CN108640140B - Preparation method of active calcium oxide sand - Google Patents

Preparation method of active calcium oxide sand Download PDF

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Publication number
CN108640140B
CN108640140B CN201810746736.1A CN201810746736A CN108640140B CN 108640140 B CN108640140 B CN 108640140B CN 201810746736 A CN201810746736 A CN 201810746736A CN 108640140 B CN108640140 B CN 108640140B
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calcium oxide
oxide sand
calcined
calcining
filter material
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CN108640140A (en
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张寒
李静捷
赵惠忠
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Linkou County Yumao Calcium Industry Co ltd
Nanjing Hezhi Technology Co ltd
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Wuhan University of Science and Engineering WUSE
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    • 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
    • C01F11/00—Compounds of calcium, strontium, or barium
    • C01F11/02—Oxides or hydroxides
    • C01F11/04—Oxides or hydroxides by thermal decomposition
    • C01F11/06—Oxides or hydroxides by thermal decomposition of carbonates
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
    • 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
    • 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
    • C01P2006/80—Compositional purity

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Physics & Mathematics (AREA)
  • Thermal Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)

Abstract

The invention relates to a preparation method of active calcium oxide sand. The technical scheme is as follows: mixing and ball-milling the materials according to the mass ratio of natural limestone to fluorite of (100-105) to 1 to obtain a ball grinding material; placing the ball-milled material in a muffle furnace, and calcining for 0.5-1 hour at 950-1000 ℃ to obtain a calcined material; adding water accounting for 55-60 wt% of the calcined material into the calcined material, and standing to obtain a precursor material; adding a hydrofluoric acid solution accounting for 1-5 wt% of the precursor material into the precursor material, stirring, and filtering to obtain a filter material; and drying the filter material at 110-120 ℃, placing the filter material in a muffle furnace, calcining the filter material at 1380-1400 ℃ for 20-30 minutes, and cooling the filter material along with the furnace to obtain the activated calcium oxide sand. The invention has the characteristic of simple process; the prepared active calcium oxide sand has high purity and good crystal grain development.

