CN106187242A - A kind of high-strength light forsterite fire resistant materials and preparation method thereof - Google Patents

A kind of high-strength light forsterite fire resistant materials and preparation method thereof Download PDF

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CN106187242A
CN106187242A CN201610581558.2A CN201610581558A CN106187242A CN 106187242 A CN106187242 A CN 106187242A CN 201610581558 A CN201610581558 A CN 201610581558A CN 106187242 A CN106187242 A CN 106187242A
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strength light
fire resistant
resistant materials
content
preparation
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CN106187242B (en
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陈少
陈少一
刘浩
王周福
王玺堂
马妍
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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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Abstract

A kind of high-strength light forsterite fire resistant materials and preparation method thereof.Its scheme is: first silicon-containing material, magnesium salt, zinc-containing raw materials, iron powder and boric acid are mixed, molding, under reducing atmosphere heat treatment, grinds, obtains A material.Again A material, surfactant, thickening agent, additive and water are mixed, ball milling, obtain slip.Then silicon-containing material, magnesia powder, zinc-containing raw materials, municipal sludge and surfactant are mixed, molding；Heat treatment under reducing atmosphere, heat treatment under neutral atmosphere, grinds, obtains B material and C material.Finally magnesia particle, magnesia powder, silicon-containing material, B material, C material, zinc-containing raw materials and slip are mixed, molding, heat treatment, prepare high-strength light forsterite fire resistant materials.Raw material sources of the present invention are wide, and production cost is low；Made goods resistance to elevated temperatures is excellent, intensity is high and Thermal Conductivity at High Temperature is low, can be with life-time service under the hot environment of the contacts such as reducing atmosphere, alkalescence dust.

Description

A kind of high-strength light forsterite fire resistant materials and preparation method thereof
Technical field
The invention belongs to white olivine technical field of refractory materials.It is specifically related to a kind of high-strength light white olivine Refractory material and preparation method thereof.
Background technology
Forsterite crystal has that fusing point is high, heat conductivity is low, stable chemical nature, resistance to metal bath and scouring high Deng good characteristic.And natural boltonite not only impurity content is big compared with high and loss on ignition, even if processing through high-temperature calcination, still can not Meet the requirement of high-grade refractory product, had a strong impact on refractory material and produced and the popularization of refractory products.
, all there is certain deficiency in the method that in prior art prepared by relevant forsterite.Mainly show as in raw material Impurity content is higher, and is limited by preparation method, makes prepared forsterite high temperature properties unstable, and appreciable impact is produced Life-time service under the high-temperature behavior of thing, and then the hot environment that cannot contact with etching medium, reducing atmosphere, alkalescence dust etc., Limit its application in refractory product.
Summary of the invention
It is contemplated that overcome the defect that prior art exists, it is therefore an objective to provide a kind of raw material sources extensively and production cost The preparation method of low high-strength light forsterite fire resistant materials；The high-strength light white olivine prepared by the method Refractory material resistance to elevated temperatures is excellent, intensity is high and Thermal Conductivity at High Temperature is low, at the height that reducing atmosphere contacts with alkalescence dust etc. Can life-time service under temperature environment.
For achieving the above object, the comprising the concrete steps that of the technical solution used in the present invention:
The first step, by the silicon-containing material of 30 ~ 50wt%, the magnesium salt of 20 ~ 40wt%, the zinc-containing raw materials of 1 ~ 10wt%, the ferrum of 1 ~ 10wt% The boric acid mix homogeneously of powder and 1 ~ 10wt%, compressing；Heat treatment 3 ~ 6 hours under the conditions of reducing atmosphere and 800 ~ 1200 DEG C, Broken, grind, screening, obtain the granularity A material less than 0.045mm.
Second step, by the described A material of 60 ~ 80wt%, the surfactant of 5 ~ 15wt%, the thickening agent of 5 ~ 15wt% and 3 ~ The additive mix homogeneously of 15wt%, obtains compound；The water of the most additional described compound 30 ~ 60wt%, ball milling, obtain slip.
3rd step, by the described silicon-containing material of 10 ~ 30wt%, the magnesia powder of 10 ~ 30wt%, 1 ~ 10wt% described containing zinc The described surfactant mix homogeneously of raw material, the municipal sludge of 30 ~ 50wt% and 1 ~ 10wt%, compressing；Then in reduction Heat treatment 3 ~ 6 hours under the conditions of atmosphere and 600 ~ 1000 DEG C, under the conditions of neutral atmosphere and 1200 ~ 1500 DEG C, heat treatment 3 ~ 6 is little Time, broken, grind, screening, obtain the granularity B material less than 0.088mm and C material that granularity is 0.088 ~ 5mm.
