CN104311006A - Simple method for preparing zirconia fiber bricks - Google Patents

Simple method for preparing zirconia fiber bricks Download PDF

Info

Publication number
CN104311006A
CN104311006A CN201410557194.5A CN201410557194A CN104311006A CN 104311006 A CN104311006 A CN 104311006A CN 201410557194 A CN201410557194 A CN 201410557194A CN 104311006 A CN104311006 A CN 104311006A
Authority
CN
China
Prior art keywords
brick
mol
simple method
yttrium oxide
zirconium white
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201410557194.5A
Other languages
Chinese (zh)
Other versions
CN104311006B (en
Inventor
白佳海
唐钰栋
杜庆洋
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Shandong University of Technology
Original Assignee
Shandong University of Technology
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Shandong University of Technology filed Critical Shandong University of Technology
Priority to CN201410557194.5A priority Critical patent/CN104311006B/en
Publication of CN104311006A publication Critical patent/CN104311006A/en
Application granted granted Critical
Publication of CN104311006B publication Critical patent/CN104311006B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Abstract

The invention provides a simple method for preparing zirconia (3mol percent of yttria) fiber bricks, belonging to the technical field of preparation of ceramic fiber materials. The simple method for preparing zirconia (3mol percent of yttria) fiber bricks is characterized by comprising the following steps: (1) dissolving a zircon salt, yttrium nitrate, urea and an auxiliary agent into distilled water so as to prepare a solution; (2) sewing a cotton-containing fabric into a brick shape; (3) soaking the brick shaped fabric into the solution for 10 minutes, taking the fabric out, extruding to remove excessive moisture, further blowing excessive moisture by using a blower, and drying at the temperature of 50 DEG C for 20 hours; and (4) putting the soaked and dried brick shaped fabric into a tunnel kiln, rapidly heating and raising the temperature to 400-800 DEG C, slowly heating and raising the temperature to 1200-1650 DEG C, preserving the temperature for 0.5-1 hour, and sintering. The method disclosed by the invention is simple in process and equipment, convenient to operate, low in energy consumption, low in cost and convenient for large-scale production.