Description

Preparation method of active calcium oxide sand
Technical Field
The invention belongs to the technical field of calcium oxide sand. In particular to a preparation method of active calcium oxide sand.
Background
The calcium oxide sand has wide source, low cost and high chemical reaction activity (with Al) at high temperature2O3、Fe2O3And SiO2Etc. common oxides can react) and can be widely used as drying agents, impurity removing agents or slag forming agents, etc. in the high-temperature industrial fields of steel, metallurgy, nonferrous metal, etc. Therefore, improving the reactivity of the calcium oxide sand is the primary consideration in preparing the calcium oxide sand.
At present, limestone is mainly used as a raw material for preparing calcium oxide sand, a high-temperature kiln is used for calcining and decomposing, and the reaction activity of the calcium oxide sand is improved by controlling the processes such as the granularity of the raw material, the calcining temperature, the heat preservation time and the like, although the calcium oxide sand has obvious advantages, the calcium oxide sand has the following defects: one is the impurity component (such as SiO) associated with natural limestone2) The calcium oxide is difficult to remove, and is easy to react with CaO to form a low-melting phase in the high-temperature calcination process, so that the content of free CaO is reduced, and the activity of the calcium oxide sand is further reduced; secondly, in the process of calcining and decomposing limestone, the abnormal growth of the periclase grains is difficult to control, and further the reaction activity of the periclase grains is influenced.
Disclosure of Invention
The invention aims to provide a preparation method of activated calcium oxide sand with simple process. The active calcium oxide sand prepared by the method has high purity and good crystal grain development.
In order to achieve the purpose, the technical scheme adopted by the invention comprises the following specific steps:
firstly, mixing natural limestone and fluorite according to a mass ratio of the natural limestone to the fluorite of (100-105): 1, and carrying out ball milling until the granularity is less than or equal to 80 mu m to obtain the ball grinding material.
And secondly, placing the ball-milled material in a muffle furnace, and calcining for 0.5-1 hour at 950-1000 ℃ to obtain a calcined material.
And thirdly, adding water accounting for 55-60 wt% of the calcined material into the calcined material, and standing for 2-3 hours to obtain a precursor material.
And fourthly, adding a hydrofluoric acid solution accounting for 1-5 wt% of the precursor material into the precursor material, stirring for 10-15 minutes, and filtering to obtain a filter material.
And fifthly, drying the filter material for 3-4 hours at 110-120 ℃, placing the filter material in a muffle furnace, calcining for 20-30 minutes at 1380-1400 ℃, and cooling along with the furnace to obtain the activated calcium oxide sand.
CaCO of the natural limestone3The content is more than or equal to 95 wt%.
CaF of said fluorite2The content is more than or equal to 98wt percent.
The hydrofluoric acid solution is chemically pure; the concentration of the hydrofluoric acid solution is 0.2-0.5 mol/L.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the following positive effects:
1. only natural limestone and fluorite are ball-milled and calcined in a muffle furnace; and adding water into the calcined material, standing, adding a hydrofluoric acid solution, stirring, filtering, drying, calcining in a muffle furnace, and cooling to obtain the activated calcium oxide sand, wherein the preparation process is simple.
2. The invention adopts a two-step calcining method, the limestone is calcined and decomposed firstly, then is digested, the impurities are removed, the content of calcium oxide is improved, and then the calcination is carried out, so that the abnormal growth of the periclase grains is prevented, and the growth and the development of the grains are complete.
The active calcium oxide sand prepared by the invention is detected as follows: the grain size is 1.0 to 1.5 μm, and the specific surface area is 5 to 8m2The content of free CaO is 99.3-99.6 wt%.
Therefore, the invention has the characteristic of simple process; the prepared active calcium oxide sand has high purity and good crystal grain development.
Detailed Description
The invention is further described with reference to specific embodiments, without limiting its scope.
In order to avoid repetition, first, the technical parameters of the materials related to this specific embodiment are uniformly described as follows, and are not described in detail in the embodiments:
CaCO of the natural limestone3The content is more than or equal to 95 wt%.
CaF of said fluorite2The content is more than or equal to 98wt percent.
The hydrofluoric acid solution is chemically pure; the concentration of the hydrofluoric acid solution is 0.2-0.5 mol/L.
Example 1
A method for preparing active calcium oxide sand. The preparation method of the embodiment comprises the following specific steps:
firstly, mixing natural limestone and fluorite according to a mass ratio of the natural limestone to the fluorite of (100-102): 1, and carrying out ball milling until the granularity is less than or equal to 80 mu m to obtain the ball grinding material.
And secondly, placing the ball-milled material in a muffle furnace, and calcining for 0.5-1 hour at 950-970 ℃ to obtain a calcined material.
And thirdly, adding water accounting for 55-57 wt% of the calcined material into the calcined material, and standing for 2-3 hours to obtain a precursor material.
