CN105271339A - Preparation method for rho-aluminium oxide binder - Google Patents

Preparation method for rho-aluminium oxide binder Download PDF

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CN105271339A
CN105271339A CN201510663161.3A CN201510663161A CN105271339A CN 105271339 A CN105271339 A CN 105271339A CN 201510663161 A CN201510663161 A CN 201510663161A CN 105271339 A CN105271339 A CN 105271339A
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powder
aluminum oxide
bonding agent
preparation
oxide bonding
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CN105271339B (en
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周德福
邹少华
邹磊
赵玉涛
陶然
贾志宏
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NANJING CHANGJIANG INDUSTRIAL FURNACE TECHNOLOGY CO LTD
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NANJING CHANGJIANG INDUSTRIAL FURNACE TECHNOLOGY CO LTD
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  • Powder Metallurgy (AREA)

Abstract

The invention relates to a preparation method for a rho-aluminium oxide binder. The preparation method comprises: performing microwave dewatering on Al(OH)3 to form a powder, then performing crushing processing on the powder, and then performing vacuum heating, so as to obtain the rho-aluminium oxide binder, and preserving the rho-aluminium oxide binder by performing sealing. The method is high in technology controllability, is capable of effectively controlling the powder purity, is easy for industrialized production, and possesses extremely high practical application value.

