical furnaces

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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-density magnesia by using magnesite spark plasma sintering.
  • the method of the present invention for preparing high-density magnesia by spark plasma sintering of magnesite adopts spark plasma sintering technology and sintering under pressure, which not only shortens the sintering time, but also facilitates the preparation of high-density magnesia.
  • the obtained magnesium hydroxide powder is calcined in a 750°C shaft kiln for 4 hours to obtain secondary lightly burned magnesium oxide powder.
  • Step 3 Second light burn
  • a method for preparing high-density magnesia by spark plasma sintering of magnesite is carried out in the following steps:
  • Step 4 Spark plasma sintering

Abstract

Disclosed is a method for preparing high-density magnesia from magnesite by means of spark plasma sintering, which belongs to the technical field of efficient utilization of metallurgical resources. The specific preparation method involves: placing magnesite into a high-temperature furnace for calcination to obtain a light-burned magnesium oxide powder; placing the light-burned magnesium oxide powder into a ball milling tank, carrying out hydration and ball milling treatments on the light-burned magnesium oxide at the same time by using deionized water as a ball milling medium, and subjecting same to a drying treatment to obtain a magnesium hydroxide powder; placing the magnesium hydroxide powder into the high-temperature furnace for secondary calcination to obtain a secondary light-burned magnesium oxide powder; and finally, placing the secondary light-burned magnesium oxide fine powder into a graphite mold of a spark plasma sintering furnace, and subjecting same to spark plasma sintering at a certain temperature, time, and pressure to obtain the high-density magnesia.

Description

一种利用菱镁矿放电等离子烧结制备高密度镁砂的方法Method for preparing high-density magnesia by using magnesite spark plasma sintering 技术领域:Technical field:
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放电等离子烧结制备高密度镁砂的方法。The invention belongs to the technical field of efficient utilization of metallurgical resources, and specifically relates to a method for preparing high-density magnesia by using magnesite spark plasma sintering.
背景技术:Background technique:
我国有着丰富的菱镁矿资源,其主要用于生产轻烧氧化镁、烧结镁砂、电熔镁砂等镁质耐火原料,这些原料主要应用于冶金、化工、建材等行业中。然而,我国的镁制品以初级和低档产品为主,高附加值镁质材料,尤其是高体积密度的烧结镁砂产量极少。因此,以低成本、多储量的菱镁矿生产高密度烧结镁砂是我国镁制品研究的一个重要方向。my country has rich magnesite resources, which are mainly used to produce magnesia refractory raw materials such as light burned magnesia, sintered magnesia, and fused magnesia. These raw materials are mainly used in metallurgy, chemical, building materials and other industries. However, my country's magnesium products are mainly primary and low-end products, and the output of high value-added magnesium materials, especially high bulk density sintered magnesia, is very small. Therefore, the production of high-density sintered magnesia from low-cost, high-reserve magnesite is an important research direction of magnesium products in my country.
目前,多以菱镁矿或轻烧氧化镁粉为原料,在回转窑或竖窑中于1500~2300℃温度范围内煅烧,使MgO通过晶体长大和致密化,转变为惰性的烧结镁砂。此方法生产镁砂的密度和质量有待进一步提高。因此,如何高效利用菱镁矿制备出高密度的烧结镁砂备受关注。At present, magnesite or light-burned magnesia powder is mostly used as raw materials and calcined in a rotary kiln or shaft kiln at a temperature of 1500-2300°C, so that MgO is transformed into inert sintered magnesia through crystal growth and densification. The density and quality of magnesia produced by this method need to be further improved. Therefore, how to efficiently use magnesite to prepare high-density sintered magnesia has attracted much attention.
