CN106637510A - Preparation method of zirconium oxide fibers - Google Patents
Preparation method of zirconium oxide fibers Download PDFInfo
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- CN106637510A CN106637510A CN201710016727.2A CN201710016727A CN106637510A CN 106637510 A CN106637510 A CN 106637510A CN 201710016727 A CN201710016727 A CN 201710016727A CN 106637510 A CN106637510 A CN 106637510A
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- zirconium
- zirconium oxide
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/04—Dry spinning methods
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/10—Other agents for modifying properties
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- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
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- General Chemical & Material Sciences (AREA)
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- Inorganic Fibers (AREA)
Abstract
The invention discloses a preparation method of zirconium oxide fibers. The preparation method comprises the following steps of mixing zirconium carbonate, water, acrylic acid, an zirconium oxide crystal phase stabilizing agent and an organic additive to prepare an acrylic polyzirconium sol spinning liquid; performing high-speed centrifugal wire throwing on the acrylic polyzirconium sol spinning liquid, so as to obtain zirconium-containing gel fibers; further sintering at high temperature, so as to obtain the zirconium oxide ceramic fibers. The preparation method of zirconium oxide fibers have the characteristics that the obtaining of raw materials is easy, the preparation method is simple, the environment-friendly effect is good, the preparation method is suitable for scaled production, and the like; the disadvantage of acetic zirconium sol sensitive to humidity is overcame by the prepared acrylic polyzirconium sol spinning liquid; the permeation and absorption of appearance of gel fibers to water can be inhibited; the fibers forming property and production controllability are better; the diameter of the prepared zirconium oxide fibers is 3 to 6mu m, the appearance is smooth, and the diameter is uniform.
Description
Technical field
The present invention relates to a kind of preparation method of Zirconium oxide fibre, belongs to field of inorganic nonmetallic material.
Background technology
Zirconia ceramics fibrous material have that high temperature resistant, thermal conductivity factor be little, acid-alkali-corrosive-resisting strong and normal temperature under for insulation
There is the advantageous property such as electric conductivity under body, high temperature, in national defence hard-core technology and civilian high-end heat-insulated wait field to have huge answering
Use demand.However, the technology of preparing of zirconia ceramics fibrous material is mainly rested in minority developed country hand, domestic zirconium oxide
The correlative study of ceramic fibre material is started late, and technology falls behind relatively.Development technology is simple, be suitable to the preparation of industrialized production
Method, produces high-temperature stability high significant with the strong zirconia ceramics fibrous material of mechanical performance.
At present, the preparation method of zirconia ceramics fiber mainly has infusion process, co-blended spinning method and colloidal sol spin processes etc..Leaching
Stain method soaks viscose fiber using zirconyl chloride solution, after removing the unnecessary zirconium salt solution between fiber surface and fiber, passes through
Fiber after calcination dipping obtains zirconia ceramics fiber.This method is used till today, simple with method, can be mass produced
The features such as.But, content of organics is high in this method precursor fiber, there is large quantity of moisture and hydrochloric acid and organic matter row during calcination
Remove, cause fiber loose porous, intensity is very low.Co-blended spinning method is the polymer adhesive using Linear Polymer chain and dispersion
Agent mixes with zirconium oxide micro mist, and adds resin as bonding agent, and slurry is obtained, and is extruded into silk by micropore high pressure and is used as forerunner
Body, by this presoma fiber is directly fired into.In the method for ensure presoma into silk, still used substantial amounts of adhesive and
Resinoid bond, and zirconium oxide grain size of micropowder is larger, presoma is thicker, and the fibre structure after firing is undesirable, it is impossible to meets and protects
The heat-insulated needs of temperature.Meanwhile, this method needs Jing complicated technologies to prepare the zirconium oxide and zirconates particle of sub-meter grade, relatively costly, no
It is suitable to large-scale production.Colloidal sol spin processes be with organic or inorganic zirconates as raw material, it is anti-in a solvent with complexing agent by zirconates
Should, prepare and be suitable to the macromolecular colloidal sol of spinning, then prepare zirconia ceramics fiber through spinning and high-temperature process.This method institute
The zirconium content for obtaining colloidal sol fiber is higher, reduces the large amount of organic in heat treatment process and decomposes the defect for causing, and can prepare
The zirconia ceramics fibrous material of good mechanical performance.
