CN101585083B - Inactivating magnesium desulfurizing agent and preparation method thereof - Google Patents

Inactivating magnesium desulfurizing agent and preparation method thereof Download PDF

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Publication number
CN101585083B
CN101585083B CN2009100533151A CN200910053315A CN101585083B CN 101585083 B CN101585083 B CN 101585083B CN 2009100533151 A CN2009100533151 A CN 2009100533151A CN 200910053315 A CN200910053315 A CN 200910053315A CN 101585083 B CN101585083 B CN 101585083B
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magnesium
desulfurizing agent
inactivating
preparation
lanthanum
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CN2009100533151A
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CN101585083A (en
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万见峰
陈文�
尤磊
马晓春
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Shanghai Jiaotong University
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Shanghai Jiaotong University
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Abstract

The invention provides an inactivating magnesium desulfurizing agent for the field of smelting technique and a preparation method thereof. The desulfurizing agent includes granulated magnesium and passivation layer, wherein the passivation layer packs granulated magnesium inward; and the components of desulfurizing agent and weight percentages are as follows: magnesium 93-96%, lanthanum 0.50-1.50%, cerium 0.35-1.05%, praseodymium 0.12-0.36%, neodymium 0.04-0.08%, samarium 0.01-0.03%, and the rest is impurity; the preparation method of the desulfurizing agent includes the following steps: solid-dissolving rare-earth into pure magnesium for obtaining granulated magnesium; formulating inactivating liquid using acetic acid and lanthanum cerium chloride, inactivating granulated magnesium using inactivating liquid for forming passivation layer; drying inactivated granulated magnesium, obtaining inactivating magnesium desulfurizing agent. The preparation method provided by the invention has the characteristics of simple technique and high productivity effect, uniformly firm of prepared desulfurizing agent passivation layer and long flame-retardant time.

