CN103664208A - Wet process sintering production method for hercynite - Google Patents

Wet process sintering production method for hercynite Download PDF

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Publication number
CN103664208A
CN103664208A CN201310605502.2A CN201310605502A CN103664208A CN 103664208 A CN103664208 A CN 103664208A CN 201310605502 A CN201310605502 A CN 201310605502A CN 103664208 A CN103664208 A CN 103664208A
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Prior art keywords
hercynite
mud
production method
sintering
sintering production
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CN201310605502.2A
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黄克忠
周红军
张东方
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HENAN RONGAN HEAT ENGINEERING NEW MATERIAL Co Ltd
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HENAN RONGAN HEAT ENGINEERING NEW MATERIAL Co Ltd
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Abstract

The invention belongs to the technical field of fire resistant material production, and particularly relates to a wet process sintering production method for hercynite. The wet process sintering production method comprises the following steps: compounding 50-65% of aluminium oxide and 35-50% of metallic iron powder according to weight percentage, adding graphite, polyvinyl alcohol and water, grinding so as to obtain mud A, and performing dehydrating, vacuum pugging, drying and sintering on the mud A so as to obtain the hercynite, wherein the dosage of the graphite and the polyvinyl alcohol is respectively 1-5% and 0.1-0.3% of the total mass of the aluminium oxide and the metallic iron powder, and the amount of water is 1.0-1.2 times of the total mass of the aluminium oxide, the metallic iron powder, the graphite and the polyvinyl alcohol. The wet process sintering production method is simple in technology, low in labor intensity, environment-friendly and low in cost, the obtained hercynite is uniform in components and high in volume density, and the crystalline phase content reaches 97%.

