CN110452009A - A kind of preparation method of in-situ preparation magnesium aluminate spinel whisker skeletal porous ceramics - Google Patents

A kind of preparation method of in-situ preparation magnesium aluminate spinel whisker skeletal porous ceramics Download PDF

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CN110452009A
CN110452009A CN201910699066.7A CN201910699066A CN110452009A CN 110452009 A CN110452009 A CN 110452009A CN 201910699066 A CN201910699066 A CN 201910699066A CN 110452009 A CN110452009 A CN 110452009A
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porous ceramics
magnesium aluminate
aluminate spinel
whisker
preparation
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罗旭东
满奕然
杨孟孟
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University of Science and Technology Liaoning USTL
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University of Science and Technology Liaoning USTL
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Abstract

The invention patent relates to a kind of preparation methods of in-situ preparation magnesium aluminate spinel whisker skeletal porous ceramics, comprising the following steps: by light-magnesite powder, activated alumina fine powder and graphite powder, is sufficiently premixed in blender；It is outer again to be subject to suitable quantity of water and starch, it is placed in and continues to be kneaded in kneading machine；It uniform pug will be kneaded is put into mold and carry out molding casting, demoulded after sample conserves in a mold；Porous ceramics green body after demoulding is dry under conditions of 110 DEG C；Green body after drying is heated up and is sintered, last Temperature fall is cooling to get to a kind of in-situ preparation magnesium aluminate spinel whisker skeletal porous ceramics.In-situ preparation magnesium aluminate spinel whisker skeletal porous ceramics prepared by the present invention are raw material preparation by resourceful Al2O3, MgO and graphite, low in cost；The magnesium aluminate spinel whisker of growth in situ solves the problems, such as to be unevenly distributed this caused by additional whisker simultaneously, helps to improve the flexural strength of sample.

