CN108793779A - A kind of preparation method of activity magnesia - Google Patents

A kind of preparation method of activity magnesia Download PDF

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Publication number
CN108793779A
CN108793779A CN201810746060.6A CN201810746060A CN108793779A CN 108793779 A CN108793779 A CN 108793779A CN 201810746060 A CN201810746060 A CN 201810746060A CN 108793779 A CN108793779 A CN 108793779A
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CN
China
Prior art keywords
added
minutes
magnesia
preparation
mixture
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Application number
CN201810746060.6A
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Chinese (zh)
Inventor
张寒
李静捷
赵惠忠
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Wuhan University of Science and Engineering WUSE
Wuhan University of Science and Technology WHUST
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Wuhan University of Science and Engineering WUSE
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Application filed by Wuhan University of Science and Engineering WUSE filed Critical Wuhan University of Science and Engineering WUSE
Priority to CN201810746060.6A priority Critical patent/CN108793779A/en
Publication of CN108793779A publication Critical patent/CN108793779A/en
Withdrawn legal-status Critical Current

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Classifications

    • 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

Abstract

The present invention relates to a kind of preparation methods of active magnesia.Its technical solution is:Magnisite is milled to granularity≤0.1mm, obtains ball milling material;The ball milling material is placed in Muffle furnace, is calcined 30~40 minutes under the conditions of 800~850 DEG C, calcining material is obtained;The water for accounting for 45~50wt% of the calcining material is added into the calcining material, mixes 5~8 minutes, obtains mixture;The hydrofluoric acid solution for accounting for the 3~4wt% of mixture is added into the mixture, mixes 8~10 minutes, stores 3~5 hours under room temperature, obtain presoma material;The presoma material is added in Muffle furnace, is calcined 20~30 minutes under the conditions of 1260~1300 DEG C, furnace cooling is to get active magnesia.Present invention process is simple, and prepared active purity of magnesite is high, reactivity is good and sintering character is excellent.

