CN109179470A - A kind of passive oxidation calcium particle and preparation method thereof - Google Patents

A kind of passive oxidation calcium particle and preparation method thereof Download PDF

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Publication number
CN109179470A
CN109179470A CN201811160093.9A CN201811160093A CN109179470A CN 109179470 A CN109179470 A CN 109179470A CN 201811160093 A CN201811160093 A CN 201811160093A CN 109179470 A CN109179470 A CN 109179470A
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CN
China
Prior art keywords
particle
calcium
calcium hydroxide
passive oxidation
agent solution
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Pending
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CN201811160093.9A
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Chinese (zh)
Inventor
魏耀武
李炳蓉
肖俊李
刘少坤
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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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Priority to CN201811160093.9A priority Critical patent/CN109179470A/en
Publication of CN109179470A publication Critical patent/CN109179470A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F11/00Compounds of calcium, strontium, or barium
    • C01F11/02Oxides or hydroxides
    • C01F11/04Oxides or hydroxides by thermal decomposition
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

Abstract

The present invention relates to a kind of passive oxidation calcium particles and preparation method thereof.Its technical solution is: calcium hydroxide powder and the water for accounting for 10~30wt% of the calcium hydroxide powder are placed in the charging basket of Granulation Equipments, start to be granulated under conditions of rotor speed is 200~2000 turns per minute, after the calcium hydroxide powder in charging basket is converted to particle, then at rotor speed be 200~2000 turns per minute under conditions of, the coupling agent solution for accounting for 0.1~6wt% of the calcium hydroxide powder is sprayed into, calcium hydroxide particle is obtained;The calcium hydroxide particle is 12~24 hours dry under 50~110 DEG C of condition degree, it is subsequently placed in heating furnace, keeps the temperature 1~5 hour under the conditions of 1500~1700 DEG C, it is cooling, passive oxidation calcium particle is made.Present invention process is simple, and prepared passive oxidation calcium particle has the characteristics that hydration resistance is good, can be used as the raw material for preparing the advanced materials such as calcium oxide ceramics and refractory material.