Description

A kind of preparation method of in-situ preparation magnesium aluminate spinel whisker skeletal porous ceramics
Technical field
The present invention relates to technical field of inorganic chemical industry, and in particular to a kind of in-situ preparation magnesium aluminate spinel whisker skeletal porous The preparation method of ceramics.
Background technique
With the development of modern science and technology, energy growing tension, environmental protection is increasingly stringent, and thermal insulation material can not as hot industry The a part lacked, low to the performance such as thermal conductivity of some keys, refractoriness is high, and applied at elevated temperature volume stability is good, heat resistanceheat resistant Shock stability is good etc. to have also been proposed new requirement, to meet the needs of light structures high temperature kiln.By burning mistake method on domestic market Or the light weeight alumina brick of foaming preparation, lightweight magnesium-aluminum spinel brick, light weight fireclay brick, light silicious brick etc., extensively Back sheet and thermal insulation layer applied to Industrial Stoves." high-strength low heat conductivity energy-saving fireproof material " patent (CN105272276A) technology It is made of micro-pore mullite aggregate, activity and micro mist, high-temperature cement and alumina fine powder.Although its heat-proof quality is preferable, The heat-resisting quantity of high aluminium material is insufficient, and high aluminium material belongs to acid refractory, and alkali resistance atmosphere erosiveness is poor.Due to high-quality Alumine is widely used in aluminium metallurgy, refractories industry, it is current it reserved resources it is fewer and fewer, the manufacture of permanent layer at This is higher and higher.Therefore it is applied to high temperature or the work face brick of superhigh temperature Industrial Stoves mainly uses magnesia porous ceramics Material is combined by forsterite or Spinel mainly with magnesium oxide particle aggregate and prepares magnesia porous material.These materials The characteristics of for bulk density it is relatively high, the porosity is lower, and thermal coefficient is relatively large, in reduce kiln weight, it is energy-saving It is unfavorable.And under the higher porosity, intensity is relatively low, limits the extensive use of magnesia porous material.The present invention Aiming at the shortcomings of the prior art, a kind of preparation method of in-situ preparation magnesium aluminate spinel whisker skeletal porous ceramics is provided.
Summary of the invention
The present invention provides a kind of preparation methods of in-situ preparation magnesium aluminate spinel whisker skeletal porous ceramics, with light-burned oxygen Change magnesium powder, active oxidation aluminium powder is raw material, and graphite is reducing agent, starch as bonding agent and pore creating material, through premix, mixing, at Type, drying, firing obtain having symphysis in situ at magnesium aluminate spinel whisker skeletal porous ceramics.It is brilliant that spinelle is formed under high temperature Palpus skeleton, further enhances the flexural strength of porous ceramics, to obtain high-intensitive, the high porous pottery of stomata magnesium aluminate spinel Porcelain.
To achieve the above object, the invention is realized by the following technical scheme:
A kind of preparation method of in-situ preparation magnesium aluminate spinel whisker skeletal porous ceramics, which is characterized in that with light calcined magnesia Powder, active oxidation aluminium powder are raw material, and graphite powder is reducing agent, starch as bonding agent and pore creating material, through premix, mixing, molding, Dry, firing obtains having a kind of in-situ preparation magnesium aluminate spinel whisker skeletal porous ceramics, specific steps are as follows:
15-22% partial size is less than light calcined magnesia fine powder, the 50-58% of 0.074mm by percentage to the quality by step 1, premix Activated alumina fine powder of the partial size less than 0.074mm and 25-35% partial size are less than the graphite powder of 0.074mm, carry out in blender Sufficiently premix, obtains premix material；
Step 2 is kneaded, and the starch of the water and 4-8% that premix material gross mass 4-8% is added to step 1 institute with added form In the premix material obtained, it is placed in kneading machine and continues to be kneaded 10-20 minutes, the pug after being kneaded；
Step 3, molding, the pug after mixing is put into mold and carries out molding casting, conserves 24-48 in a mold to sample It is demoulded after hour, obtains porous ceramics green body；
Step 4, it is dry, the porous ceramics green body after demoulding is 24-48 hours dry under conditions of 110 DEG C；
Step 5, firing, is warming up to 600-700 DEG C for the porous ceramics green body after drying with the heating rate of 5-15 DEG C/min, Heat preservation 2-6 hours, is continuously heating to 1350-1550 DEG C, then keep the temperature 2-6 hours, is then dropped with the rate of temperature fall of 10-20 DEG C/min Temperature keeps the temperature 2-6 hours to 600-700 DEG C, and last Temperature fall is cooling to get to a kind of in-situ preparation magnesium aluminate spinel crystalline substance It must skeletal porous ceramics.
Heating rate should be lower than rate of temperature fall in the step 5.
Compared with prior art, the beneficial effects of the present invention are: 1) in-situ preparation magnesium aluminate spinel prepared by the present invention is brilliant Palpus skeletal porous ceramics, by resourceful Al2O3, MgO and graphite be raw material preparation, it is low in cost；2) magnesium aluminate spinel whisker With excellent high temperature resistant, corrosion-resistant, superior thermal shock resistance and mechanical property, being introduced into porous ceramic film material be can be improved The toughness of material increases impact strength, is conducive to the service life for improving ceramics.3) whisker can play the work of toughening to brick body With the excessive toughening effect of the draw ratio of whisker is poor, and draw ratio is too small, and product can't be whisker, referred to as crystal grain, major diameter Than for reinforcing effect between 10 ~ 70 it is best.