Description

A kind of simple method preparing Zirconium oxide fibre brick
Technical field
The invention provides the simple method that one prepares zirconium white (3 mol% yttrium oxide) fiber brick, belong to ceramic fiber material preparing technical field.
Background technology
Zirconium oxide fibre brick has high temperature resistant, the advantage such as intensity is high, good toughness, porosity are high, specific surface area is large, heat-insulation and heat-preservation, can be used as high-temperature flame-proof lagging material, the sorbent material of toxic substance, support of the catalyst, film support and chemical filler etc.The preparation method of traditional fibre brick is heated to high temperature original ingredient and makes its melting, with getting rid of the processes for forming cellulose such as silk, wire drawing, and then utilizes the technology such as bonding, compacting, high temperature sintering to be prepared into fiber brick.Because zirconic fusing point is up to 2700 DEG C, if use traditional scorification to prepare highly purified Zirconium oxide fibre brick, then have that energy consumption is high, equipment is complicated, high in cost of production shortcoming, this strongly limits the application of high-purity mangesium oxide zirconium fiber brick in high-temperature flame-proof lagging material, support of the catalyst, toxic substance sorbent material and film support etc.In addition, use wet chemical method (mainly sol-gel processing) to prepare technological process and the equipment complexity of Zirconium oxide fibre both at home and abroad, cost is high; If bondd further, suppress, sinter brick into, cost can improve further, this seriously inhibits widespread use and the popularization of Zirconium oxide fibre brick.
On the other hand, along with increasing of China's expanding economy and the size of population, the consumption of textiles increases sharply, a large amount of waste textile by as garbage bury, burning, both cause the waste of resource, also result in environmental pollution.Therefore, develop and effectively technology is utilized to waste textile, can economic benefit be produced, also there is huge social benefit.The present invention is to provide a kind of preparation method of simple zirconium white (3 mol% yttrium oxide) fiber brick.The method can with new be template containing cotton cloth, but have more meaning be can directly with washes clean waste and old containing cotton cloth as template, also can use regeneration containing cotton cloth as template.That a kind of cotton cloth that contains of concrete selection, as template, depends on the Application Areas of produced Zirconium oxide fibre brick.The Zirconium oxide fibre brick produced as the present invention as chemical filler or lagging material (envrionment temperature of application is no more than 1500 DEG C), directly can adopt washes clean waste and old be template containing cotton cloth; The Zirconium oxide fibre brick produced as the present invention as high temperature (higher than 1800 DEG C) flame-proof thermal insulation material, then need to select new containing cotton cloth or highly purified regeneration containing cotton cloth as template.Therefore, provided by the invention with containing the method for cotton cloth for template production Zirconium oxide fibre brick, except there is wide economic outlook, also there is huge social benefit.
The present invention is to provide a kind of simple method to be Template preparation zirconium white (3mol% yttrium oxide) fiber brick containing cotton cloth, the method has the advantages such as equipment is simple, energy consumption is low, cost is low, convenient operation, is convenient to realize commercial scale production.
Summary of the invention
The zirconium white (3 mol% yttrium oxide) fiber brick, the i.e. ZrO that the object of this invention is to provide a kind of technique simple, easy to operate, energy consumption is low, cost is low, are produced on a large scale 2(3% mol Y 2o 3) preparation method of fiber brick, its technical scheme is:
One prepares the simple method of zirconium white (3 mol% yttrium oxide) fiber brick, it is characterized in that adopting following steps: (1) is dissolved into zirconates, Yttrium trinitrate, urea, auxiliary in distilled water and is mixed with solution; (2) brick shape is sewn into containing cotton cloth; (3) described brick shape cloth is put into above-mentioned solution to soak 10 minutes; Carry out after taking-up extruding to get rid of unnecessary moisture, then blow out unnecessary moisture further with blower, and at 50 DEG C dry 20 hours.(4) described immersion, dried brick shape cloth are put into tunnel furnace, rapid heating is warmed up to 400-800 DEG C, then slowly heats to 1200-1650 DEG C and is incubated 0.5-1 hour sintering.
Described one prepares the simple method of zirconium white (3 mol% yttrium oxide) fiber brick, it is characterized in that the one of the zirconates described in step (1) mainly in zirconium nitrate, Zircosol ZN, zirconium oxychloride.
Described one prepares the simple method of zirconium white (3 mol% yttrium oxide) fiber brick, it is characterized in that Zr in the solution described in step (1) 4+concentration be 0.3-0.8 mol/L, Y 3+concentration be Zr 4+concentration 6%, the concentration of urea is 0.5-2.0 mol/L.
Described one prepares the simple method of zirconium white (3 mol% yttrium oxide) fiber brick, and the auxiliary that it is characterized in that in step (1) refers to the one in polyvinyl alcohol, polyoxyethylene glycol, polypropylene glycol; The add-on of auxiliary is 1 ~ 5 % of urea quality.
The preparation method of the simple zirconium white of described one (3 mol% yttrium oxide) fiber brick, it is characterized in that the cotton cloth that contains in step (2) refers to that the mass percentage of cotton fibre in cloth is 80-90%, the mass percentage of polyster fibre is 5-15%, and the mass percentage of spandex fibre is 5-10 %.
Described one prepares the simple method of zirconium white (3 mol% yttrium oxide) fiber brick, and it is characterized in that in step (2) can being new for cotton cloth containing cotton cloth, also can be waste and old containing cotton cloth, can also be that regeneration is containing cotton cloth.
The preparation method of described a kind of simple sapphire whisker brick, is characterized in that the rapid heating intensification in step (4) refers to that heat-up rate is 20-50 DEG C/min.
Described one prepares the simple method of zirconium white (3 mol% yttrium oxide) fiber brick, and the slow heat temperature raising in step (4) refers to that heat-up rate is 0.1 ~ 1 DEG C/min.