发明内容:Summary of the invention:
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放电等离子烧结制备高密度镁砂的方法。该方法的主要工序如下:首先,将菱镁矿置于高温炉内一次煅烧,获得一次轻烧氧化镁粉;其次,将一次轻烧氧化镁粉置于球磨罐中,以去离子水为球磨介质,同时对轻烧氧化镁完成水化和球磨处理,经过干燥处理,获得氢氧化镁粉;然后,将氢氧化镁粉置于高温炉内二次煅烧,再获得二次轻烧氧化镁粉;最后,将二次轻烧氧化镁粉置于放电等离子烧结炉的石墨模具内,在一定温度、时间和压力下进行放电等离子烧结,制得高密度镁砂。The purpose of the present invention is to overcome the shortcomings of the above-mentioned prior art and provide a method for preparing high-density magnesia by spark plasma sintering of magnesite. The main steps of the method are as follows: firstly, calcine the magnesite in a high-temperature furnace once to obtain a lightly burnt magnesia powder; secondly, place the lightly burnt magnesia powder in a ball milling tank, and use deionized water as the ball mill The medium, at the same time, complete hydration and ball milling of light burned magnesia, and obtain magnesium hydroxide powder after drying treatment; then, the magnesium hydroxide powder is placed in a high-temperature furnace for secondary calcination, and then secondary light burned magnesia powder is obtained ; Finally, the second light-fired magnesia powder is placed in the graphite mold of the spark plasma sintering furnace, and the spark plasma sintering is performed at a certain temperature, time and pressure to obtain high-density magnesia.
为实现上述目的,本发明采用以下技术方案:In order to achieve the above objectives, the present invention adopts the following technical solutions:
一种利用菱镁矿放电等离子烧结制备高密度镁砂的方法,按以下步骤进行:A method for preparing high-density magnesia by spark plasma sintering of magnesite is carried out in the following steps:
步骤1:一次轻烧Step 1: One light burn
将菱镁矿在高温炉内进行煅烧,获得一次轻烧氧化镁粉;Calcining the magnesite in a high-temperature furnace to obtain primary light-burned magnesia powder;
步骤2:水化+湿磨+干燥Step 2: Hydration + Wet Grinding + Drying
(1)将一次轻烧氧化镁粉和去离子水置于球磨罐中进行湿磨,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; (1) Put the lightly burned magnesia powder and deionized water in a ball mill tank for wet grinding, and run at a speed of 200~300r·min -1 for 10~15 hours in one direction, and complete hydration and wet grinding treatment at the same time to form a ball mill After slurry
(2)将球磨后料浆干燥,得到氢氧化镁粉;(2) Dry the slurry after ball milling to obtain magnesium hydroxide powder;
步骤3:二次轻烧Step 3: Second light burn
将氢氧化镁粉进行二次煅烧,获得二次轻烧氧化镁粉;The magnesium hydroxide powder is calcined twice to obtain the second lightly burned magnesium oxide powder;
步骤4:放电等离子烧结Step 4: Spark plasma sintering
将二次轻烧氧化镁粉置于放电等离子烧结炉的石墨模具中,烧结,获得高密度镁砂,其中,所述的烧结压力为50~100MPa,烧结温度为1350~1550℃,烧结保温时间为10~30min。Place the secondary light-burned magnesia powder in a graphite mold in a spark plasma sintering furnace and sinter to obtain high-density magnesia, wherein the sintering pressure is 50-100 MPa, the sintering temperature is 1350-1550°C, and the sintering holding time For 10 to 30 minutes.
所述的步骤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。In the step 1, the high-temperature furnace is one of a shaft kiln, a boiling furnace, and a suspension furnace; the calcination temperature is 800 to 900° C., and the calcination time is 2 to 4 hours.
所述的步骤2(1)中,所述的去离子水的与一次轻烧氧化镁粉按液体积与固体质量比为(3~4):1添加,单位ml:g;所述的球磨采用真空球磨罐和ZrO 2磨球。 In the step 2(1), the deionized water and the primary lightly burned magnesia powder are added at a ratio of liquid volume to solid mass of (3~4):1, unit ml:g; the ball mill Use vacuum ball milling tank and ZrO 2 milling ball.
所述的步骤2(2)中,干燥温度为100~120℃,干燥时间为20~24h。In the step 2(2), the drying temperature is 100-120°C, and the drying time is 20-24h.
所述的步骤3中,二次煅烧操作在高温炉中进行,所述的二次轻烧氧化镁粉比一次轻烧氧化镁粉粒度更细。In the step 3, the secondary calcination operation is performed in a high-temperature furnace, and the secondary lightly burned magnesia powder has a finer particle size than the primary lightly burned magnesia powder.