Detailed description of the invention
Fig. 1 is process flow diagram of the invention.
Specific embodiment
Preparation method of the invention is described further below with reference to embodiment:
Embodiment 1:
The in-situ preparation magnesium aluminate spinel whisker skeletal porous ceramics that the present embodiment provides, be made of following raw material: partial size is less than The active oxidation aluminium powder 50kg of light-magnesite powder 15kg, partial size less than 0.074mm, the partial size of 0.074mm is less than 0.074mm's Graphite powder 35kg.Additional starch is that bonding agent and pore creating material are prepared in situ raw by premix, mixing, molding, drying and firing At magnesium aluminate spinel whisker skeletal porous ceramics, specific steps are as follows:
Step 1, premix first carry out above-mentioned light-magnesite powder, active oxidation aluminium powder and graphite powder sufficiently in blender Premix, obtains premix material；
Step 2 is kneaded, 4kg water and 6kg starch is added in the resulting premix material of step 1 with added form, are placed in mixed Continue to be kneaded 20 minutes in mill, the pug after being kneaded；
Step 3, molding, the pug after mixing is put into mold and carries out molding casting, is conserved in a mold to sample 24 hours After demould, obtain porous ceramics green body；
Step 4, it is dry, the porous ceramics green body after demoulding is 24 hours dry under conditions of 110 DEG C；
Porous ceramics green body after drying is warming up to 600 DEG C with the heating rate of 5 DEG C/min by step 5, firing, and heat preservation 2 is small When, 1350 DEG C are continuously heating to, then keep the temperature 2 hours, are then cooled to 600 DEG C with the rate of temperature fall of 10 DEG C/min, heat preservation 2 is small When, last Temperature fall is cooling to get to a kind of in-situ preparation magnesium aluminate spinel whisker skeletal porous ceramics.
The draw ratio of magnesium aluminate spinel whisker in porous ceramics manufactured in the present embodiment is 10.2, and magnesium aluminate spinel is mutual Connection forms interlocking structure, high temperature break resistant intensity 7.3MPa, apparent porosity 76.5%.
Embodiment 2:
The in-situ preparation magnesium aluminate spinel whisker skeletal porous ceramics that the present embodiment provides, be made of following raw material: partial size is less than The active oxidation aluminium powder 51kg of light-magnesite powder 19kg, partial size less than 0.074mm, the partial size of 0.074mm is less than 0.074mm's Graphite powder 30kg.Additional starch is that bonding agent and pore creating material are prepared in situ raw by premix, mixing, molding, drying and firing At magnesium aluminate spinel whisker skeletal porous ceramics, specific steps are as follows:
Step 1, premix first carry out above-mentioned light-magnesite powder, active oxidation aluminium powder and graphite powder sufficiently in blender Premix, obtains premix material；
Step 2 is kneaded, 5kg water and 6kg starch is added in the resulting premix material of step 1 with added form, are placed in mixed Continue to be kneaded 10 minutes in mill, the pug after being kneaded；
Step 3, molding, the pug after mixing is put into mold and carries out molding casting, is conserved in a mold to sample 48 hours After demould, obtain porous ceramics green body；
Step 4, it is dry, the porous ceramics green body after demoulding is 36 hours dry under conditions of 110 DEG C；
Porous ceramics green body after drying is warming up to 600 DEG C with the heating rate of 5 DEG C/min by step 5, firing, and heat preservation 2 is small When, 1450 DEG C are continuously heating to, then keep the temperature 3 hours, are then cooled to 600 DEG C with the rate of temperature fall of 10 DEG C/min, heat preservation 2 is small When, last Temperature fall is cooling to get to a kind of in-situ preparation magnesium aluminate spinel whisker skeletal porous ceramics.
The draw ratio of magnesium aluminate spinel whisker in porous ceramics manufactured in the present embodiment is 65.2, and magnesium aluminate spinel is mutual Connection forms interlocking structure, high temperature break resistant intensity 12.7MPa, apparent porosity 68.5%.
Embodiment 3:
The in-situ preparation magnesium aluminate spinel whisker skeletal porous ceramics that the present embodiment provides, be made of following raw material: partial size is less than The active oxidation aluminium powder 54kg of light-magnesite powder 21kg, partial size less than 0.074mm, the partial size of 0.074mm is less than 0.074mm's Graphite powder 25kg.Additional starch is that bonding agent and pore creating material are prepared in situ raw by premix, mixing, molding, drying and firing At magnesium aluminate spinel whisker skeletal porous ceramics, specific steps are as follows:
Step 1, premix first carry out above-mentioned light-magnesite powder, active oxidation aluminium powder and graphite powder sufficiently in blender Premix, obtains premix material；
Step 2 is kneaded, 6kg water and 4kg starch is added in the resulting premix material of step 1 with added form, are placed in mixed Continue to be kneaded 15 minutes in mill, the pug after being kneaded；
Step 3, molding, the pug after mixing is put into mold and carries out molding casting, is conserved in a mold to sample 36 hours After demould, obtain porous ceramics green body；
Step 4, it is dry, the porous ceramics green body after demoulding is 48 hours dry under conditions of 110 DEG C；
Porous ceramics green body after drying is warming up to 600 DEG C with the heating rate of 5 DEG C/min by step 5, firing, and heat preservation 2 is small When, 1550 DEG C are continuously heating to, then keep the temperature 4 hours, are then cooled to 600 DEG C with the rate of temperature fall of 10 DEG C/min, heat preservation 2 is small When, last Temperature fall is cooling to get to a kind of in-situ preparation magnesium aluminate spinel whisker skeletal porous ceramics.
The draw ratio of the magnesium aluminate spinel whisker of porous ceramics manufactured in the present embodiment is 30.1, and high temperature break resistant intensity is 9.8MPa, apparent porosity 59.1%.