Compared with prior art, tool has the following advantages in the present invention:
1. the present invention is to provide the wet chemical method that one prepares zirconium white (3 mol% yttrium oxide) fiber brick, without the need to original ingredient being heated to high temperature and making its melting, the subsequent technique process such as also do not bond, shaping, therefore technique is simple, operational safety, energy consumption is low, and total cost is low, and is easy to realize industrialization;
2. zirconium white (the 3 mol% yttrium oxide) fiber brick prepared by the present invention and the described brick shape cloth as template have identical texture structure, the length and diameter etc. of the shape of Zirconium oxide fibre brick, size and fiber, depend primarily on containing the staple length and diameter etc. in the shape of cotton cloth, size and cloth.Therefore, the length and diameter etc. of the shape of the Zirconium oxide fibre brick prepared by the present invention, size and fiber can control according to actual needs and flexibly;
3. the method preparing zirconium white (3 mol% yttrium oxide) fiber brick provided by the invention, can be used for preparing some abnormity (as wedge brick, arch brick etc.) fire resistant heat preserving fiber brick;
4. in the preparation method of zirconium white provided by the present invention (3 mol% yttrium oxide) fiber brick, available washes clean waste and old containing cotton cloth or regeneration containing cotton cloth be template, realize the recycling of scrap fabric, there is huge economic benefit and social benefit.
Embodiment
Embodiment 1
Basic zirconium chloride, Yttrium trinitrate, urea and polyvinyl alcohol (auxiliary) are dissolved in distilled water and are mixed with solution, control Zr 4+0.3 mol/L, 0.018 mol/L and 0.5 mol/L respectively with the concentration of urea.Wherein, the addition of polyvinyl alcohol is 1% of urea quality.New is sewn into brick shape containing cotton cloth (cotton content 80wt%, terylene 10 wt%, spandex 10 wt%); Brick shape cloth is put into above-mentioned solution to soak 10 minutes; Carry out after taking-up extruding to get rid of unnecessary moisture, then blow out unnecessary moisture further with blower, and at 50 DEG C dry 20 hours.Described immersion, dried brick shape cloth are put into tunnel furnace, with the heating rate of 20 DEG C/min to 400 DEG C, is then being warmed up to 1650 DEG C with the heating rate of 0.1 DEG C/min and is being incubated 0.5 hour sintering; Zirconium white (3 mol% yttrium oxide) fiber brick can be prepared after cooling.
Embodiment 2
Zircosol ZN, Yttrium trinitrate, urea and polyoxyethylene glycol (auxiliary) are dissolved in distilled water and are mixed with solution, control Zr 4+, Y 3+0.6 mol/L, 0.036 mol/L and 1.2 mol/L respectively with the concentration of urea.Wherein, the addition of polyoxyethylene glycol is 2 % of urea quality.New is sewn into brick shape containing cotton cloth (cotton content 87wt%, terylene 5 wt%, spandex 8 wt%); Brick shape cloth is put into above-mentioned solution to soak 10 minutes; Carry out after taking-up extruding to get rid of unnecessary moisture, then blow out unnecessary moisture further with blower, and at 50 DEG C dry 20 hours.Described immersion, dried brick shape cloth are put into tunnel furnace, with the heating rate of 30 DEG C/min to 600 DEG C, is then warmed up to 1200 DEG C with the heating rate of 1 DEG C/min and is incubated 1 hour sintering; Zirconium white (3mol% yttrium oxide) fiber brick can be prepared after cooling.
Embodiment 3
Basic zirconium chloride, Yttrium trinitrate, urea and polypropylene glycol (auxiliary) be dissolved in distilled water and be mixed with solution, control Zr 4+, Y 3+0.8 mol/L, 0.048 mol/L and 2 mol/L respectively with the concentration of urea.Wherein, the addition of polypropylene glycol is 3% of urea quality.Regeneration is sewn into brick shape containing cotton cloth (cotton content 90 wt%, terylene 5 wt%, spandex 5 wt%); Brick shape cloth is put into above-mentioned solution to soak 10 minutes; Carry out after taking-up extruding to get rid of unnecessary moisture, then blow out unnecessary moisture further with blower, and at 50 DEG C dry 20 hours.Described immersion, dried brick shape cloth are put into tunnel furnace, with the heating rate of 40 DEG C/min to 500 DEG C, is then warmed up to 1600 DEG C with the heating rate of 0.3 DEG C/min and is incubated 0.5 hour sintering; Zirconium white (3mol% yttrium oxide) fiber brick can be prepared after cooling.
Embodiment 4
Zirconium nitrate, Yttrium trinitrate, urea and polyvinyl alcohol (auxiliary) are dissolved in distilled water and are mixed with solution, control Zr 4+, Y 3+0.5 mol/L, 0.03 and 1.0 mol/L respectively with the concentration of urea.Wherein, the addition of polyvinyl alcohol is 5% of urea quality.Regeneration is sewn into brick shape containing cotton cloth (cotton content 86wt%, terylene 6 wt%, spandex 8 wt%); Brick shape cloth is put into above-mentioned solution to soak 10 minutes; Carry out after taking-up extruding to get rid of unnecessary moisture, then blow out unnecessary moisture further with blower, and at 50 DEG C dry 20 hours.Described immersion, dried brick shape cloth are put into tunnel furnace, with the heating rate of 50 DEG C/min to 450 DEG C, is then warmed up to 1400 DEG C with the heating rate of 0.7 DEG C/min and is incubated 0.5 hour sintering; Zirconium white (3mol% yttrium oxide) fiber brick can be prepared after cooling.
Embodiment 5
Zircosol ZN, Yttrium trinitrate, urea, be dissolved in distilled water be mixed with solution, control Zr with polyoxyethylene glycol (auxiliary) 4+, Y 3+0.7 mol/L, 0.042 mol/L and 2.0mol/L respectively with the concentration of urea.Wherein, the addition of polyoxyethylene glycol is 3.5 % of urea quality.Brick shape is sewn into containing cotton cloth (cotton content 83wt%, terylene 9 wt%, spandex 8 wt%) by waste and old; Brick shape cloth is put into above-mentioned solution to soak 10 minutes; Carry out after taking-up extruding to get rid of unnecessary moisture, then blow out unnecessary moisture further with blower, and at 50 DEG C dry 20 hours.Described immersion, dried brick shape cloth are put into tunnel furnace, with the heating rate of 40 DEG C/min to 600 DEG C, is then warmed up to 1500 DEG C with the heating rate of 1 DEG C/min and is incubated 0.5 hour sintering; Zirconium white (3mol% yttrium oxide) fiber brick can be prepared after cooling.The sorbent material, film support etc. of chemical filler, flame-proof thermal insulation material (not higher than 1500 DEG C), support of the catalyst, toxic substance is can be used for the Zirconium oxide fibre brick that scrap fabric does Template preparation.