所述的步骤3中,所述高温炉为竖窑、沸腾炉、悬浮炉中的一种;所述的高温炉的煅烧温度为750~850℃,煅烧时间为2~4h。In the step 3, the high temperature furnace is one of a shaft kiln, a boiling furnace, and a suspension furnace; the calcination temperature of the high temperature furnace is 750-850°C, and the calcination time is 2 to 4 hours.
所述的步骤4中,制备的高密度镁砂中氧化镁含量大于97.5%。In the step 4, the magnesium oxide content in the prepared high-density magnesia is greater than 97.5%.
所述的步骤4中,制备的高密度镁砂体积密度为3.52~3.56g·cm -3In the step 4, the volume density of the prepared high-density magnesia is 3.52~3.56 g·cm -3 .
本发明的有益效果:The beneficial effects of the present invention:
1.本发明的利用菱镁矿放电等离子烧结制备高密度镁砂的方法实现了菱镁矿的高附加值利用,采用放电等离子烧结升温快、保温短,大大降低了生产成本,而且易制得高密度的镁砂,有利于高附加值镁质材料的发展。1. The method of the present invention for preparing high-density magnesite by spark plasma sintering of magnesite realizes the utilization of high added value of magnesite. The use of spark plasma sintering has fast temperature rise and short heat preservation, greatly reduces production costs, and is easy to prepare High-density magnesia is conducive to the development of high value-added magnesia materials.
2.本发明的利用菱镁矿放电等离子烧结制备高密度镁砂的方法操作简单易行。2. The method of the present invention for preparing high-density magnesia by spark plasma sintering of magnesite is simple and easy to operate.
3.本发明的利用菱镁矿放电等离子烧结制备高密度镁砂的方法,采用放电等离子烧结技术,在加压中烧结,不仅缩短了烧结时间,而且有利于高密度镁砂的制备。3. The method of the present invention for preparing high-density magnesia by spark plasma sintering of magnesite adopts spark plasma sintering technology and sintering under pressure, which not only shortens the sintering time, but also facilitates the preparation of high-density magnesia.
附图说明:Description of the drawings:
图1是本发明的利用菱镁矿放电等离子烧结制备高密度镁砂的方法工艺流程图。Fig. 1 is a process flow diagram of the method for preparing high-density magnesia by spark plasma sintering of magnesite according to the present invention.
具体实施方式:detailed description:
下面结合实施例对本发明作进一步的详细说明。The present invention will be further described in detail below in conjunction with the embodiments.
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。 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.
实施例1Example 1
一种利用菱镁矿放电等离子烧结制备高密度镁砂的方法,其工艺流程图如图1所示,按以下步骤进行:A method for preparing high-density magnesia by spark plasma sintering of magnesite. The process flow chart is shown in Figure 1, and it is carried out according to the following steps:
步骤1:一次轻烧Step 1: One light burn
将菱镁矿置于800℃竖窑中煅烧2h,获得一次轻烧氧化镁粉;The magnesite is calcined in a shaft kiln at 800°C for 2 hours to obtain a lightly burned magnesia powder;
步骤2:水化+湿磨+干燥Step 2: Hydration + Wet Grinding + Drying
(1)将1000g的一次轻烧氧化镁粉和3倍体积分数,即3000ml的去离子水置于球磨罐中,以200r·min -1转速单向运行10h,同时完成水化和湿磨处理; (1) Put 1000g of lightly burned magnesia powder and 3 times the volume fraction, that is, 3000ml of deionized water in a ball milling tank, and run at a speed of 200r·min -1 for 10 hours in one direction, and complete hydration and wet grinding at the same time. ;
(2)将球磨后料浆在100℃下干燥24h,得到氢氧化镁粉;(2) Dry the ball milled slurry at 100°C for 24 hours to obtain magnesium hydroxide powder;
步骤3:二次轻烧Step 3: Second light burn
将获得的氢氧化镁粉置于750℃竖窑中煅烧4h,获得二次轻烧氧化镁粉。The obtained magnesium hydroxide powder is calcined in a 750°C shaft kiln for 4 hours to obtain secondary lightly burned magnesium oxide powder.
步骤4:放电等离子烧结Step 4: Spark plasma sintering
将二次轻烧氧化镁粉置于放电等离子烧结炉的石墨模具中,施加100MPa的压力,在1350℃的烧结温度下保温20min,制备得到高密度的镁砂。Place the secondary light-burned magnesia powder in a graphite mold of a spark plasma sintering furnace, apply a pressure of 100 MPa, and keep the temperature at a sintering temperature of 1350° C. for 20 minutes to prepare high-density magnesia.