Description

The preparation method of a kind of ρ-aluminum oxide bonding agent
Technical field
The present invention relates to a kind of high-purity high-content ρ-alumina powder jointed, this powder has high reactivity, normal temperature hydrating capacity, can be used as preparing the bonding agent in high purity aluminium oxide sintered compact.
Background technology
ρ-aluminum oxide is the one of aluminum oxide crystal formation, be the senior bonding agent of one grown up in recent decades, this aluminum oxide very easily absorbs moisture, again aquation and form hydrated alumina, after the reaction, a kind of hard block is formed by meal or slurry; And have high temperature resistant, intensity is high, volume stability is strong, the advantage such as corrosion-resistant, is therefore widely used in the fields such as high grade refractory, ceramic coating, support of the catalyst, sorbent material, siccative.Particularly in senior unshape refractory, having special performance, both played bonding agent effect, itself is again high grade refractory.The hydrated alumina formed because of ρ-aluminum oxide aquation can change the α-Al with good properties at high temperature into 2o 3, therefore with ρ-aluminum oxide for bonding agent, can solve due to the introducing of impurity element the problem that high purity aluminium oxide material has a negative impact.
ρ-aluminum oxide bonding agent that general industry obtains is ρ-Al 2o 3, χ-Al 2o 3with remaining Al (OH) 3mixture, ρ-alumina content higher its bonding effect better, the usual ρ-alumina content ρ more than 50%-aluminum oxide bonding agent just can be used for industrial production.
Preparation method the most frequently used is at present rapid dehydration method.Chinese patent literature CN1608726A discloses a kind of rapid dehydration method and prepares ρ-aluminum oxide, be that raw material is after shattering process with aluminium hydroxide, shower roasting 850 ~ 950 DEG C, 0.1 ~ 01s obtain ρ-aluminum oxide, the method technique is simple, cost is low, but because the method needs to be rapidly heated, to lower the temperature, technique is difficult to control; Whole technological process exposes in atmosphere, and the moisture easily absorbed in air reduces content.
Above-mentioned technique also exists technique difficulty and controls, and the shortcomings such as ρ-alumina content low (ρ-alumina content is about 50%), so for problems of the prior art, the defect overcome in prior art is very necessary.
Summary of the invention
The object of the invention is to solve the deficiencies in the prior art, provide a kind of preparation method of novel ρ-aluminum oxide bonding agent, this technique is simple and easy to control, and obtained ρ-aluminum oxide bonding agent has the advantage of high purity, high-content.
Technical scheme
The preparation method of ρ of the present invention-aluminum oxide bonding agent: by Al (OH) 3slurry carries out microwave dehydration and becomes powder, then carries out pulverization process to powder, then carries out heating under vacuum, obtains ρ-aluminum oxide bonding agent, preserves its sealing.
Described Al (OH) 3slurry purity is greater than activated aluminum powder that 99.999% high-purity aluminium ingot powder by atomization obtains to be hydrolyzed the product of reaction.
Further, the temperature of described microwave dehydration is 80 ~ 120 DEG C, and the time is 20 ~ 60min.Described microwave dehydration adopts continuous-type microwave dehydration equipment.This equipment adopts tetrafluoroethylene as conveyor materials, and its advantage does not contact with other materials in dehydration, can not be mixed into impurity, can ensure the purity of material; And facilitate scale operation.
Further, described pulverization process is comminution by gas stream mode, and stream pressure is 1 ~ 2MPa, and the powder granularity after pulverizing is 0.5 ~ 5 μm.
Further, described heating under vacuum was divided into for four stages: the first stage is warming up to 180 ~ 200 DEG C with the speed of 5 ~ 8 DEG C/min; Subordinate phase is warming up to 450 ~ 600 DEG C with the speed of 7 ~ 10 DEG C/min; Phase III is at this temperature 1 ~ 2h; Finally lower the temperature with stove.Heating under vacuum can ensure not contact wetting in the process of heating, prevents it from hydration reaction occurring, can ensure the content of ρ-aluminum oxide bonding agent.
ρ-aluminum oxide bonding agent is poured into sealing bag, is placed in drying basin and preserves after referring to and taking out from stove by described sealing preservation immediately, and its preservation process contacts any moisture hardly, prevents it from hydration reaction occurring, can ensure the content of ρ-aluminum oxide bonding agent.
The purity of ρ-aluminum oxide bonding agent prepared by the inventive method is greater than 99.999%, granularity is micron order (being less than 5 μm) and be evenly distributed without obviously reuniting, the content of ρ-aluminum oxide is higher than 60%.Advantage of the present invention: (1), due to omnidistance heating under vacuum, technique is easy to control, and is easy to suitability for industrialized production; (2) whole process carries out contacting any impurity, can be good at controlling purity; (3) ρ-alumina content prepared is high, granularity is little, has very high actual application value.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention;
Fig. 2 is the Electronic Speculum figure of ρ of the present invention-aluminum oxide bonding agent;
Fig. 3 is the sreen analysis graphic representation of ρ of the present invention-aluminum oxide bonding agent.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
High-purity Al (OH) that following embodiment adopts 3slurry purity is greater than activated aluminum powder that 99.999% high-purity aluminium ingot powder by atomization obtains to be hydrolyzed the product of reaction, and concrete purity test is in table 1.
Table 1 aluminium hydroxide elemental composition table
Embodiment 1
High-purity Al (OH) 3slurry carries out 80 DEG C × 60min microwave dehydration and becomes powder, and powder is carried out comminution by gas stream process; The powder pulverized is placed in vacuum oven (vacuum tightness is 1 ~ 2Pa), first stage is warming up to 200 DEG C with the speed of 5 DEG C/min, subordinate phase is warming up to 450 DEG C with the speed of 10 DEG C/min, phase III is at this temperature 1h, finally with stove cooling, obtain ρ-aluminum oxide bonding agent that purity is 99.999% (concrete purity test report is in table 2), granularity is 0.9 μm (concrete sreen analysis graphic representation as shown in Figure 3), content is 75.6%.
Table 2 ρ-aluminum oxide bonding agent elemental composition table
Embodiment 2
High-purity Al (OH) 3slurry carries out 80 DEG C × 60min microwave dehydration and becomes powder, and powder is carried out comminution by gas stream process; The powder pulverized is placed in vacuum oven (vacuum tightness is 1 ~ 2Pa), first stage is warming up to 200 DEG C with the speed of 7 DEG C/min, subordinate phase is warming up to 500 DEG C with the speed of 8 DEG C/min, phase III is at this temperature 2h, finally with stove cooling, obtain ρ-aluminum oxide bonding agent that purity is 99.999%, granularity is 5 μm, content is 67.3%.
Embodiment 3
High-purity Al (OH) 3slurry carries out 80 DEG C × 60min microwave dehydration and becomes powder, and powder is carried out comminution by gas stream process; The powder pulverized is placed in vacuum oven (vacuum tightness is 1 ~ 2Pa), first stage is warming up to 200 DEG C with the speed of 5 DEG C/min, subordinate phase is warming up to 550 DEG C with the speed of 10 DEG C/min, phase III is at this temperature 1h, finally with stove cooling, obtain ρ-aluminum oxide bonding agent that purity is 99.999%, granularity is 2 μm, content is 60.4%.