Description

Inactivating magnesium desulfurizing agent and preparation method thereof
Technical field
The present invention relates to a kind of desulfurizing agent that is used for technical field of smelting and preparation method thereof, be specifically related to a kind of inactivating magnesium desulfurizing agent and preparation method thereof.
Background technology
At present engineerings such as auto industry, oil exploitation, large ship are more and more higher to the requirement of steel product quality, the countries in the world steel and iron industry all hardy by reduce in the steel impurity particularly the approach of sulfur content improve steel product quality.The external desulfurization of hot metal of implementing as converter smelting high-quality steel grade or alloy steel grade generally needs dark desulfurization that sulphur is taken off the level to " two zero ", promptly less than 0.005%~0.001%.Magnesium granules is used for the steel desulfurization, and excellent performance, desulfuration efficiency are better than far away with former CaO and CaC 2, can carry out deep desulfuration, S content is reduced to below 0.002%; The granularity of used magnesium granules between 0.1~0.9mm, duration of fire resistance in the time of 1000 ℃ 〉=15 second, ignition point is more than 770 ℃, such magnesium granules could satisfy the desulfurization requirement of present high-quality steel.But because the latent heat of magnesium is low, no matter be to cut magnesium granules or cover salt magnesium grain, its duration of fire resistance is short, and ignition point is low, all can not satisfy the requirement of steel desulfurization well; When spraying in the molten steel with spray gun, very easily, can't be deep into molten steel inside in the surface gasification, finally cause desulfurized effect undesirable.In order to satisfy the requirement of steel desulfurization, the development of new inactivating magnesium desulfurizing agent is imperative.
The Chinese patent publication number is the patent of invention of CN1354057, applies one deck hydrophobic layer and one deck flame-retardant layer successively on the surface of metal magnesium powder; Hydrophobic layer is mixtures such as rosin, pitch, resin, and flame-retardant layer is CaO, CaCO 3, MgO, MgCO 3, Al 2O 3, SiO 2Deng compound, its greatest problem is the band quantity of slag that its hydrophobic layer will increase molten iron; Chinese patent publication number CN2378399 discloses and has constituted the epidermis material by particle magnesium, anti-oxidant flame-retardant layer, boron oxide or calcium oxide and form the composite bed passivation particle magnesium; The disclosed passivation particle magnesium of Chinese patent publication number CN1485461 is to wrap magnesia or magnesium fluoride pulvis to form anti oxidation layer by the surface at granular metal magnesium, forms after the passivation again; Said method all must increase production cost at particle magnesium surface cover layer, and technological process is increased, and when industrially desulfurized molten steel, molten iron are easily had side effects, and cover layer easily comes off in transit, has influenced the result of use of desulfurizing agent.
The disclosed coating granule magnesium of Chinese patent publication number CN1459510 then is that chloride solution is sprayed on the particle magnesium that rotates in the axe with spray equipment.This method is subjected to the restriction of manufacturing equipment, can't produce in batches.
Summary of the invention
The objective of the invention is to provides a kind of inactivating magnesium desulfurizing agent and preparation method thereof at the deficiencies in the prior art.Preparation method of the present invention has the advantages that technology is simple, production efficiency is high, and the desulfurizing agent passivation layer for preparing is evenly firm, and duration of fire resistance is long.
The present invention realizes by following technical scheme:
The present invention relates to a kind of inactivating magnesium desulfurizing agent, comprise particle magnesium and passivation layer, in wherein passivation layer is wrapped in particle magnesium; The component of desulfurizing agent and percentage by weight are: magnesium: 93~96%, and lanthanum: 0.50~1.50%, cerium: 0.35~1.05%, praseodymium: 0.12~0.36%, neodymium: 0.04~0.08%, samarium: 0.01~0.03%, surplus is an impurity.
The invention still further relates to a kind of method for preparing above-mentioned inactivating magnesium desulfurizing agent, comprise the steps:
Step 1 is solidly soluted into rare earth in the pure magnesium, obtains particle magnesium;
Step 2 with acetic acid and lanthanum-cerium chloride preparation passivating solution, utilizes passivating solution with the passivation of particle magnesium, forms passivation layer;
Step 3, the particle magnesium after the oven dry passivation obtains inactivating magnesium desulfurizing agent.
In the step 2, described passivating solution is specially, and the 1L passivating solution is composed of the following components: lanthanum-cerium chloride 70~90g, and acetic acid 15~25g, surplus is a water.
In the step 2, the weight ratio of passivating solution and particle magnesium is 1: (80~100).
In the step 3, the temperature of described oven dry is 120 ℃, and the time is 40min.
Compared with prior art, the present invention has following beneficial effect: the present invention combines with the surface passivation treatment technology RE alloyed, is about to mishmetal and is solidly soluted in the particle magnesium, to improve the resistance combustion temperature of desulfurizing agent; In passivating solution, adopt the chloride of rare earth, reduce the loss of magnesium metal in the passivating process, also make this novel inactivating magnesium desulfurizing agent can satisfy the requirement of desulfurizing iron well.Preparation method of the present invention has the advantages that technology is simple, production efficiency is high, and the desulfurizing agent passivation layer for preparing is evenly firm, and duration of fire resistance is long.
The specific embodiment
Present embodiment has provided detailed embodiment and process being to implement under the prerequisite with the technical solution of the present invention, but protection scope of the present invention is not limited to following embodiment.The experimental technique of unreceipted actual conditions in the following example, usually according to normal condition, or the condition of advising according to manufacturer.
Embodiment 1