经检测,所得镁砂的体积密度为3.52g·cm -3,镁砂中氧化镁含量大于97.5%,且氧化镁晶粒发育良好。 After testing, the obtained magnesia has a bulk density of 3.52 g·cm -3 , the content of magnesium oxide in the magnesia is greater than 97.5%, and the magnesium oxide crystal grains are well developed.
实施例2Example 2
一种利用菱镁矿放电等离子烧结制备高密度镁砂的方法,按以下步骤进行:A method for preparing high-density magnesia by spark plasma sintering of magnesite is carried out in the following steps:
步骤1:一次轻烧Step 1: One light burn
将菱镁矿置于850℃竖窑中煅烧2h,获得一次轻烧氧化镁粉;The magnesite is calcined in a shaft kiln at 850°C for 2 hours to obtain a lightly burned magnesia powder;
步骤2:水化+湿磨+干燥Step 2: Hydration + Wet Grinding + Drying
(1)将1000g的一次轻烧氧化镁粉和3倍体积分数,即3000ml的去离子水置于球磨罐中,以300r·min -1转速单向运行10h,同时完成水化和湿磨处理; (1) Put 1000g of lightly burned magnesia powder and 3 times the volume fraction, that is, 3000ml of deionized water in a ball milling tank, and run at 300r·min -1 for 10 hours in one direction, and complete the hydration and wet grinding treatment at the same time. ;
(2)将球磨后料浆在120℃下干燥20h,得到氢氧化镁粉;(2) Dry the ball milled slurry at 120°C for 20 hours to obtain magnesium hydroxide powder;
步骤3:二次轻烧Step 3: Second light burn
将氢氧化镁粉置于800℃竖窑中煅烧2h,获得二次轻烧氧化镁粉。The magnesium hydroxide powder was calcined in a shaft kiln at 800°C for 2 hours to obtain secondary lightly burned magnesium oxide powder.
步骤4:放电等离子烧结Step 4: Spark plasma sintering
将二次轻烧氧化镁粉置于放电等离子烧结炉的石墨模具中,施加50MPa的压力,在1400℃的烧结温度下保温20min,制备得到高密度的镁砂。Place the secondary light-burned magnesia powder in a graphite mold of a spark plasma sintering furnace, apply a pressure of 50 MPa, and keep the temperature for 20 minutes at a sintering temperature of 1400° C. to prepare high-density magnesia.
经检测,所得镁砂的体积密度为3.52g·cm -3,镁砂中氧化镁含量大于97.5%,且氧化镁晶粒发育良好。 After testing, the obtained magnesia has a bulk density of 3.52 g·cm -3 , the content of magnesium oxide in the magnesia is greater than 97.5%, and the magnesium oxide crystal grains are well developed.
实施例3Example 3
一种利用菱镁矿放电等离子烧结制备高密度镁砂的方法,按以下步骤进行:A method for preparing high-density magnesia by spark plasma sintering of magnesite is carried out in the following steps:
步骤1:一次轻烧Step 1: One light burn
将菱镁矿置于900℃沸腾炉中煅烧2h,获得轻烧氧化镁粉;The magnesite is calcined in a boiling furnace at 900°C for 2 hours to obtain light burnt magnesia powder;
步骤2:水化+湿磨+干燥Step 2: Hydration + Wet Grinding + Drying
(1)将1000g的一次轻烧氧化镁粉和3倍体积分数,即3000ml的去离子水置于球磨罐中,以300r·min -1转速单向运行15h; (1) Put 1000g of lightly burned magnesium oxide powder and 3 times the volume fraction, that is, 3000ml of deionized water in a ball milling tank, and run at 300r·min -1 for 15h in one direction;
(2)将球磨后料浆在120℃下干燥24h,得到氢氧化镁粉;(2) Dry the ball milled slurry at 120°C for 24 hours to obtain magnesium hydroxide powder;
步骤3:二次轻烧Step 3: Second light burn
将氢氧化镁粉置于850℃沸腾炉中煅烧3h,获得二次轻烧氧化镁粉。The magnesium hydroxide powder was calcined in a boiling furnace at 850° C. for 3 hours to obtain secondary lightly burned magnesium oxide powder.