Claims (4)

1. a preparation method for ρ-aluminum oxide bonding agent, is characterized in that, by Al (OH) 3slurry carries out microwave dehydration and becomes powder, then carries out pulverization process to powder, then carries out heating under vacuum, obtains ρ-aluminum oxide bonding agent, preserves its sealing;
Described Al (OH) 3slurry purity is greater than activated aluminum powder that 99.999% high-purity aluminium ingot powder by atomization obtains to be hydrolyzed the product of reaction.
2. the preparation method of ρ-aluminum oxide bonding agent as claimed in claim 1, it is characterized in that, the temperature of described microwave dehydration is 80 ~ 120 DEG C, and the time is 20 ~ 60min.
3. the preparation method of ρ-aluminum oxide bonding agent as claimed in claim 1, it is characterized in that, described pulverization process is comminution by gas stream mode, and stream pressure is 1 ~ 2MPa, and the powder granularity after pulverizing is 0.5 ~ 5 μm.
4. the preparation method of the ρ-aluminum oxide bonding agent as described in claim 1 or 2 or 3, it is characterized in that, described heating under vacuum was divided into for four stages: the first stage is warming up to 180 ~ 200 DEG C with the speed of 5 ~ 8 DEG C/min; Subordinate phase is warming up to 450 ~ 600 DEG C with the speed of 7 ~ 10 DEG C/min; Phase III is at this temperature 1 ~ 2h; Finally lower the temperature with stove.
CN201510663161.3A 2015-10-14 2015-10-14 A kind of ρ aoxidizes the preparation method of Al binding agent Expired - Fee Related CN105271339B (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112174177A (en) * 2020-10-13 2021-01-05 中国铝业股份有限公司 Hydraulic alumina and preparation method thereof

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DD248108A1 (en) * 1986-04-14 1987-07-29 Leuna Werke Veb METHOD FOR THE PRODUCTION OF PRACTICALLY PURE RAW ALUMINUM OXIDE
CN1394807A (en) * 2002-07-09 2003-02-05 刘明 Preparation method of high-purity superfine alumina powder body
CN1608726A (en) * 2003-03-04 2005-04-27 中国铝业股份有限公司 Production process of adsorbent active alumina ball
CN103818939A (en) * 2014-01-14 2014-05-28 淄博贝格工贸有限公司 Aluminum oxide specially used for hydrogen peroxide fluidized bed and production technology for aluminum oxide

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DD248108A1 (en) * 1986-04-14 1987-07-29 Leuna Werke Veb METHOD FOR THE PRODUCTION OF PRACTICALLY PURE RAW ALUMINUM OXIDE
CN1394807A (en) * 2002-07-09 2003-02-05 刘明 Preparation method of high-purity superfine alumina powder body
CN1608726A (en) * 2003-03-04 2005-04-27 中国铝业股份有限公司 Production process of adsorbent active alumina ball
CN103818939A (en) * 2014-01-14 2014-05-28 淄博贝格工贸有限公司 Aluminum oxide specially used for hydrogen peroxide fluidized bed and production technology for aluminum oxide

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
李晓明等: "《特种不定形耐火材料及不烧耐火砖》", 30 September 1992, 冶金工业出版社 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112174177A (en) * 2020-10-13 2021-01-05 中国铝业股份有限公司 Hydraulic alumina and preparation method thereof

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