Description

A kind of wet method sintering production method of hercynite
Technical field
The invention belongs to refractory materials production technical field, relate in particular to a kind of wet method sintering production method of hercynite.
Background technology
Past dry method cement rotary kiln sintering zone is main mainly with magnesia chrome brick greatly with refractory materials, but with Cr a small amount of in rear magnesia chrome brick 6+a kind of water miscible carcinogenic ion, contaminate environment.Cr in the residual brick of magnesium chromium after cement rotary kiln is used 6+content be about 0.1-0.5%, it mainly contains harmful substances is K 2crO 4, be a kind of weak oxide compound, chemical stability is high, and in many occasions, these contain Cr 6+compound in nature, causes long-term pollution to environment by stable existence.Refractory materials worker is seeking new material replacement magnesia chrome brick in recent years, therefore hercynite will be the development trend of refractory materials for cement rotary kiln sintering zone.
In application number CN200510019267.6, " a kind of method of synthesizing ferrum-aluminium spinelle " mentioned and adopted buried charcoal sintering, and wayward ferriferous oxide changes the degree of fe in actual production, the difficulty of therefore synthetic sintered iron aluminate is larger, and does not realize so far suitability for industrialized production.
In application number CN101823872.A, " a kind of method of synthesizing ferrous aluminum spinel " mentioned iron containing compounds and aluminum contained compound by Fe n+: Al 3+mol ratio carry out proportioning at 1: 2, the bonding agent of additional said mixture weight 1-6%, through mixing, compacting, dry after under nitrogen atmosphere sintering make, sintering temperature is 1300-1700 ℃, soaking time is 2-12 hour.This technique is to kiln, and manufacturing technique requirent is complicated, is difficult to be implemented in production.
Conventionally hercynite all adopts electric smelting method to produce, and is about to after chloride raw material and iron filings mix by a certain percentage put into electric furnace, adopts the electric smelting of 90-220V voltage, all after melting, continues melting 25-60 minute; Or by the cooling 24-48 hour in electric arc furnace of the high temperature synthetic material after melting.This method power cost is very high, seriously restricts the popularization of product.
Summary of the invention
In order to address the above problem, object of the present invention aims to provide a kind of wet method sintering production method of hercynite, its advantage is that technique is simple, labour intensity is low, environmental protection and cost low, gained hercynite composition is even, volume density is high, and crystal content reaches 97%.
For achieving the above object, the technical scheme that the present invention takes is as follows:
A kind of wet method sintering production method of hercynite: by after the metal iron powder batching of the aluminum oxide of 50-65% and 35-50%, add graphite, polyvinyl alcohol, water by mass percentage, grind and obtain mud A; Mud A, through dehydration, vacuum pugging, dry, sintering, obtains hercynite; Wherein the consumption of graphite and polyvinyl alcohol is respectively 1-5%, the 0.1-0.3% of aluminum oxide and metal iron powder total mass, and the water yield is aluminum oxide, metal iron powder, graphite and polyvinyl alcohol total mass 1.0-1.2 times.
Preferably, described aluminum oxide is Alpha-alumina or gama-alumina, aluminum oxide purity >=98%(quality), metal iron powder purity >=95%(quality); Polyvinyl alcohol viscosity is at 15-30 mpas.
Preferably, to tail over be 325 order < 5% to the grain graininess of mud A.
Further, described dehydration, vacuum pugging, drying process are: mud A is pumped into the mud cake B that dewaters to obtain in pressure filter, adopt de-airing extruder to carry out vacuum pugging, extruding to mud cake B, formation mud section C after cutting, then mud section C is sent into the dry D of the obtaining material of chain dryer.
Further again, pressure filter dewatering pressure must not be greater than 2.5Mpa, and mud cake B moisture is less than 28%; Vacuum tightness >=0.085Mpa in de-airing extruder; D material residual water-content is less than 1%.
Preferably, when dry, parameter is: temperature 250-280 ℃, time 60-90min.
Preferably, during sintering, parameter is: temperature 1650-1700 ℃, soaking time 15-30min, whole sintering time 10-15h.
Preferably, sintering in rotary kiln.
The present invention adopts a kind of production technique sintered iron aluminate of full wet method, makes hercynite, and composition is even, and volume density is high, and crystal content reaches 97%, its advantage:
(1), the present invention makes the product identical in quality with electric smelting gained hercynite with wet method sintering method, and is implemented in production.
(2), wet method sintered iron aluminate production cost is more much lower than fused hercynite production cost, and has the features such as environmental protection, labour intensity is low, output is large.
(3), gained hercynite detects through XRD, hercynite crystalline phase reaches 97%, section is black light colour, quality is fine and close, is a kind of refractory raw material of very high-quality.