4th step, by the magnesia particle of 10 ~ 30wt%, the described magnesia powder of 5 ~ 10wt%, 5 ~ 10wt% described siliceous former Material, the described B material of 10 ~ 30wt%, the described C material of 10 ~ 30wt%, the described zinc-containing raw materials of 1 ~ 10wt% and the institute of 1 ~ 10wt% State slip mix homogeneously, compressing；Then heat treatment 3 ~ 6 hours under the conditions of 1300 ~ 1500 DEG C, prepare high-strength light magnesium Olivine refractory.
The granularity of described silicon-containing material is less than 0.088mm；Described silicon-containing material is quartz sand or is fused quartz, silicon-containing material In SiO2Content is more than 99wt%.
The granularity of described magnesium salt is less than 0.088mm；Described magnesium salt is magnesium nitrate or is magnesium sulfate, Mg in described magnesium nitrate (NO3)2Content more than 99wt%, MgSO in described magnesium sulfate4Content more than 99wt%.
The granularity of described zinc-containing raw materials is less than 0.088mm；Described zinc-containing raw materials is zinc sulfate or is zinc phosphate, described sulphuric acid ZnSO in zinc4Content more than 99wt%, Zn in described zinc phosphate3(PO4)2Content more than 99wt%.
The water content of described municipal sludge is less than 10wt%, and the granularity of municipal sludge is less than 0.088mm；Described municipal sludge In: SiO2Content is more than 30wt%, Fe2O3Content is less than 6wt%, Al2O3Content is more than 10wt%.
Described reducing atmosphere is hydrogen atmosphere or is carbon monoxide atmosphere.
Described surfactant is lauric acid amide of ethanol or is alkyl polyglucoside.
Described thickening agent is hydroxyethyl cellulose or is modified starch.
Described additive is Ludox or is white carbon；SiO in described Ludox2Content be 25 ~ 30wt%, described in vain SiO in white carbon black2Content more than 92wt%.
Described magnesia is magnesite clinker or is fused magnesite, and the content of MgO of described magnesia is more than 96wt%；Described magnesia is thin The granularity of powder is less than 0.088mm, and the granularity of described magnesia particle is 1 ~ 5mm.
Described neutral atmosphere is nitrogen atmosphere or is argon gas atmosphere.
Described compressing pressure is 50 ~ 100MPa.
Owing to using technique scheme, the present invention compared with prior art has a following good effect:
Raw material sources of the present invention are extensive, and production cost is low；The present invention is by the atmosphere in each step, raw material grain The strict control of the operations such as degree, briquetting pressure and heat treatment, not only improves the homogenizing of different material granule and various feed particles Between close contact, also provide proportional space for the formation of micro structure, thus prepared high-strength light forsterite Fire resistant materials has higher compressive resistance, relatively low bulk density and relatively low heat conductivity, in reducing atmosphere and alkalescence Can life-time service under the hot environment of the contact such as dust.
High-strength light forsterite fire resistant materials prepared by the present invention is after testing: compressive resistance is more than 5MPa；Volume Density is less than 1.0g/cm3；Heat conductivity in the range of 200 ~ 1400 DEG C is 0.05 ~ 0.3W/ (m K).
Therefore, raw material sources of the present invention are extensive, and production cost is low；Prepared high-strength light white olivine fire proofed wood The resistance to elevated temperatures of material is excellent, intensity is high and Thermal Conductivity at High Temperature is low, at the high temperature ring that reducing atmosphere contacts with alkalescence dust etc. Can life-time service under border.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the invention will be further described, not the restriction to its protection domain.
For avoiding repeating, first by the material number involved by this detailed description of the invention and compressing pressure Unify legislation such as Under, embodiment repeats no more:
The granularity of described silicon-containing material is less than 0.088mm, the SiO of described silicon-containing material2Content is more than 99wt%.
The granularity of described magnesium salt is less than 0.088mm；Mg (NO in described magnesium nitrate3)2Content more than 99wt%, described sulphuric acid MgSO in magnesium4Content more than 99wt%.
The granularity of described zinc-containing raw materials is less than 0.088mm.
SiO in described Ludox2Content be 25 ~ 30wt%, SiO in described white carbon2Content more than 92wt%.