Description

A kind of preparation method of activity magnesia
Technical field
The invention belongs to magnesia technical fields.More particularly to a kind of preparation method of active magnesia.
Background technology
Magnesia be using MgO as main chemical compositions, with the synthesis material that periclase is main object phase, for magnesia brick, magnesium carbon The preparation of the basic refractories such as brick and magnesia-calcium brick.The chemism of magnesia is higher, prepared basic refractory agglutinating property It can be better.Therefore, the activity of magnesia directly determines the comprehensive performance of basic refractory and correlated product.
Currently, active magnesia is made mainly with magnesite (or clout after magnesite flotation) for raw material after light-burned activation , its shortcoming is that impurity composition (such as SiO in magnesite (or clout after magnesite flotation)2、Al2O3Deng) easily with MgO it is anti- The compounds such as olivine or spinelle should be formed, the content of free MgO is on the one hand reduced, on the other hand also affects magnesia Reactivity reduces the sintering character of magnesia.
Invention content
The purpose of the present invention is to provide the preparation methods of active magnesia a kind of simple for process and at low cost.Use this method Prepared active purity of magnesite is high, activity is good and sintering character is excellent.
To achieve the above object, the technical solution adopted by the present invention comprises the concrete steps that:
Magnisite is added in ball mill the first step, is milled to granularity≤0.1mm, obtains ball milling material.
The ball milling material is placed in Muffle furnace by second step, is calcined 30~40 minutes, is obtained under the conditions of 800~850 DEG C Calcining material.
The water for accounting for 45~50wt% of the calcining material is added into the calcining material for third step, mixes 5~8 minutes, obtains Mixture.
The hydrofluoric acid solution for accounting for the 3~4wt% of mixture is added into the mixture for 4th step, mixes 8~10 points Clock is stored 3~5 hours, obtains presoma material under room temperature.
The presoma material is added in Muffle furnace 5th step, is calcined 20~30 minutes under the conditions of 1260~1300 DEG C, Activity magnesia is made in furnace cooling.
The main chemical compositions of the magnisite are:MgCO3Content >=95wt%;SiO2Content≤2wt%.
The hydrofluoric acid solution is that chemistry is pure;0.2~0.5mol/L of concentration of the hydrofluoric acid solution.
Due to the adoption of the above technical scheme, the present invention has the positive effect that compared with prior art:
1, in preparation process of the present invention only will after magnesite ball milling calcine, mix and secondary clacining, be not necessarily to special processing Equipment and complicated preparation method, preparation process is simple and production cost is low.
2, the present invention first will be digested after magnesite calcining and activating, cleaned using hydrofluoric acid and introduce Fluorine source, improve magnesia Purity simultaneously promotes periclase grain crystalline to be nucleated, and improves the reactivity of magnesia, sintering character is excellent.
Active magnesia prepared by the present invention is after testing:Free content of MgO is 98.5~99.0wt%, specific surface area 20 ~25m2/g。
Therefore, the present invention has the characteristics that simple for process low with production cost;Prepared active purity of magnesite is high, reacts Activity is good and sintering character is excellent.
Specific implementation mode
The invention will be further described With reference to embodiment, not to the limitation of its protection domain.
It is first that the technical parameter Unify legislation of material involved by present embodiment is as follows to avoid repeating, embodiment In repeat no more:
The main chemical compositions of the magnisite are:MgCO3Content >=95wt%;SiO2Content≤2wt%.
The hydrofluoric acid solution is that chemistry is pure;0.2~0.5mol/L of concentration of the hydrofluoric acid solution.
Embodiment 1
A kind of preparation method of activity magnesia.Preparation method described in the present embodiment comprises the concrete steps that:
Magnisite is added in ball mill the first step, is milled to granularity≤0.1mm, obtains ball milling material.
The ball milling material is placed in Muffle furnace by second step, is calcined 30~40 minutes, is obtained under the conditions of 800~820 DEG C Calcining material.
The water for accounting for 45~47wt% of the calcining material is added into the calcining material for third step, mixes 5~8 minutes, obtains Mixture.
The hydrofluoric acid solution for accounting for the 3~4wt% of mixture is added into the mixture for 4th step, mixes 8~10 points Clock is stored 3~5 hours, obtains presoma material under room temperature.
The presoma material is added in Muffle furnace 5th step, is calcined 20~30 minutes under the conditions of 1260~1276 DEG C, Activity magnesia is made in furnace cooling.
Activity magnesia manufactured in the present embodiment is after testing:Free content of MgO is 98.5~98.7wt%, specific surface area 20 ~22m2/g。
Embodiment 2
A kind of preparation method of activity magnesia.Preparation method described in the present embodiment comprises the concrete steps that:
Magnisite is added in ball mill the first step, is milled to granularity≤0.1mm, obtains ball milling material.
The ball milling material is placed in Muffle furnace by second step, is calcined 30~40 minutes, is obtained under the conditions of 810~830 DEG C Calcining material.
The water for accounting for 46~48wt% of the calcining material is added into the calcining material for third step, mixes 5~8 minutes, obtains Mixture.
The hydrofluoric acid solution for accounting for the 3~4wt% of mixture is added into the mixture for 4th step, mixes 8~10 points Clock is stored 3~5 hours, obtains presoma material under room temperature.
The presoma material is added in Muffle furnace 5th step, is calcined 20~30 minutes under the conditions of 1268~1284 DEG C, Activity magnesia is made in furnace cooling.
Activity magnesia manufactured in the present embodiment is after testing:Free content of MgO is 98.6~98.8wt%, specific surface area 21 ~23m2/g。
Embodiment 3
A kind of preparation method of activity magnesia.Preparation method described in the present embodiment comprises the concrete steps that:
Magnisite is added in ball mill the first step, is milled to granularity≤0.1mm, obtains ball milling material.
The ball milling material is placed in Muffle furnace by second step, is calcined 30~40 minutes, is obtained under the conditions of 820~840 DEG C Calcining material.
The water for accounting for 47~49wt% of the calcining material is added into the calcining material for third step, mixes 5~8 minutes, obtains Mixture.
The hydrofluoric acid solution for accounting for the 3~4wt% of mixture is added into the mixture for 4th step, mixes 8~10 points Clock is stored 3~5 hours, obtains presoma material under room temperature.
The presoma material is added in Muffle furnace 5th step, is calcined 20~30 minutes under the conditions of 1276~1292 DEG C, Activity magnesia is made in furnace cooling.
Activity magnesia manufactured in the present embodiment is after testing:Free content of MgO is 98.7~98.9wt%, specific surface area 22 ~24m2/g。
Embodiment 4
A kind of preparation method of activity magnesia.Preparation method described in the present embodiment comprises the concrete steps that:
Magnisite is added in ball mill the first step, is milled to granularity≤0.1mm, obtains ball milling material.
The ball milling material is placed in Muffle furnace by second step, is calcined 30~40 minutes, is obtained under the conditions of 830~850 DEG C Calcining material.
The water for accounting for 48~50wt% of the calcining material is added into the calcining material for third step, mixes 5~8 minutes, obtains Mixture.
The hydrofluoric acid solution for accounting for the 3~4wt% of mixture is added into the mixture for 4th step, mixes 8~10 points Clock is stored 3~5 hours, obtains presoma material under room temperature.
The presoma material is added in Muffle furnace 5th step, is calcined 20~30 minutes under the conditions of 1284~1300 DEG C, Activity magnesia is made in furnace cooling.
Activity magnesia manufactured in the present embodiment is after testing:Free content of MgO is 98.8~99.0wt%, specific surface area 23 ~25m2/g。
Present embodiment has the positive effect that compared with prior art:
1, in present embodiment preparation process only will after magnesite ball milling calcine, mix and secondary clacining, without spy Different processing equipment and complicated preparation method, preparation process is simple and production cost is low.
2, present embodiment first will be digested after magnesite calcining and activating, cleaned using hydrofluoric acid and introduce Fluorine source, be carried The purity of high magnesia simultaneously promotes periclase grain crystalline to be nucleated, and improves the reactivity of magnesia, sintering character is excellent.
Active magnesia prepared by present embodiment is after testing:Free content of MgO is 98.5~99.0wt%, compares table Area is 20~25m2/g。
Therefore, present embodiment has the characteristics that simple for process low with production cost;Prepared active magnesia is pure Degree is high, reactivity is good and sintering character is excellent.