Claims (8)

1. prepare a simple method for zirconium white (3 mol% yttrium oxide) fiber brick, it is characterized in that adopting following steps: (1) is dissolved into zirconates, Yttrium trinitrate, urea, auxiliary in distilled water and is mixed with solution; (2) brick shape is sewn into containing cotton cloth; (3) described brick shape cloth is put into above-mentioned solution to soak 10 minutes; Carry out after taking-up extruding to get rid of unnecessary moisture, then blow out unnecessary moisture further with blower, and at 50 DEG C dry 20 hours; (4) described immersion, dried brick shape cloth are put into tunnel furnace, rapid heating is warmed up to 400-800 DEG C, then slowly heats to 1200-1650 DEG C and is incubated 0.5-1 hour sintering.
2. the one as described in right 1 prepares the simple method of zirconium white (3 mol% yttrium oxide) fiber brick, it is characterized in that: the zirconates described in step (1) is the one in zirconium nitrate, Zircosol ZN, zirconium oxychloride.
3. the one as described in right 1 prepares the simple method of zirconium white (3 mol% yttrium oxide) fiber brick, it is characterized in that: Zr in the solution described in step (1) 4+concentration be 0.3-0.8 mol/L, Y 3+concentration be Zr 4+concentration 6%, the concentration of urea is 0.5-2.0 mol/L.
4. the one as described in right 1 prepares the simple method of zirconium white (3 mol% yttrium oxide) fiber brick, it is characterized in that: the auxiliary in step (1) refers to the one in polyvinyl alcohol, polyoxyethylene glycol, polypropylene glycol; The add-on of auxiliary is 1 ~ 5 % of urea quality.
5. the one as described in right 1 prepares the simple method of zirconium white (3 mol% yttrium oxide) fiber brick, it is characterized in that: the cotton cloth that contains in step (2) refers to that the mass percentage of cotton fibre in cloth is 80-90%, the mass percentage of polyster fibre is 5-15%, and the mass percentage of spandex fibre is 5-10 %.
6. the one as described in right 1 prepares the simple method of zirconium white (3 mol% yttrium oxide) fiber brick, it is characterized in that: in step (2) can be new for cotton cloth containing cotton cloth, also can be waste and old containing cotton cloth, can also be that regeneration is containing cotton cloth.
7. the one as described in right 1 prepares the simple method of zirconium white (3 mol% yttrium oxide) fiber brick, it is characterized in that: the rapid heating in step (4) heats up and refers to that heat-up rate is 20-50 DEG C/min.
8. the one as described in right 1 prepares the simple method of zirconium white (3 mol% yttrium oxide) fiber brick, it is characterized in that: the slow heat temperature raising in step (4) refers to that heat-up rate is 0.1 ~ 1 DEG C/min.
CN201410557194.5A 2014-10-21 2014-10-21 A kind of method of the Zirconium oxide fibre brick prepared containing 3mol% yittrium oxide Expired - Fee Related CN104311006B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201410557194.5A CN104311006B (en) 2014-10-21 2014-10-21 A kind of method of the Zirconium oxide fibre brick prepared containing 3mol% yittrium oxide