(4), when wet method sintered iron aluminate, add graphite, making furnace atmosphere is reducing atmosphere, through fully mixing, has guaranteed that ferriferous raw material becomes the transformation degree of iron protoxide.
(5), when wet method sintered iron aluminate, add polyvinyl alcohol or polyacrylamide, guarantee after material forming the intensity in the transportations such as dry, sintering.
(6), hercynite adopts rotary kiln tunnel furnace, greatly reduced sintering time, improved output, reduced costs.
Embodiment
Embodiment 1:
Take commercial alumina primary aluminum and iron sponge powder as raw material, and the method for wet method SINTERING PRODUCTION hercynite, comprises the following steps:
A: batching, grind: by mass percentage by after 120 order iron sponge powders (Fe mass content >=95%) batching of 50% gama-alumina primary aluminum (quality of alumina content >=98%) and 50%, add 1% crystalline flake graphite, 0.1% polyvinyl alcohol (viscosity 15 mpas) and water, in ball mill by wet process, grind, it is to calculate basis that wherein said crystalline flake graphite, polyvinyl alcohol consumption all be take aluminum oxide and iron sponge powder total mass, and described quality is 1.0 times of unclassified stores total mass; According to the particle fineness analysis of material in mud, grind 15 hours blowings, it is that 325 orders are less than 1%(quality that the rear mud particle granularity of grinding tails over), obtain mud A;
B: mud A is pumped in pressure filter and dewatered with slush pump, and the mud cake moisture obtaining according to press filtration regulates filter mud pressure (must not be greater than 2.5Mpa), and after 10 minutes, obtaining moisture is 20%(quality) mud cake B;
C: vacuum pugging: employing vacuum tightness is that the de-airing extruder of 0.085 Mpa carries out vacuum pugging to mud cake B, and through extruding, obtaining diameter is 20 millimeters, and length is the cylindrical mud section of 50 millimeters, forms mud section C after cutting;
D: dry: mud section C is sent into chain dryer, and described chain dryer medial temperature 250 is spent, and drying time was at 90 minutes, and obtaining residual water-content is 0.5%(quality) D material;
E: sintering: D material is sent into sintering in rotary kiln, and sintering temperature is 1650 ℃, and soaking time is 30 minutes, total sintering time is 15 hours, obtains hercynite after kiln discharge.Hercynite volume density is 3.70g/cm after testing 3, through XRD, detecting crystal content is 93%.
Embodiment 2
Take calcining Alpha-alumina and metal iron powder is raw material, and the method for wet method SINTERING PRODUCTION hercynite, comprises the following steps:
A: batching, grind: by mass percentage by after 120 order metal iron powders (Fe mass content >=95%) batching of 65% Alpha-alumina primary aluminum (quality of alumina content >=98%) and 35%, add 5% crystalline flake graphite, 0.3% polyvinyl alcohol (viscosity 30mpas) and water, in ball mill by wet process, grind, it is to calculate basis that wherein said crystalline flake graphite, polyvinyl alcohol all be take aluminum oxide and metal iron powder total mass, and described quality is 1.2 times of unclassified stores total mass.According to the particle fineness of material in mud, give and analyze, grind 15 hours blowings, it is that 325 orders are less than 1%(quality that the rear mud particle granularity of grinding tails over), obtain mud A;
B: A material is pumped in pressure filter and dewatered with slush pump, and the mud cake moisture obtaining according to press filtration regulates filter mud pressure (must not be greater than 2.5Mpa), and after 10 minutes, obtaining moisture is 28%(quality) mud cake B;
C: vacuum pugging: employing vacuum tightness is that the de-airing extruder of 0.085 Mpa carries out vacuum pugging to mud cake B, and through extruding, obtaining diameter is 25 millimeters, and length is the cylindrical mud section of 50 millimeters, forms mud section C after cutting;
D: dry: mud section C is sent into chain dryer, and described chain dryer medial temperature 280 is spent, and drying time was at 60 minutes, and obtaining residual water-content is 0.5%(quality) D material.
E: sintering: D material is sent into sintering in rotary kiln, and sintering temperature is 1700 ℃, and soaking time is 30 minutes, total sintering time is 10 hours, obtains hercynite after kiln discharge.Hercynite volume density is 3.68g/cm after testing 3, through XRD, detecting crystal content is 97%.
In above-described embodiment, the mensuration of volume density is with reference to GB/T2999-2002.
In above-mentioned example, main raw material aluminum oxide and metal iron powder, the order of addition of graphite, polyvinyl alcohol and water can be also first to add graphite and polyvinyl alcohol, then limit adds water in limit when adding aluminum oxide and metal iron powder, then in ball mill by wet process, grinds.
In above-mentioned example, diameter and shape that vacuum pugging obtains mud section C also can change according to production practical situation.
Obviously; above-mentioned example is only for giving an example of doing is clearly described; but not restriction to embodiment; to those of ordinary skill in the art; can also make different changes and variation on the basis of the above description, and the apparent variation of being amplified out thus or change are still among institute of the present invention protection domain.