The preparation of the poly- zirconium colloidal sol of spinnability is the key that colloidal sol spin processes prepare zirconia ceramics material.Conventional colloidal sol network
Mixture mainly has beta-diketon class, organic carboxyl acid class alcohols and alcamines complexing agent.For example：Patent ZL200410024264.7 is utilized
Zirconium oxychloride, acetylacetone,2,4-pentanedione, ethanol, triethylamine etc. prepare acetylacetone,2,4-pentanedione zirconium, then acetylacetone,2,4-pentanedione zirconium and yttrium nitrate are dissolved in
Zirconium colloidal sol spinning solution is prepared in methyl alcohol.Substantial amounts of volatile organic solvent and triethylamine etc. are directed in this method poisonous inflammable
Quick-fried material, causes control of product quality unstable and industrialization is difficult.Patent CN102181962B adopts zirconium oxycarbonate, ice
Acetic acid and water prepare poly- zirconium colloidal sol spinning solution, although process route with respect to environmental protection, but by colloidal sol spinning obtain it is solidifying
Glue fiber is sensitive to ambient temperature and humidity so that the fibre-forming performance of colloidal sol spinning solution is poor, obtains easy moisture absorption bonding after gelatinous fibre,
Cause the Zirconium oxide fibre pattern and intensity of preparation not good.Therefore, development technology is simple, and environmental protection is cheap, can be used for
The poly- zirconium spinning colloidal sols for preparing high-performance zirconia fibrous material have great importance.
The content of the invention
To overcome serious prior art processes complexity, environmental pollution, spinning colloidal sols and gelatinous fibre property stable in the air
The defect such as poor, the invention provides a kind of preparation method of Zirconium oxide fibre.
The preparation method of Zirconium oxide fibre of the present invention, is as core technology including as follows with the poly- zirconium spinning colloidal sols of acrylic acid
Step：
1st, the preparation of the poly- zirconium colloidal sol spinning solution of acrylic acid
Acrylic acid is added to the water and is uniformly mixed, zirconium carbonate is added after being warming up to 45-75 DEG C, continue to stir to thing
Expect transparent clarification, obtain final product the poly- zirconium solution of acrylic acid；Zirconium oxide crystalline phase stabilizer is added in the poly- zirconium solution of gained acrylic acid and is had
Machine additive, continues the stirring at 45-75 DEG C and is concentrated by evaporation, progressively moisture content unnecessary in removing system, when zirconium oxide in system
When mass concentration reaches 45-60%, that is, the poly- zirconium colloidal sol spinning solution of acrylic acid is obtained；
The mol ratio fed intake according to zirconium oxide, water and acrylic acid in reaction system is 1:5-15:The ratio of 0.5-3, weighs
The zirconium carbonate of corresponding weight, water and acrylic acid.
The zirconium oxide crystalline phase stabilizer is yttrium nitrate, according to zirconium oxide in reaction system and Y2O3The mol ratio for feeding intake is
90-95:The ratio of 10-5, weighs the zirconium carbonate and yttrium nitrate of corresponding weight.
The organic additive is one or two in acetic acid, citric acid, according to zirconium oxide in reaction system and acetic acid
The mol ratio for feeding intake is 1:The mol ratio that 0.5-2.5, zirconium oxide and citric acid feed intake is 1:The ratio of 0.1-0.3, weighs corresponding
The zirconium carbonate of weight, acetic acid and citric acid.
2nd, the shaping of gelatinous fibre
The poly- zirconium colloidal sol spinning solution of acrylic acid that step 1 is obtained is placed in high speed centrifugation tumbling machine, in high speed centrifugation effect
Under power by getting rid of wire tray aperture by obtain gelatinous fibre containing zirconium into fine；The rotating speed of high speed centrifugation tumbling machine is 10000- per second
13000 turns.