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201410557194.5A CN104311006B (en) 2014-10-21 2014-10-21 A kind of method of the Zirconium oxide fibre brick prepared containing 3mol% yittrium oxide

Publications (2)

Publication Number Publication Date
CN104311006A true CN104311006A (en) 2015-01-28
CN104311006B CN104311006B (en) 2016-09-28

Family

ID=52366356

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201410557194.5A Expired - Fee Related CN104311006B (en) 2014-10-21 2014-10-21 A kind of method of the Zirconium oxide fibre brick prepared containing 3mol% yittrium oxide

Country Status (1)

Country Link
CN (1) CN104311006B (en)

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104671812A (en) * 2015-02-27 2015-06-03 山东磊宝锆业科技股份有限公司 Method for producing stable zirconia powder fiber felt
CN115522184B (en) * 2022-10-09 2024-03-19 华能国际电力股份有限公司 YSZ coating, ferronickel-based superalloy and preparation method thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101555026A (en) * 2009-05-07 2009-10-14 济南大学 Method for preparing nano-magnesia with cotton cloth form

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101555026A (en) * 2009-05-07 2009-10-14 济南大学 Method for preparing nano-magnesia with cotton cloth form

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
RUI-QIN SUN ET AL: "Synthesizing nanocrystal-assembled mesoporous magnesium oxide using cotton fibres as exotemplate", 《MICROPOROUS AND MESOPOROUS MATERIALS》, vol. 111, 15 August 2007 (2007-08-15) *

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104671812A (en) * 2015-02-27 2015-06-03 山东磊宝锆业科技股份有限公司 Method for producing stable zirconia powder fiber felt
CN115522184B (en) * 2022-10-09 2024-03-19 华能国际电力股份有限公司 YSZ coating, ferronickel-based superalloy and preparation method thereof

Also Published As

Publication number Publication date
CN104311006B (en) 2016-09-28

Similar Documents

Publication Publication Date Title
CN100497248C (en) Soluble pyroceram fibre, preparation method and application thereof
CN104005115B (en) A kind of preparation method of ceramic alumina fiber
CN106929927B (en) Preparation method of polyacetylacetonatozirconium precursor sol spinning solution and submicron zirconia crystal fiber
CN103191718A (en) Preparation method of low-cost honeycomb denitration catalyst
CN105481355B (en) A kind of aluminum oxide closed cell foamed ceramics of Zirconium oxide fibre enhancing and preparation method thereof
CN104311006A (en) Simple method for preparing zirconia fiber bricks
CN102465357B (en) Preparation method of polycrystal zirconia fiber and zirconia/alumina composite fiber
CN103755220A (en) Method for preparing zirconia ceramic fiber board
CN106220213A (en) A kind of preparation method of carbon/ceramic composite material
CN104341151A (en) Simple method for preparing zirconium oxide fiber fabric by using cotton-containing fabric as template
CN105622095A (en) High-temperature-resistant zirconia fiber ceramic plate and preparation method thereof
CN106835357A (en) A kind of method that cotton fiber prepares many hollow zirconium fibers
CN104326735A (en) Simple method for preparing magnesium oxide fiber cloth by taking cotton-containing fabric as template
CN104326738B (en) A kind of simple method to be Template preparation alumina fibre cloth containing cotton cloth
CN104326736A (en) Simple method for preparing magnesium oxide fiber brick
CN104326737B (en) A kind of simple method preparing sapphire whisker brick
CN106187224A (en) A kind of heat-barrier material compositions based on hollow zirconium and preparation method
CN104311092A (en) Simple method for preparing magnesium-aluminum spinel fiber brick
CN104326741B (en) A kind of to contain the simple method of cotton cloth as Template preparation magnesium aluminum spinel fibre cloth
CN104387098B (en) Simple preparation method of ferrous aluminum spinel fiber brick
CN101634056B (en) Method for preparing alumina-based continuous fiber
CN103757749A (en) Preparation method for zirconia crystal fiber
CN104264448B (en) A kind of to prepare the method for ferrous aluminum spinel fiber cloth containing cotton cloth as template
CN113023775A (en) Preparation method of ligand-modified zirconia sol and zirconia polycrystalline fiber
CN106187114A (en) A kind of preparation method of the alumina fibre of high heat-resistant high-strength

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20160928

Termination date: 20171021