Claims (8)

1. a wet method sintering production method for hercynite, is characterized in that: by after the metal iron powder batching of the aluminum oxide of 50-65% and 35-50%, add graphite, polyvinyl alcohol, water by mass percentage, grind and obtain mud A; Mud A, through dehydration, vacuum pugging, dry, sintering, obtains hercynite; Wherein the consumption of graphite and polyvinyl alcohol is respectively 1-5%, the 0.1-0.3% of aluminum oxide and metal iron powder total mass, and the water yield is aluminum oxide, metal iron powder, graphite and polyvinyl alcohol total mass 1.0-1.2 times.
2. the wet method sintering production method of hercynite as claimed in claim 1, is characterized in that: described aluminum oxide is Alpha-alumina or gama-alumina aluminum oxide purity >=98%, metal iron powder purity >=95%; Polyvinyl alcohol viscosity is at 15-30 mpas.
3. the wet method sintering production method of hercynite as claimed in claim 1 or 2, is characterized in that: it is 325 order < 5% that the grain graininess of mud A tails over.
4. the wet method sintering production method of hercynite as claimed in claim 1 or 2, it is characterized in that described dehydration, vacuum pugging, drying process are: mud A is pumped into the mud cake B that dewaters to obtain in pressure filter, adopt de-airing extruder to carry out vacuum pugging, extruding to mud cake B, after cutting, form mud section C, then it is dry that D expects that mud section C is sent into chain dryer.
5. the wet method sintering production method of hercynite as claimed in claim 4, is characterized in that: pressure filter dewatering pressure≤2.5Mpa, mud cake B moisture < 28%; Vacuum tightness >=0.085Mpa in de-airing extruder; D material residual water-content < 1%.
6. the wet method sintering production method of hercynite as claimed in claim 1 or 2, is characterized in that when dry, parameter is: temperature 250-280 ℃, time 60-90min.
7. the wet method sintering production method of hercynite as claimed in claim 1 or 2, while it is characterized in that sintering, parameter is: temperature 1650-1700 ℃, soaking time 15-30min, whole sintering time 10-15h.
8. the wet method sintering production method of hercynite as claimed in claim 7, is characterized in that: sintering in rotary kiln.
CN201310605502.2A 2013-11-26 2013-11-26 Wet process sintering production method for hercynite Pending CN103664208A (en)

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104591292A (en) * 2014-07-08 2015-05-06 河北科技大学 Hercynite synthesis method
CN104803422A (en) * 2015-03-30 2015-07-29 同济大学 Preparation method of nanoscale hercynite
CN105133001A (en) * 2015-08-31 2015-12-09 北京科技大学 Preparing method for large-dimension octahedral hercynite single crystal
CN105886880A (en) * 2016-04-29 2016-08-24 武汉科技大学 Low-carbon iron-aluminum alloy and preparation method thereof
CN113880567A (en) * 2021-10-29 2022-01-04 河南安培新材料科技有限公司 Method for preparing hercynite from aluminum ash

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101654365A (en) * 2009-09-22 2010-02-24 武汉科技大学 Fused hercynite-corundum composite material and preparation method thereof
CN101913630A (en) * 2010-08-06 2010-12-15 三门峡市新仰韶合成料有限公司 Wet production process of magnesia-alumina spinel
CN102583462A (en) * 2012-01-17 2012-07-18 中钢集团洛阳耐火材料研究院有限公司 Method for synthesizing hercynite
CN102603315A (en) * 2012-03-01 2012-07-25 河南科技大学 Preparation method of hercynite

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101654365A (en) * 2009-09-22 2010-02-24 武汉科技大学 Fused hercynite-corundum composite material and preparation method thereof
CN101913630A (en) * 2010-08-06 2010-12-15 三门峡市新仰韶合成料有限公司 Wet production process of magnesia-alumina spinel
CN102583462A (en) * 2012-01-17 2012-07-18 中钢集团洛阳耐火材料研究院有限公司 Method for synthesizing hercynite
CN102603315A (en) * 2012-03-01 2012-07-25 河南科技大学 Preparation method of hercynite

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104591292A (en) * 2014-07-08 2015-05-06 河北科技大学 Hercynite synthesis method
CN104591292B (en) * 2014-07-08 2016-07-13 河北科技大学 A kind of method of synthesizing ferrum-aluminium spinelle
CN104803422A (en) * 2015-03-30 2015-07-29 同济大学 Preparation method of nanoscale hercynite
CN105133001A (en) * 2015-08-31 2015-12-09 北京科技大学 Preparing method for large-dimension octahedral hercynite single crystal
CN105133001B (en) * 2015-08-31 2017-10-24 北京科技大学 A kind of preparation method of the hercynite monocrystalline of large scale octahedral build
CN105886880A (en) * 2016-04-29 2016-08-24 武汉科技大学 Low-carbon iron-aluminum alloy and preparation method thereof
CN113880567A (en) * 2021-10-29 2022-01-04 河南安培新材料科技有限公司 Method for preparing hercynite from aluminum ash

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Application publication date: 20140326