Description

A kind of passive oxidation calcium particle and preparation method thereof
Technical field
The invention belongs to calcia material technical fields.More particularly to a kind of passive oxidation calcium particle and preparation method thereof.
Background technique
It is special type fire material made from essential mineral (CaO is main component) that calcium oxide products, which are using calcium oxide (square calcium stone), Material.Calcium oxide products have many advantages, such as that high-temperature behavior is good, alkali resistance slag action is strong and can cleaning high-temp melt, in noble metal smelting The metallurgy industries such as refining are widely applied.But calcium oxide raw material or material containing free calcium oxide easily water in air Change, aquation will lead to material cracks and dusting, seriously constrain calcium oxide raw material and material containing free calcium oxide in the industry Popularization and application.Meanwhile calcia linker is the primary raw material of calcium oxide products preparation, performance and manufacturing cost height will be straight Connect the quality and price for influencing calcium oxide products.
The preparation method of calcia linker includes sintering process and electric smelting method: sintering process is first by lime stone 1200~1300 It is calcined under the conditions of DEG C, briquet after cooling, then block is burnt into 1700 DEG C or so, be broken into calcium oxide particle after cooling Material;Electric smelting method is that directly by marble blocks, electrically smelting is needed before electric smelting for calcia linker by marble in three-phase electric arc At particulate material or balling-up, it then can just be put into electric smelting in electric furnace.In sintering process, also it has been proposed that following technical solution: first will Lime stone is light-burned, active calcium oxide is made, then calcium hydroxide slurry is made in active calcium oxide digestion (adding water), by slurry mistake Calcium hydroxide green body is obtained after filter, drying.Then various additives are added and calcium hydroxide green body is ground altogether, be pressed into base, will To green body calcined under the conditions of 1600~1800 DEG C, calcium oxide green body is made, is finally aoxidized calcium oxide green body is broken Calcium particle.
As can be seen that the preparation method of existing calcium oxide particle is not only at high cost and energy consumption is high, and complex process.Applicant Team it is proposed that comminution granulation prepares the method (ZL201610535065.5 and ZL201610535082.9) of calcium oxide particle simultaneously Applied to practice, preferable effect is achieved.But the hydration resistance of calcium oxide particle still needs to continue to improve.
Summary of the invention
The present invention is directed to overcome the shortage of prior art, it is therefore an objective to provide a kind of system of the passive oxidation calcium particle of simple process Preparation Method, the passive oxidation calcium particle hydration resistance prepared with this method is good, can be used as preparing calcium oxide ceramics and fire proofed wood The raw material of the advanced materials such as material.
To achieve the above object, the technical scheme adopted by the invention is that:
Calcium hydroxide powder and the water for accounting for 10~30wt% of the calcium hydroxide powder are placed in the charging basket of Granulation Equipments, Start to be granulated under conditions of rotor speed is 200~2000 turns per minute, be converted to the calcium hydroxide powder in charging basket Grain after, then at rotor speed be 200~2000 turns per minute under conditions of, penetrating account for 0.1~6wt% of the calcium hydroxide powder Coupling agent solution, obtain calcium hydroxide particle;By the calcium hydroxide particle dry 12~24 under 50~110 DEG C of condition degree Hour, it is subsequently placed in heating furnace, keeps the temperature 1~5 hour under the conditions of 1500~1700 DEG C, it is cooling, passive oxidation calcium is made Grain.
Ca (OH) in the calcium hydroxide powder2Content >=95wt%;Partial size is 1~300 μm.
The coupling agent solution is titanate coupling agent solution, aluminate coupling agent solution, zirconic acid rouge coupling agent solution, phosphorus One of acid esters coupling agent solution and rare-earth coupling agent solution.
Due to the adoption of the above technical scheme, the present invention has following good effect compared with prior art:
1) present invention is directly granulated calcium hydroxide powder, up to dense granule calcium oxide, production technology after high-temperature process Simply.
2) during the high temperature treatment process, the coupling agent and calcium oxide on calcium hydroxide particle surface layer occur hair and answer the present invention, promote Into calcium hydroxide particle surface sintering and form cenotype and be wrapped in final products calcium oxide particle surface, cenotype is to be not easy The substance of aquation, such as: calcium zirconate, calcium aluminate and calcium phosphate etc..Cenotype is sintered by the oxygen in the vapor and particle in air Change calcium component to keep apart, to improve the hydration resistance of passive oxidation calcium particle.