Claims (3)

1. a kind of preparation method of activity magnesia, it is characterised in that the preparation method comprises the concrete steps that:
Magnisite is added in ball mill the first step, is milled to granularity≤0.1mm, obtains ball milling material;
The ball milling material is placed in Muffle furnace by second step, is calcined 30~40 minutes, is calcined under the conditions of 800~850 DEG C Material;
The water for accounting for 45~50wt% of the calcining material is added into the calcining material for third step, mixes 5~8 minutes, is mixed Material;
The hydrofluoric acid solution for accounting for the 3~4wt% of mixture is added into the mixture for 4th step, mixes 8~10 minutes, It stores 3~5 hours under room temperature, obtains presoma material;
The presoma material is added in Muffle furnace 5th step, is calcined 20~30 minutes under the conditions of 1260~1300 DEG C, with stove It is cooling, activity magnesia is made.
2. the preparation method of activity magnesia according to claim 1, it is characterised in that mainization of the magnisite Studying point is:MgCO3Content >=95wt%;SiO2Content≤2wt%.
3. the preparation method of activity magnesia according to claim 1, it is characterised in that the hydrofluoric acid solution is that chemistry is pure; 0.2~0.5mol/L of concentration of the hydrofluoric acid solution.
CN201810746060.6A 2018-07-09 2018-07-09 A kind of preparation method of activity magnesia Withdrawn CN108793779A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111925191A (en) * 2020-07-13 2020-11-13 辽宁东和新材料股份有限公司 Method for producing high-density high-purity sintered magnesia by using low-grade magnesite

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3276882A (en) * 1961-04-22 1966-10-04 Dolomitwerke Gmbh Highly hydration stable sinters of dolomite, magnesite, lime or the like
CN1057631A (en) * 1991-06-29 1992-01-08 叶青柏 The production method of electro-smelting magnesite with low silicon content
CN1792940A (en) * 2005-11-18 2006-06-28 东北大学 Process for prepering active magnesium oxide
CN103204641A (en) * 2012-01-16 2013-07-17 东北大学 Purification method for low-grade magnesite via hydration
CN106565115A (en) * 2016-11-17 2017-04-19 营口镁质材料研究院有限公司 Method for roguing and purifying low-grade magnesite

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3276882A (en) * 1961-04-22 1966-10-04 Dolomitwerke Gmbh Highly hydration stable sinters of dolomite, magnesite, lime or the like
CN1057631A (en) * 1991-06-29 1992-01-08 叶青柏 The production method of electro-smelting magnesite with low silicon content
CN1792940A (en) * 2005-11-18 2006-06-28 东北大学 Process for prepering active magnesium oxide
CN103204641A (en) * 2012-01-16 2013-07-17 东北大学 Purification method for low-grade magnesite via hydration
CN106565115A (en) * 2016-11-17 2017-04-19 营口镁质材料研究院有限公司 Method for roguing and purifying low-grade magnesite

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111925191A (en) * 2020-07-13 2020-11-13 辽宁东和新材料股份有限公司 Method for producing high-density high-purity sintered magnesia by using low-grade magnesite

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Application publication date: 20181113