The content of MgO of described magnesia is more than 96wt%；The granularity of described magnesia powder is less than 0.088mm, described magnesia particle Granularity be 1 ~ 5mm.
The water content of described municipal sludge is less than 10wt%, and the granularity of municipal sludge is less than 0.088mm；Described municipal sludge In: SiO2Content is more than 30wt%, Fe2O3Content is less than 6wt%, Al2O3Content is more than 10wt%.
Described compressing pressure is 50 ~ 100MPa.
Embodiment 1
A kind of high-strength light forsterite fire resistant materials and preparation method thereof.The step of preparation method described in the present embodiment It is:
The first step, by the silicon-containing material of 30 ~ 40wt%, the magnesium salt of 30 ~ 40wt%, the zinc-containing raw materials of 1 ~ 10wt%, the ferrum of 1 ~ 10wt% The boric acid mix homogeneously of powder and 1 ~ 10wt%, compressing；Heat treatment 3 ~ 6 hours under the conditions of reducing atmosphere and 800 ~ 1100 DEG C, Broken, grind, screening, obtain the granularity A material less than 0.045 mm.
Second step, by the described A material of 60 ~ 70wt%, the surfactant of 10 ~ 15wt%, the thickening agent of 10 ~ 15wt% and 3 The additive mix homogeneously of ~ 10wt%, obtains compound；The water of the most additional described compound 30 ~ 50wt%, ball milling, obtain slip.
3rd step, by the described silicon-containing material of 10 ~ 20wt%, the magnesia powder of 20 ~ 30wt%, 1 ~ 6wt% described former containing zinc Material, the municipal sludge of 40 ~ 50wt% and the described surfactant mix homogeneously of 1 ~ 6wt%, compressing；Then at reducing atmosphere With 600 ~ 900 DEG C under the conditions of heat treatment 3 ~ 6 hours, heat treatment 3 ~ 6 hours under the conditions of neutral atmosphere and 1200 ~ 1400 DEG C, broken Broken, grind, screening, obtain the granularity B material less than 0.088mm and C material that granularity is 0.088 ~ 5mm.
4th step, by the magnesia particle of 10 ~ 20wt%, the described magnesia powder of 5 ~ 10wt%, 5 ~ 10wt% described siliceous former Material, the described B material of 20 ~ 30wt%, the described C material of 10 ~ 20wt%, the described zinc-containing raw materials of 5 ~ 10wt% and the institute of 5 ~ 10wt% State slip mix homogeneously, compressing；Then heat treatment 3 ~ 6 hours under the conditions of 1300 ~ 1400 DEG C, prepare high-strength light magnesium Olivine refractory.
In the present embodiment:
Described silicon-containing material is quartz sand；
Described magnesium salt is magnesium nitrate；
Described zinc-containing raw materials is zinc sulfate；
Described reducing atmosphere is hydrogen atmosphere；
Described surfactant is lauric acid amide of ethanol；
Described thickening agent is hydroxyethyl cellulose；
Described additive is Ludox；
Described magnesia is magnesite clinker；
Described neutral atmosphere is nitrogen atmosphere.
Embodiment 2
A kind of high-strength light forsterite fire resistant materials and preparation method thereof.In addition to following material, remaining is with embodiment 1:
Described silicon-containing material is fused quartz；
Described magnesium salt is magnesium sulfate；
Described zinc-containing raw materials is zinc phosphate；
Described reducing atmosphere is carbon monoxide atmosphere；
Described surfactant is alkyl polyglucoside；
Described thickening agent is modified starch；
Described additive is white carbon；
Described magnesia is fused magnesite；
Described neutral atmosphere is argon gas atmosphere.
Embodiment 3
A kind of high-strength light forsterite fire resistant materials and preparation method thereof.The step of preparation method described in the present embodiment It is:
The first step, by the silicon-containing material of 40 ~ 50wt%, the magnesium salt of 20 ~ 30wt%, the zinc-containing raw materials of 1 ~ 10wt%, the ferrum of 1 ~ 10wt% The boric acid mix homogeneously of powder and 1 ~ 10wt%, compressing；Heat treatment 3 ~ 6 hours under the conditions of reducing atmosphere and 900 ~ 1200 DEG C, Broken, grind, screening, obtain the granularity A material less than 0.045mm.