Claims (2)

1. a kind of preparation method of in-situ preparation magnesium aluminate spinel whisker skeletal porous ceramics, which is characterized in that with light-burned oxidation Magnesium powder, active oxidation aluminium powder are raw material, graphite powder is reducing agent, starch as bonding agent and pore creating material, through premix, mixing, at Type, drying, firing obtain having a kind of in-situ preparation magnesium aluminate spinel whisker skeletal porous ceramics, and concrete operation step is such as Under:
15-22% partial size is less than light calcined magnesia fine powder, the 50-58% of 0.074mm by percentage to the quality by step 1, premix Activated alumina fine powder of the partial size less than 0.074mm and 25-35% partial size are less than the graphite powder of 0.074mm, carry out in blender Sufficiently premix, obtains premix material；
Step 2 is kneaded, and the starch of the water and 4-8% that premix material gross mass 4-8% is added to step 1 institute with added form In the premix material obtained, it is placed in kneading machine and continues to be kneaded 10-20 minutes, the pug after being kneaded；
Step 3, molding, the pug after mixing is put into mold and carries out molding casting, conserves 24-48 in a mold to sample It is demoulded after hour, obtains porous ceramics green body；
Step 4, it is dry, the porous ceramics green body after demoulding is 24-48 hours dry under conditions of 110 DEG C；
Step 5, firing, is warming up to 600-700 DEG C for the porous ceramics green body after drying with the heating rate of 5-15 DEG C/min, Heat preservation 2-6 hours, is continuously heating to 1350-1550 DEG C, then keep the temperature 2-6 hours, is then dropped with the rate of temperature fall of 10-20 DEG C/min Temperature keeps the temperature 2-6 hours to 600-700 DEG C, and last Temperature fall is cooling to get to a kind of in-situ preparation magnesium aluminate spinel crystalline substance It must skeletal porous ceramics.
2. a kind of preparation method of in-situ preparation magnesium aluminate spinel whisker skeletal porous ceramics according to claim 1, It is characterized in that, the heating rate in the step 5 should be lower than rate of temperature fall.
CN201910699066.7A 2019-07-31 2019-07-31 A kind of preparation method of in-situ preparation magnesium aluminate spinel whisker skeletal porous ceramics Pending CN110452009A (en)

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Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112358288A (en) * 2020-11-27 2021-02-12 武汉科技大学 Forsterite-spinel ceramic based on high-carbon ferrochrome slag and preparation method thereof
CN116120093A (en) * 2023-02-20 2023-05-16 江门市俞嘉科技有限公司 Heat insulation wallboard and production method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108977884A (en) * 2018-09-25 2018-12-11 太仓弘潞新材料有限公司 A kind of preparation method of magnesium aluminate spinel whisker

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108977884A (en) * 2018-09-25 2018-12-11 太仓弘潞新材料有限公司 A kind of preparation method of magnesium aluminate spinel whisker

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112358288A (en) * 2020-11-27 2021-02-12 武汉科技大学 Forsterite-spinel ceramic based on high-carbon ferrochrome slag and preparation method thereof
CN116120093A (en) * 2023-02-20 2023-05-16 江门市俞嘉科技有限公司 Heat insulation wallboard and production method thereof

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