3) present invention is crushed processing without carrying out to the passive oxidation calcium particle obtained after high-temperature process again, will not destroy The sinter layer that passive oxidation calcium particle surface is formed during the high temperature treatment process, thus, obtained passive oxidation calcium particle Hydration resistance is good, convenient for storage and production, the particulate material that can be prepared directly as calcium oxide-based refractory material and refractory ceramics It uses.
Passive oxidation calcium particle prepared by the present invention is through detecting: partial size is 0.1~8mm, CaO content >=94wt%, volume Density >=2.8g/cm3;Under 50 DEG C and 90% damp condition, 10h is kept, after 110 DEG C of drying, passive oxidation calcium particle Aquation rate of body weight gain≤1%.
Therefore, present invention process is simple, and prepared passive oxidation calcium particle hydration resistance is good, can be used as preparation oxidation The raw material of the advanced materials such as calcium ceramics and refractory material.
Specific embodiment
The present invention will be further described With reference to embodiment, not to the limitation of its protection scope.
Present embodiment: Ca (OH) in the calcium hydroxide powder2Content >=95wt%;Partial size is 1~300 μm. It is repeated no more in embodiment:
Embodiment 1
A kind of passive oxidation calcium particle and preparation method thereof.Preparation method described in the present embodiment is: by calcium hydroxide powder Body and the water for accounting for 10~20wt% of the calcium hydroxide powder are placed in the charging basket of Granulation Equipments, are per minute in rotor speed Start to be granulated under conditions of 1700~2000 turns, after the calcium hydroxide powder in charging basket is converted to particle, then at rotor speed Under conditions of 200~800 turns per minute, the coupling agent solution for accounting for 0.5~2wt% of the calcium hydroxide powder is sprayed into, is obtained Calcium hydroxide particle;The calcium hydroxide particle is 12~16 hours dry under 90~110 DEG C of condition degree, it is subsequently placed in heating In furnace, 3~5 hours are kept the temperature under the conditions of 1500~1600 DEG C, it is cooling, passive oxidation calcium particle is made.
The coupling agent solution is titanate coupling agent solution.
Passive oxidation calcium particle manufactured in the present embodiment is through detecting: the partial size of calcium oxide particle is 0.1~3mm, CaO content For 94~96wt%, 2.80~3.0g/cm of bulk density3;Under 50 DEG C, 90% damp condition, 10h is kept, is dried in 110 DEG C Afterwards, the aquation rate of body weight gain of calcium oxide particle is 0.8~1%.
Embodiment 2
A kind of passive oxidation calcium particle and preparation method thereof.Preparation method described in the present embodiment is: by calcium hydroxide powder Body and the water for accounting for 20~30wt% of the calcium hydroxide powder are placed in the charging basket of Granulation Equipments, are per minute in rotor speed Start to be granulated under conditions of 1400~1700 turns, after the calcium hydroxide powder in charging basket is converted to particle, then at rotor speed Under conditions of 800~1400 turns per minute, the coupling agent solution for accounting for 2~4wt% of the calcium hydroxide powder is sprayed into, hydrogen is obtained Calcium oxide particle;The calcium hydroxide particle is 16~20 hours dry under 80~100 DEG C of condition degree, it is subsequently placed in heating furnace In, 1~3 hour is kept the temperature under the conditions of 1600~1700 DEG C, it is cooling, passive oxidation calcium particle is made.
The coupling agent solution is aluminate coupling agent solution.
Passive oxidation calcium particle manufactured in the present embodiment is through detecting: the partial size of calcium oxide particle is 2~5mm, and CaO content is 95~97wt%, 2.9~3.1g/cm of bulk density3;Under 50 DEG C, 90% damp condition, 10h is kept, after 110 DEG C of drying, The aquation rate of body weight gain of calcium oxide particle is 0.7~0.9%.
Embodiment 3
A kind of passive oxidation calcium particle and preparation method thereof.Preparation method described in the present embodiment is: by calcium hydroxide powder Body and the water for accounting for 10~20wt% of the calcium hydroxide powder are placed in the charging basket of Granulation Equipments, are per minute in rotor speed Start to be granulated under conditions of 900~1400 turns, after the calcium hydroxide powder in charging basket is converted to particle, is then at rotor speed Under conditions of 1400~1700 turns per minute, the coupling agent solution for accounting for 4~6wt% of the calcium hydroxide powder is sprayed into, hydrogen is obtained Calcium oxide particle;The calcium hydroxide particle is 20~24 hours dry under 50~70 DEG C of condition degree, it is subsequently placed in heating furnace In, 1~3 hour is kept the temperature under the conditions of 1500~1600 DEG C, it is cooling, passive oxidation calcium particle is made.