Step 1 is solidly soluted into rare earth in the pure magnesium, obtains particle magnesium; Wherein the weight ratio of magnesium and rare earth is, 97: 3; The component of rare earth and percentage by weight are: lanthanum 50%, cerium 35%, praseodymium 12%, neodymium 2.3%, samarium 0.4%, non-rare earth impurity 0.3%;
Step 2, with acetic acid and lanthanum-cerium chloride preparation passivating solution, the 1L passivating solution is composed of the following components: lanthanum-cerium chloride 70g, acetic acid 15g, surplus is a water; Passivating solution and particle magnesium weight ratio are 1: 80; Utilize passivating solution with the passivation of particle magnesium, form passivation layer;
Step 3,120 ℃ of particle magnesium 40min of drying down after the passivation obtain inactivating magnesium desulfurizing agent.
Each component and percentage by weight thereof are in the inactivating magnesium desulfurizing agent that present embodiment finally obtains: magnesium: 96%, and lanthanum: 1.50%, cerium: 1.05%, praseodymium: 0.36%, neodymium: 0.08%, samarium: 0.03%, surplus is an impurity.
The inactivating magnesium desulfurizing agent outward appearance that present embodiment obtains is silver gray, is shaped as regular spherical, 1000 ℃ of duration of fire resistance 18s, and 640 ℃ of burning-points, particle mean size is 1mm.
Embodiment 2
Step 1 is solidly soluted into rare earth in the pure magnesium, obtains particle magnesium; Wherein the weight ratio of magnesium and rare earth is, 98: 2; The component of rare earth and percentage by weight are: lanthanum 50%, cerium 35%, praseodymium 12%, neodymium 2.3%, samarium 0.4%, non-rare earth impurity 0.3%;
Step 2, with acetic acid and lanthanum-cerium chloride preparation passivating solution, the 1L passivating solution is composed of the following components: lanthanum-cerium chloride 90g, acetic acid 20g, surplus is a water; Passivating solution and particle magnesium weight ratio are 1: 90; Utilize passivating solution with the passivation of particle magnesium, form passivation layer;
Step 3,120 ℃ of particle magnesium 40min of drying down after the passivation obtain inactivating magnesium desulfurizing agent.
Each component and percentage by weight thereof are in the inactivating magnesium desulfurizing agent that present embodiment obtains: magnesium: 93%, and lanthanum: 1%, cerium: 0.95%, praseodymium: 0.24%, neodymium: 0.07%, samarium: 0.01%, surplus is an impurity.
The inactivating magnesium desulfurizing agent outward appearance that present embodiment obtains is silver gray, is shaped as regular spherical, 1000 ℃ of duration of fire resistance 21s, and 640 ℃ of burning-points, particle mean size is 1mm.
Embodiment 3
Step 1 is solidly soluted into rare earth in the pure magnesium, obtains particle magnesium; Wherein the weight ratio of magnesium and rare earth is, 99: 1; The component of rare earth and percentage by weight are: lanthanum 50%, cerium 35%, praseodymium 12%, neodymium 2.3%, samarium 0.4%, non-rare earth impurity 0.3%;
Step 2, with acetic acid and lanthanum-cerium chloride preparation passivating solution, the 1L passivating solution is composed of the following components: lanthanum-cerium chloride 80g, acetic acid 25g, surplus is a water; Passivating solution and particle magnesium weight ratio are 1: 100; Utilize passivating solution with the passivation of particle magnesium, form passivation layer;
Step 3,120 ℃ of particle magnesium 40min of drying down after the passivation obtain inactivating magnesium desulfurizing agent.
Each component and percentage by weight thereof are in the inactivating magnesium desulfurizing agent that present embodiment obtains: magnesium: 94.5%, and lanthanum: 0.75%, cerium: 0.55%, praseodymium: 0.12%, neodymium: 0.05%, samarium: 0.02%, surplus is an impurity.
The inactivating magnesium desulfurizing agent outward appearance that present embodiment obtains is silver gray, is shaped as regular spherical, 1000 ℃ of duration of fire resistance 23s, and 640 ℃ of burning-points, particle mean size is 1mm.
Embodiment 4
Step 1 is solidly soluted into rare earth in the pure magnesium, obtains particle magnesium; Wherein the weight ratio of magnesium and rare earth is, 98.5: 1.5; The component of rare earth and percentage by weight are: lanthanum 50%, cerium 35%, praseodymium 12%, neodymium 2.3%, samarium 0.4%, non-rare earth impurity 0.3%;
Step 2, with acetic acid and lanthanum-cerium chloride preparation passivating solution, the 1L passivating solution is composed of the following components: lanthanum-cerium chloride 85g, acetic acid 18g, surplus is a water; Passivating solution and particle magnesium weight ratio are 1: 85; Utilize passivating solution with the passivation of particle magnesium, form passivation layer;
Step 3,120 ℃ of particle magnesium 40min of drying down after the passivation obtain inactivating magnesium desulfurizing agent.
Each component and percentage by weight thereof are in the inactivating magnesium desulfurizing agent that present embodiment obtains: magnesium: 93.8%, and lanthanum: 0.5%, cerium: 0.35%, praseodymium: 0.2%, neodymium: 0.04%, samarium: 0.015%, surplus is an impurity.
The inactivating magnesium desulfurizing agent outward appearance that present embodiment obtains is silver gray, is shaped as regular spherical, 1000 ℃ of duration of fire resistance 18s, and 620 ℃ of burning-points, particle mean size is 1mm.
Embodiment 5
Step 1 is solidly soluted into rare earth in the pure magnesium, obtains particle magnesium; Wherein the weight ratio of magnesium and rare earth is, 97.5: 2.5; The component of rare earth and percentage by weight are: lanthanum 50%, cerium 35%, praseodymium 12%, neodymium 2.3%, samarium 0.4%, non-rare earth impurity 0.3%;
Step 2, with acetic acid and lanthanum-cerium chloride preparation passivating solution, the 1L passivating solution is composed of the following components: lanthanum-cerium chloride 75g, acetic acid 23g, surplus is a water; Passivating solution and particle magnesium weight ratio are 1: 95; Utilize passivating solution with the passivation of particle magnesium, form passivation layer;
Step 3,120 ℃ of particle magnesium 40min of drying down after the passivation obtain inactivating magnesium desulfurizing agent.
Each component and percentage by weight thereof are in the inactivating magnesium desulfurizing agent that present embodiment obtains: magnesium: 95%, and lanthanum: 1.25%, cerium: 0.70%, praseodymium: 0.31%, neodymium: 0.06%, samarium: 0.02%, surplus is an impurity.
The inactivating magnesium desulfurizing agent outward appearance that present embodiment obtains is silver gray, is shaped as regular spherical, 1000 ℃ of duration of fire resistance 18s, and 620 ℃ of burning-points, particle mean size is 1mm.