And fourthly, adding a hydrofluoric acid solution accounting for 1-4 wt% of the precursor material into the precursor material, stirring for 10-15 minutes, and filtering to obtain a filter material.
And fifthly, drying the filter material for 3-4 hours at 110-120 ℃, placing the filter material in a muffle furnace, calcining for 20-30 minutes at 1380-1388 ℃, and cooling along with the furnace to obtain the activated calcium oxide sand.
The activated calcium oxide sand prepared in the embodiment is detected as follows: the grain size is 1.0 to 1.2 μm, and the specific surface area is 6 to 8m2The content of free CaO is 99.3-99.5 wt%.
Example 2
A method for preparing active calcium oxide sand. The preparation method of the embodiment comprises the following specific steps:
firstly, mixing natural limestone and fluorite according to a mass ratio of (101-103): 1, and carrying out ball milling until the particle size is less than or equal to 80 mu m to obtain the ball grinding material.
And secondly, placing the ball-milled material in a muffle furnace, and calcining for 0.5-1 hour at 960-980 ℃ to obtain a calcined material.
And thirdly, adding water accounting for 56-58 wt% of the calcined material into the calcined material, and standing for 2-3 hours to obtain a precursor material.
And fourthly, adding a hydrofluoric acid solution accounting for 1-4 wt% of the precursor material into the precursor material, stirring for 10-15 minutes, and filtering to obtain a filter material.
And fifthly, drying the filter material for 3-4 hours at 110-120 ℃, placing the filter material in a muffle furnace, calcining for 20-30 minutes at 1384-1392 ℃, and cooling along with the furnace to obtain the activated calcium oxide sand.
The activated calcium oxide sand prepared in the embodiment is detected as follows: the grain size is 1.1 to 1.3 μm, and the specific surface area is 6 to 8m2The content of free CaO is 99.3-99.5 wt%.
Example 3
A method for preparing active calcium oxide sand. The preparation method of the embodiment comprises the following specific steps:
firstly, mixing natural limestone and fluorite according to a mass ratio of (102-104): 1, and carrying out ball milling until the particle size is less than or equal to 80 mu m to obtain the ball grinding material.
And secondly, placing the ball-milled material in a muffle furnace, and calcining for 0.5-1 hour at 970-990 ℃ to obtain a calcined material.
And thirdly, adding water accounting for 57-59 wt% of the calcined material into the calcined material, and standing for 2-3 hours to obtain a precursor material.
And fourthly, adding a hydrofluoric acid solution which accounts for 2-5 wt% of the precursor material into the precursor material, stirring for 10-15 minutes, and filtering to obtain a filter material.
And fifthly, drying the filter material for 3-4 hours at 110-120 ℃, placing the filter material in a muffle furnace, calcining for 20-30 minutes at 1388-1396 ℃, and cooling along with the furnace to obtain the activated calcium oxide sand.
The activated calcium oxide sand prepared in the embodiment is detected as follows: the grain size is 1.2 to 1.4 μm, and the specific surface area is 5 to 7m2The content of free CaO is 99.4-99.6 wt%.
Example 4
A method for preparing active calcium oxide sand. The preparation method of the embodiment comprises the following specific steps:
firstly, mixing natural limestone and fluorite according to a mass ratio of (103-105) to 1, and performing ball milling until the particle size is less than or equal to 80 mu m to obtain the ball grinding material.
And secondly, placing the ball-milled material in a muffle furnace, and calcining for 0.5-1 hour at 980-1000 ℃ to obtain a calcined material.
And thirdly, adding water accounting for 58-60 wt% of the calcined material into the calcined material, and standing for 2-3 hours to obtain a precursor material.
And fourthly, adding a hydrofluoric acid solution which accounts for 2-5 wt% of the precursor material into the precursor material, stirring for 10-15 minutes, and filtering to obtain a filter material.
And fifthly, drying the filter material for 3-4 hours at 110-120 ℃, placing the filter material in a muffle furnace, calcining for 20-30 minutes at 1392-1400 ℃, and cooling along with the furnace to obtain the activated calcium oxide sand.
The activated calcium oxide sand prepared in the embodiment is detected as follows: the grain size is 1.3 to 1.5 μm, and the specific surface area is 5 to 7m2The content of free CaO is 99.4-99.6 wt%.
Compared with the prior art, the specific implementation mode has the following positive effects:
1. in the specific embodiment, only natural limestone and fluorite are subjected to ball milling and calcined in a muffle furnace; and adding water into the calcined material, standing, adding a hydrofluoric acid solution, stirring, filtering, drying, calcining in a muffle furnace, and cooling to obtain the activated calcium oxide sand, wherein the preparation process is simple.
2. The specific implementation mode adopts a two-step calcining method, limestone is calcined and decomposed, then is digested, impurities are removed, the content of calcium oxide is increased, and then calcining is carried out, so that abnormal growth of periclase grains is prevented, and the grains are well grown and developed.
The activated calcium oxide sand prepared by the embodiment is detected as follows: the grain size is 1.0 to 1.5 μm, and the specific surface area is 5 to 8m2The content of free CaO is 99.3-99.6 wt%.
Therefore, the specific implementation mode has the characteristic of simple process; the prepared active calcium oxide sand has high purity and good crystal grain development.