The coupling agent solution is zirconic acid rouge coupling agent solution.
Passive oxidation calcium particle manufactured in the present embodiment is through detecting: the partial size of calcium oxide particle is 5~8mm, CaO content 96 ~98wt%, 3.0~3.2g/cm of bulk density3.Under 50 DEG C, 90% damp condition, 10h is kept, after 110 DEG C of drying, oxygen The aquation rate of body weight gain for changing calcium particle is 0.5~0.8%.
Embodiment 4
A kind of passive oxidation calcium particle and preparation method thereof.Preparation method described in the present embodiment is: by calcium hydroxide powder Body and the water for accounting for 20~30wt% of the calcium hydroxide powder are placed in the charging basket of Granulation Equipments, are per minute in rotor speed Start to be granulated under conditions of 200~900 turns, after the calcium hydroxide powder in charging basket is converted to particle, is then at rotor speed Under conditions of 1700~2000 turns per minute, the coupling agent solution for accounting for 0.2~1wt% of the calcium hydroxide powder is sprayed into, is obtained Calcium hydroxide particle;The calcium hydroxide particle is 12~18 hours dry under 60~80 DEG C of condition degree, it is subsequently placed in heating In furnace, 1~5 hour is kept the temperature under the conditions of 1600~1700 DEG C, it is cooling, passive oxidation calcium particle is made.
The coupling agent solution is phosphate coupling agent solution.
Passive oxidation calcium particle manufactured in the present embodiment is through detecting: the partial size of calcium oxide particle is 5~8mm, CaO content 97 ~99wt%, 3.1~3.3g/cm of bulk density3.Under 50 DEG C, 90% damp condition, 10h is kept, after 110 DEG C of drying, oxygen The aquation rate of body weight gain for changing calcium particle is 0.4~0.6%.
Embodiment 5
A kind of passive oxidation calcium particle and preparation method thereof.Preparation method described in the present embodiment is: by calcium hydroxide powder Body and the water for accounting for 20~30wt% of the calcium hydroxide powder are placed in the charging basket of Granulation Equipments, are per minute in rotor speed Start to be granulated under conditions of 200~900 turns, after the calcium hydroxide powder in charging basket is converted to particle, is then at rotor speed Under conditions of 1700~2000 turns per minute, the coupling agent solution for accounting for 1~3wt% of the calcium hydroxide powder is sprayed into, hydrogen is obtained Calcium oxide particle;The calcium hydroxide particle is 20~24 hours dry under 70~90 DEG C of condition degree, it is subsequently placed in heating furnace In, 3~5 hours are kept the temperature under the conditions of 1500~1600 DEG C, it is cooling, passive oxidation calcium particle is made.
The coupling agent solution is rare-earth coupling agent solution.
Passive oxidation calcium particle manufactured in the present embodiment is through detecting: the partial size of calcium oxide particle is 5~8mm, CaO content 97 ~99wt%, 3.1~3.2g/cm of bulk density3.Under 50 DEG C, 90% damp condition, 10h is kept, after 110 DEG C of drying, oxygen The aquation rate of body weight gain for changing calcium particle is 0.3~0.5%.
Present embodiment has following good effect compared with prior art:
1) present embodiment is directly granulated calcium hydroxide powder, up to dense granule calcium oxide after high-temperature process, Simple production process.
2) during the high temperature treatment process, the coupling agent and calcium oxide on calcium hydroxide particle surface layer occur present embodiment Hair is answered, and is promoted the sintering on calcium hydroxide particle surface and is formd cenotype and is wrapped in final products calcium oxide particle surface, newly Be mutually be not easy the substance of aquation, such as: calcium zirconate, calcium aluminate and calcium phosphate etc..Be sintered cenotype by air vapor and Calcium oxide component in grain is kept apart, to improve the hydration resistance of passive oxidation calcium particle.
3) present embodiment is not necessarily to carry out being crushed processing again to the passive oxidation calcium particle obtained after high-temperature process, The sinter layer that passive oxidation calcium particle surface is formed during the high temperature treatment process will not be destroyed, thus, obtained passive oxidation The hydration resistance of calcium particle is good, convenient for storage and production, can prepare directly as calcium oxide-based refractory material and refractory ceramics Particulate material use.
Present embodiment preparation passive oxidation calcium particle through detecting: partial size be 0.1~8mm, CaO content >= 94wt%, bulk density >=2.8g/cm3;Under 50 DEG C and 90% damp condition, 10h is kept, after 110 DEG C of drying, is passivated oxygen Change aquation rate of body weight gain≤1% of calcium particle.
Therefore, present embodiment simple process, prepared passive oxidation calcium particle hydration resistance is good, can be used as Prepare the raw material of the advanced materials such as calcium oxide ceramics and refractory material.