Claims (5)

1. an inactivating magnesium desulfurizing agent is characterized in that, comprises particle magnesium and passivation layer, in wherein passivation layer is wrapped in particle magnesium; The component of desulfurizing agent and percentage by weight are: magnesium: 93~96%, and lanthanum: 0.50~1.50%, cerium: 0.35~1.05%, praseodymium: 0.12~0.36%, neodymium: 0.04~0.08%, samarium: 0.01~0.03%, surplus is an impurity.
2. the preparation method of an inactivating magnesium desulfurizing agent as claimed in claim 1 is characterized in that, comprises the steps:
Step 1 is solidly soluted into lanthanum, cerium, praseodymium, neodymium, samarium in the pure magnesium, obtains particle magnesium;
Step 2 with acetic acid and lanthanum-cerium chloride preparation passivating solution, utilizes passivating solution with the passivation of particle magnesium, forms passivation layer;
Step 3, the particle magnesium after the oven dry passivation obtains inactivating magnesium desulfurizing agent.
3. preparation method according to claim 2 is characterized in that, in the step 2, described passivating solution is specially, and the 1L passivating solution is composed of the following components: lanthanum-cerium chloride 70~90g, and acetic acid 15~25g, surplus is a water.
4. preparation method according to claim 2 is characterized in that, in the step 2, the weight ratio of passivating solution and particle magnesium is 1: (80~100).
5. preparation method according to claim 2 is characterized in that, in the step 3, the temperature of described oven dry is 120 ℃, and the time is 40min.
CN2009100533151A 2009-06-18 2009-06-18 Inactivating magnesium desulfurizing agent and preparation method thereof Expired - Fee Related CN101585083B (en)

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CN102108431B (en) * 2009-12-24 2013-06-05 营口东邦冶金设备耐材有限公司 Composite-coating granular magnesium desulfurizer
CN112605375A (en) * 2020-11-27 2021-04-06 辽阳钢铁有限公司 High-purity pig iron production system and process
CN113355486A (en) * 2021-05-27 2021-09-07 湛江申翰科技实业有限公司 Composite desulfurizer and preparation method thereof

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