Second step, by the described A material of 70 ~ 80wt%, the surfactant of 5 ~ 10wt%, the thickening agent of 5 ~ 10wt% and 8 ~ The additive mix homogeneously of 15wt%, obtains compound；The water of the most additional described compound 40 ~ 60wt%, ball milling, obtain slip.
3rd step, by the described silicon-containing material of 20 ~ 30wt%, the magnesia powder of 10 ~ 20wt%, 5 ~ 10wt% described containing zinc The described surfactant mix homogeneously of raw material, the municipal sludge of 30 ~ 40wt% and 5 ~ 10wt%, compressing；Then in reduction Heat treatment 3 ~ 6 hours under the conditions of atmosphere and 700 ~ 1000 DEG C, under the conditions of neutral atmosphere and 1300 ~ 1500 DEG C, heat treatment 3 ~ 6 is little Time, broken, grind, screening, obtain the granularity B material less than 0.088mm and C material that granularity is 0.088 ~ 5mm.
4th step, by the magnesia particle of 20 ~ 30wt%, the described magnesia powder of 5 ~ 10wt%, 5 ~ 10wt% described siliceous former Material, the described B material of 10 ~ 20wt%, the described C material of 20 ~ 30wt%, the described zinc-containing raw materials of 1 ~ 6wt% and 1 ~ 6wt%'s is described Slip mix homogeneously, compressing；Then heat treatment 3 ~ 6 hours under the conditions of 1400 ~ 1500 DEG C, prepare high-strength light magnesium olive Olive stone fire resistant materials.
In the present embodiment:
Described silicon-containing material is fused quartz；
Described magnesium salt is magnesium sulfate；
Described zinc-containing raw materials is zinc phosphate；
Described reducing atmosphere is carbon monoxide atmosphere；
Described surfactant is alkyl polyglucoside；
Described thickening agent is modified starch；
Described additive is white carbon；
Described magnesia is fused magnesite；
Described neutral atmosphere is argon gas atmosphere.
Embodiment 4
A kind of high-strength light forsterite fire resistant materials and preparation method thereof.In addition to following material, remaining is with embodiment 1:
Described silicon-containing material is quartz sand；
Described magnesium salt is magnesium nitrate；
Described zinc-containing raw materials is zinc sulfate；
Described reducing atmosphere is hydrogen atmosphere；
Described surfactant is lauric acid amide of ethanol；
Described thickening agent is hydroxyethyl cellulose；
Described additive is Ludox；
Described magnesia is magnesite clinker；
Described neutral atmosphere is nitrogen atmosphere.
This detailed description of the invention compared with prior art has a following good effect:
The raw material sources that this detailed description of the invention is used are extensive, and production cost is low；This detailed description of the invention is by each step In the strict control of the operation such as atmosphere, raw material granularity, briquetting pressure and heat treatment, not only improve the homogenizing of different material granule And the close contact between various feed particles, also the formation for micro structure provides proportional space, thus prepared high-strength Degree light forsterite fire resistant materials has higher compressive resistance, relatively low bulk density and relatively low heat conductivity, Can life-time service under the hot environment that reducing atmosphere contacts with alkalescence dust etc..
High-strength light forsterite fire resistant materials prepared by this detailed description of the invention is after testing: compressive resistance is more than 5MPa；Bulk density is less than 1.0g/cm3；Heat conductivity in the range of 200 ~ 1400 DEG C is 0.05 ~ 0.3W/ (m K).
Therefore, this detailed description of the invention raw material sources are extensive, and production cost is low；Prepared high-strength light forsterite The resistance to elevated temperatures of fire resistant materials is excellent, intensity is high and Thermal Conductivity at High Temperature is low, contacts with alkalescence dust etc. at reducing atmosphere Hot environment under can life-time service.