Claims (1)

1. The preparation method of the active calcium oxide sand is characterized by comprising the following specific steps:
firstly, mixing natural limestone and fluorite according to a mass ratio of the natural limestone to the fluorite of (100-105): 1, and carrying out ball milling until the particle size is less than or equal to 80 mu m to obtain a ball grinding material;
secondly, placing the ball-milled material in a muffle furnace, and calcining for 0.5-1 hour at 950-1000 ℃ to obtain a calcined material;
thirdly, adding water accounting for 55-60 wt% of the calcined material into the calcined material, and standing for 2-3 hours to obtain a precursor material;
fourthly, adding a hydrofluoric acid solution which accounts for 1-5 wt% of the precursor material into the precursor material, stirring for 10-15 minutes, and filtering to obtain a filter material;
fifthly, drying the filter material at 110-120 ℃ for 3-4 hours, placing the filter material in a muffle furnace, calcining at 1380-1400 ℃ for 20-30 minutes, and cooling along with the furnace to obtain activated calcium oxide sand;
CaCO of the natural limestone3The content is more than or equal to 95 wt%;
CaF of said fluorite2The content is more than or equal to 98 wt%;
the hydrofluoric acid solution is chemically pure; the concentration of the hydrofluoric acid solution is 0.2-0.5 mol/L.
CN201810746736.1A 2018-07-09 2018-07-09 Preparation method of active calcium oxide sand Active CN108640140B (en)

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Publication number Priority date Publication date Assignee Title
CN110773110B (en) * 2019-09-24 2022-08-16 九江中船化学科技有限公司 High-specific-surface-area calcium oxide drying agent and preparation method thereof

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4366257A (en) * 1981-06-03 1982-12-28 Ube Industries, Ltd. Process for producing a calcia clinker
CN1803703A (en) * 2006-01-20 2006-07-19 东北大学 Method for preparing compact calcium oxide sand
CN101293780A (en) * 2008-06-26 2008-10-29 河南省耕生耐火材料有限公司 Method for synthesizing calcium sand and producing calcium filter for pouring box sublimation

Family Cites Families (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP3153637B2 (en) * 1992-06-23 2001-04-09 美濃窯業株式会社 Method for producing calcia clinker

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US4366257A (en) * 1981-06-03 1982-12-28 Ube Industries, Ltd. Process for producing a calcia clinker
CN1803703A (en) * 2006-01-20 2006-07-19 东北大学 Method for preparing compact calcium oxide sand
CN101293780A (en) * 2008-06-26 2008-10-29 河南省耕生耐火材料有限公司 Method for synthesizing calcium sand and producing calcium filter for pouring box sublimation

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Effective date of registration: 20230725

Address after: A7-104, No. 199 Mufu East Road, Gulou District, Nanjing City, Jiangsu Province, 210009

Patentee after: Nanjing Hezhi Technology Co.,Ltd.

Address before: 430081 No. 947 Heping Avenue, Qingshan District, Hubei, Wuhan

Patentee before: WUHAN University OF SCIENCE AND TECHNOLOGY

Effective date of registration: 20230725

Address after: 157000 Yu Qing Cun, Kuishan Town, Linkou County, Mudanjiang City, Heilongjiang Province

Patentee after: Linkou County Yumao Calcium Industry Co.,Ltd.

Address before: A7-104, No. 199 Mufu East Road, Gulou District, Nanjing City, Jiangsu Province, 210009

Patentee before: Nanjing Hezhi Technology Co.,Ltd.