步骤4:放电等离子烧结Step 4: Spark plasma sintering
将二次轻烧氧化镁粉置于放电等离子烧结炉中的石墨坩埚中,施加50MPa的压力,在1550℃的烧结温度下保温10min,制备得到高密度的镁砂。Place the secondary lightly burned magnesia powder in a graphite crucible in a spark plasma sintering furnace, apply a pressure of 50 MPa, and hold the sintering temperature at 1550° C. for 10 minutes to prepare high-density magnesia.
经检测,所得镁砂的体积密度为3.54g·cm -3,镁砂中氧化镁含量大于97.5%,且氧化镁晶粒发育良好。 After testing, the obtained magnesia has a bulk density of 3.54 g·cm -3 , the content of magnesium oxide in the magnesia is greater than 97.5%, and the magnesium oxide crystal grains are well developed.
实施例4Example 4
一种利用菱镁矿放电等离子烧结制备高密度镁砂的方法,按以下步骤进行:A method for preparing high-density magnesia by spark plasma sintering of magnesite is carried out in the following steps:
步骤1:一次轻烧Step 1: One light burn
将菱镁矿置于850℃悬浮炉中煅烧2h,获得一次轻烧氧化镁粉;Place the magnesite in a suspension furnace at 850°C for 2 hours to obtain a lightly burned magnesium oxide powder;
步骤2:水化+湿磨+干燥Step 2: Hydration + Wet Grinding + Drying
(1)将1000g的一次轻烧氧化镁粉和4倍体积分数,即4000ml的去离子水置于球磨罐中,以300r·min -1转速单向运行15h; (1) Put 1000g of lightly burned magnesium oxide powder and 4 times the volume fraction, that is, 4000ml of deionized water in a ball milling tank, and run it in one direction at 300r·min -1 for 15h;
(2)将球磨后料浆在120℃下干燥24h,得到氢氧化镁粉;(2) Dry the ball milled slurry at 120°C for 24 hours to obtain magnesium hydroxide powder;
步骤3:二次轻烧Step 3: Second light burn
将氢氧化镁粉置于800℃悬浮炉中煅烧2h,获得二次轻烧氧化镁粉。The magnesium hydroxide powder was calcined in a 800°C suspension furnace for 2 hours to obtain secondary lightly burned magnesium oxide powder.
步骤4:放电等离子烧结Step 4: Spark plasma sintering
将二次轻烧氧化镁粉置于放电等离子烧结炉的石墨模具中,施加100MPa的压力,在1550℃的烧结温度下保温30min,制备得到高密度的镁砂。Place the secondary light-burned magnesia powder in a graphite mold of a spark plasma sintering furnace, apply a pressure of 100 MPa, and hold the sintering temperature at 1550° C. for 30 minutes to prepare high-density magnesia.
经检测,所得镁砂的体积密度为3.56g·cm -3,镁砂中氧化镁含量大于97.5%。 After testing, the bulk density of the obtained magnesia is 3.56 g·cm -3 , and the content of magnesium oxide in the magnesia is greater than 97.5%.

Claims (7)

  1. 一种利用菱镁矿放电等离子烧结制备高密度镁砂的方法,其特征在于,按以下步骤进行:A method for preparing high-density magnesia by spark plasma sintering of magnesite is characterized in that it is carried out in the following steps:
    步骤1:一次轻烧Step 1: One light burn
    将菱镁矿在高温炉内进行煅烧,获得一次轻烧氧化镁粉;Calcining the magnesite in a high-temperature furnace to obtain primary light-burned magnesia powder;
    步骤2:水化+湿磨+干燥Step 2: Hydration + Wet Grinding + Drying
    (1)将一次轻烧氧化镁粉和去离子水置于球磨罐中进行湿磨,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; (1) Put the lightly burned magnesia powder and deionized water in a ball mill tank for wet grinding, and run at a speed of 200~300r·min -1 for 10~15 hours in one direction, and complete hydration and wet grinding treatment at the same time to form a ball mill After slurry
    (2)将球磨后料浆干燥,得到氢氧化镁粉;(2) Dry the slurry after ball milling to obtain magnesium hydroxide powder;
    步骤3:二次轻烧Step 3: Second light burn
    将氢氧化镁粉进行二次煅烧,获得二次轻烧氧化镁粉;The magnesium hydroxide powder is calcined twice to obtain the second lightly burned magnesium oxide powder;
    步骤4:放电等离子烧结Step 4: Spark plasma sintering
    将二次轻烧氧化镁粉置于放电等离子烧结炉的石墨模具中,烧结,获得高密度镁砂,其中,所述的烧结压力为50~100MPa,烧结温度为1350~1550℃,烧结保温时间为10~30min。Place the secondary light-burned magnesia powder in a graphite mold in a spark plasma sintering furnace and sinter to obtain high-density magnesia, wherein the sintering pressure is 50-100 MPa, the sintering temperature is 1350-1550°C, and the sintering holding time For 10 to 30 minutes.