Claims (9)

1. the preparation method of a high-strength light forsterite fire resistant materials, it is characterised in that described preparation method is:
The first step, by the silicon-containing material of 30 ~ 50wt%, the magnesium salt of 20 ~ 40wt%, the zinc-containing raw materials of 1 ~ 10wt%, the ferrum of 1 ~ 10wt% The boric acid mix homogeneously of powder and 1 ~ 10wt%, compressing；Heat treatment 3 ~ 6 hours under the conditions of reducing atmosphere and 800 ~ 1200 DEG C, Broken, grind, screening, obtain the granularity A material less than 0.045mm；
Second step, by described A material, the surfactant of 5 ~ 15wt%, the thickening agent of 5 ~ 15wt% and the 3 ~ 15wt% of 60 ~ 80wt% Additive mix homogeneously, obtain compound；The water of the most additional described compound 30 ~ 60wt%, ball milling, obtain slip；
3rd step, by the described silicon-containing material of 10 ~ 30wt%, the magnesia powder of 10 ~ 30wt%, the described zinc-containing raw materials of 1 ~ 10wt%, The municipal sludge of 30 ~ 50wt% and the described surfactant mix homogeneously of 1 ~ 10wt%, compressing；Then at reducing atmosphere and Heat treatment 3 ~ 6 hours under the conditions of 600 ~ 1000 DEG C, heat treatment 3 ~ 6 hours under the conditions of neutral atmosphere and 1200 ~ 1500 DEG C is broken Broken, grind, screening, obtain the granularity B material less than 0.088mm and C material that granularity is 0.088 ~ 5mm；
4th step, by the magnesia particle of 10 ~ 30wt%, the described magnesia powder of 5 ~ 10wt%, the described silicon-containing material of 5 ~ 10wt%, The described B material of 10 ~ 30wt%, the described C material of 10 ~ 30wt%, the described zinc-containing raw materials of 1 ~ 10wt% and 1 ~ 10wt%'s is described Slip mix homogeneously, compressing；Then heat treatment 3 ~ 6 hours under the conditions of 1300 ~ 1500 DEG C, prepare high-strength light magnesium olive Olive stone fire resistant materials；
The granularity of described silicon-containing material is less than 0.088mm；Described silicon-containing material is quartz sand or is fused quartz, described silicon-containing material In SiO2Content is more than 99wt%；
The granularity of described magnesium salt is less than 0.088mm；Described magnesium salt is magnesium nitrate or is magnesium sulfate, Mg (NO in described magnesium nitrate3)2 Content more than 99wt%, MgSO in described magnesium sulfate4Content more than 99wt%；
The granularity of described zinc-containing raw materials is less than 0.088mm；Described zinc-containing raw materials is zinc sulfate or is zinc phosphate, in described zinc sulfate ZnSO4Content more than 99wt%, Zn in described zinc phosphate3(PO4)2Content more than 99wt%；
The water content of described municipal sludge is less than 10wt%, and the granularity of municipal sludge is less than 0.088mm；In described municipal sludge: SiO2Content is more than 30wt%, Fe2O3Content is less than 6wt%, Al2O3Content is more than 10wt%.
The preparation method of high-strength light forsterite fire resistant materials the most according to claim 1, it is characterised in that described Reducing atmosphere is hydrogen atmosphere or is carbon monoxide atmosphere.
The preparation method of high-strength light forsterite fire resistant materials the most according to claim 1, it is characterised in that described Surfactant is lauric acid amide of ethanol or is alkyl polyglucoside.
The preparation method of high-strength light forsterite fire resistant materials the most according to claim 1, it is characterised in that described Thickening agent is hydroxyethyl cellulose or is modified starch.
The preparation method of high-strength light forsterite fire resistant materials the most according to claim 1, it is characterised in that described Additive is Ludox or is white carbon；SiO in described Ludox2Content be 25 ~ 30wt%, SiO in described white carbon2Contain Amount is more than 92wt%.
The preparation method of high-strength light forsterite fire resistant materials the most according to claim 1, it is characterised in that described Magnesia is magnesite clinker or is fused magnesite, and the content of MgO of described magnesia is more than 96wt%；The granularity of described magnesia powder is less than 0.088mm, the granularity of described magnesia particle is 1 ~ 5mm.
The preparation method of high-strength light forsterite fire resistant materials the most according to claim 1, it is characterised in that described Neutral atmosphere is nitrogen atmosphere or is argon gas atmosphere.
The preparation method of high-strength light forsterite fire resistant materials the most according to claim 1, it is characterised in that described Compressing pressure is 50 ~ 100MPa.
9. a high-strength light forsterite fire resistant materials, it is characterised in that described high-strength light white olivine is fire-resistant Material is made according to the preparation method of high-strength light forsterite fire resistant materials according to any one of claim 1 ~ 8 Standby high-strength light forsterite fire resistant materials.
CN201610581558.2A 2016-07-22 2016-07-22 A kind of high-strength light forsterite fire resistant materials and preparation method thereof Expired - Fee Related CN106187242B (en)

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CN103011870A (en) * 2013-01-17 2013-04-03 武汉科技大学 Forsterite refractory and production method thereof
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