Claims (4)

1. a kind of preparation method of passive oxidation calcium particle, it is characterised in that: by calcium hydroxide powder and account for the calcium hydroxide The water of 10~30wt% of powder is placed in the charging basket of Granulation Equipments, under conditions of rotor speed is 200~2000 turns per minute Start to be granulated, is 200~2000 turns per minute then at rotor speed after the calcium hydroxide powder in charging basket is converted to particle Under the conditions of, the coupling agent solution for accounting for 0.1~6wt% of the calcium hydroxide powder is sprayed into, calcium hydroxide particle is obtained;By the hydrogen Calcium oxide particle is 12~24 hours dry under 50~110 DEG C of condition degree, is subsequently placed in heating furnace, in 1500~1700 DEG C of items 1~5 hour is kept the temperature under part, it is cooling, passive oxidation calcium particle is made.
2. the preparation method of passive oxidation calcium particle according to claim 1, it is characterised in that the calcium hydroxide powder Middle Ca (OH)2Content >=95wt%;Partial size is 1~300 μm.
3. the preparation method of passive oxidation calcium particle according to claim 1, it is characterised in that the coupling agent solution is Titanate coupling agent solution, aluminate coupling agent solution, zirconic acid rouge coupling agent solution, phosphate coupling agent solution and rare earth coupling One of agent solution.
4. a kind of passive oxidation calcium particle, it is characterised in that the passive oxidation calcium particle be according to claim 1~3 in appoint Passive oxidation calcium particle prepared by the preparation method of passive oxidation calcium particle described in one.
CN201811160093.9A 2018-09-30 2018-09-30 A kind of passive oxidation calcium particle and preparation method thereof Pending CN109179470A (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109678190A (en) * 2019-02-22 2019-04-26 武汉科技大学 A kind of core-shell structure calcium oxide particle and preparation method thereof
CN110041085A (en) * 2019-04-08 2019-07-23 武汉科技大学 A kind of calcium carbon composite and preparation method thereof
CN111217613A (en) * 2020-02-17 2020-06-02 武汉科技大学 Magnesium-calcium material and preparation method thereof
CN111268711A (en) * 2020-02-17 2020-06-12 武汉科技大学 Coated anti-hydration calcium oxide material and preparation method thereof

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CN108264364A (en) * 2018-03-01 2018-07-10 武汉科技大学 A kind of titanium coating calcia material and preparation method thereof
CN108383533A (en) * 2018-03-01 2018-08-10 武汉科技大学 A kind of hydration resistant calcia material and preparation method thereof
CN108557856A (en) * 2018-05-08 2018-09-21 武汉科技大学 A kind of calcium oxide particle and preparation method thereof based on vacuum-sintering

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CN106219585A (en) * 2016-07-08 2016-12-14 武汉科技大学 A kind of dense granule calcia material and preparation method thereof
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CN108264364A (en) * 2018-03-01 2018-07-10 武汉科技大学 A kind of titanium coating calcia material and preparation method thereof
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN109678190A (en) * 2019-02-22 2019-04-26 武汉科技大学 A kind of core-shell structure calcium oxide particle and preparation method thereof
CN110041085A (en) * 2019-04-08 2019-07-23 武汉科技大学 A kind of calcium carbon composite and preparation method thereof
CN111217613A (en) * 2020-02-17 2020-06-02 武汉科技大学 Magnesium-calcium material and preparation method thereof
CN111268711A (en) * 2020-02-17 2020-06-12 武汉科技大学 Coated anti-hydration calcium oxide material and preparation method thereof

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