  2. 根据权利要求1所述的一种利用菱镁矿放电等离子烧结制备高密度镁砂的方法,其特征在于,所述的步骤1中,所述的高温炉为竖窑、沸腾炉、悬浮炉中的一种,所述的烧温度为800~900℃,煅烧时间为2~4h。The method for preparing high-density magnesia by spark plasma sintering of magnesite according to claim 1, characterized in that, in the step 1, the high-temperature furnace is a shaft kiln, a boiling furnace, or a suspension furnace. One, the calcination temperature is 800-900°C, and the calcination time is 2 to 4 hours.
  3. 根据权利要求1所述的一种利用菱镁矿放电等离子烧结制备高密度镁砂的方法,其特征在于,所述的步骤2(1)中,所述的去离子水的与一次轻烧氧化镁粉按液体积与固体质量比为(3~4):1添加,单位ml:g;所述的球磨采用真空球磨罐和ZrO 2磨球。 The method for preparing high-density magnesia by spark plasma sintering of magnesite according to claim 1, characterized in that, in the step 2 (1), the deionized water is combined with a light burn oxidation Magnesium powder is added according to the ratio of liquid volume to solid mass of (3~4):1, and the unit is ml:g; the ball mill adopts a vacuum ball mill tank and a ZrO 2 ball mill.
  4. 根据权利要求1所述的一种利用菱镁矿放电等离子烧结制备高密度镁砂的方法,其特征在于,所述的步骤2(2)中,干燥温度为100~120℃,干燥时间为20~24h。The method for preparing high-density magnesia by spark plasma sintering of magnesite according to claim 1, characterized in that, in the step 2 (2), the drying temperature is 100-120°C, and the drying time is 20°C. ~24h.
  5. 根据权利要求1所述的一种利用菱镁矿放电等离子烧结制备高密度镁砂的方法,其特征在于,所述的步骤3中,二次煅烧温度为750~850℃,煅烧时间为2~4h。The method for preparing high-density magnesia by spark plasma sintering of magnesite according to claim 1, characterized in that, in said step 3, the secondary calcination temperature is 750-850°C, and the calcination time is 2~ 4h.
  6. 根据权利要求1所述的一种利用菱镁矿放电等离子烧结制备高密度镁砂的方法,其特征在于,所述的步骤4中,制备的高密度镁砂中氧化镁含量大于97.5%。The method for preparing high-density magnesia by spark plasma sintering of magnesite according to claim 1, wherein in said step 4, the magnesium oxide content in the prepared high-density magnesia is greater than 97.5%.
  7. 根据权利要求1所述的一种利用菱镁矿放电等离子烧结制备高密度镁砂的方法,其特征在于,所述的步骤4中,制备的高密度镁砂体积密度为3.52~3.56g·cm -3The method for preparing high-density magnesia by spark plasma sintering of magnesite according to claim 1, wherein in said step 4, the bulk density of the prepared high-density magnesia is 3.52~3.56g·cm -3 .
PCT/CN2019/076094 2019-02-01 2019-02-26 Method for preparing high-density magnesia from magnesite by means of spark plasma sintering WO2020155243A1 (en)

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CN110498621B (en) * 2019-09-02 2021-11-05 于景坤 Preparation method of superfine purified concentrate powder sintered magnesia
CN113880463B (en) * 2021-11-04 2022-08-09 福州大学 Method for producing magnesium oxide for magnesium phosphate cement by radio frequency plasma technology
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