3rd, it is heat-treated
The gelatinous fibre containing zirconium that step 2 is obtained is warming up to 550 DEG C and is incubated 1h, then raises temperature to 1000-1600 DEG C simultaneously
Insulation 1h, obtains the Zirconium oxide fibre of a diameter of 3-6 microns by being cooled to after room temperature.
The heating rate for being warming up to 550 DEG C is 0.5-1.5 DEG C/min；The heating rate for being warming up to 1000-1600 DEG C is 1-5
℃/min。
Beneficial effects of the present invention are embodied in：
1st, the poly- zirconium colloidal sol of acrylic acid of the invention is prepared in a simple way using conventional reaction vessel, is not related to electrolysis
Deng complicated technology, and solvent is made using water, it is to avoid the use of a large amount of organic solvents, cost is relatively low, is suitable to large-scale production.
2nd, the poly- zirconium colloidal sol spinning solution of acrylic acid of the invention overcomes shortcoming of the acetic acid zirconium colloidal sol to humidity sensitive, can press down
The apparent infiltration and absorption to moisture of gelatinous fibre processed, so that the poly- zirconium colloidal sol of acrylic acid possesses preferable fibre forming property and life
Produce controllability.
3rd, prepared by the poly- zirconium colloidal sol spinning solution Jing high speed centrifugations dry spinning of acrylic acid of the invention and subsequent heat treatment
Zirconium oxide fibre is a diameter of 3-6 μm, and apparent smooth, uniform diameter, high-temperature behavior is excellent.
Description of the drawings
Fig. 1 is the digital camera photo of the poly- zirconium colloidal sol spinning solution of acrylic acid of the present invention.
Fig. 2 is the digital camera photo of Zirconium oxide fibre of the present invention.
Fig. 3 is the stereoscan photograph of Zirconium oxide fibre of the present invention.
Specific embodiment
Embodiment 1：
The preparation method of Zirconium oxide fibre is as follows in the present embodiment：
1st, the preparation of the poly- zirconium colloidal sol spinning solution of acrylic acid
11.7g acrylic acid is added in 29.2g water and is uniformly mixed, 100g carbonic acid is gradually added after being warming up to 45 DEG C
Zirconium, continues to stir to the transparent clarification of material, obtains final product the poly- zirconium solution of acrylic acid and (zirconium oxide in reaction system, water and acrylic acid rubs
You are than being 1:5:0.5)；Zirconium oxide crystalline phase stabilizer yttrium nitrate 27.6g is added in the poly- zirconium solution of gained acrylic acid and organic is added
Plus agent acetic acid 48.8g, continue the stirring at 45 DEG C and be concentrated by evaporation, progressively moisture content unnecessary in removing system, when oxidation in system
When zirconium mass concentration reaches 45%, that is, the poly- zirconium colloidal sol spinning solution of acrylic acid is obtained；
2nd, the shaping of gelatinous fibre
The poly- zirconium colloidal sol spinning solution of acrylic acid that step 1 is obtained is placed in high speed centrifugation tumbling machine, with 10000 turns per second
Speed gets rid of silk into fibre, obtains gelatinous fibre containing zirconium；
3rd, it is heat-treated
The gelatinous fibre containing zirconium that step 2 is obtained is warming up to 550 DEG C and is incubated 1h with the heating rate of 0.5 DEG C/min, with
It is warming up to 1000 DEG C with the heating rate of 1 DEG C/min afterwards and is incubated 1h, a diameter of 3-6 microns is obtained by being cooled to after room temperature
Zirconium oxide fibre.Using SEM sem tests its average diameters be 3.6 μm, fibre diameter it is uniform and apparent smooth, compared with
The Zirconium oxide fibre of 4-15 μm of filament diameter prepared by ZL200410024264.7 is thinner, performance more preferably, according to ISO11566-
1996 test its average monofilament tensile strength, its average monofilament tensile strength is up to 1100MPa.
Embodiment 2：
The preparation method of Zirconium oxide fibre is as follows in the present embodiment：
1st, the preparation of the poly- zirconium colloidal sol spinning solution of acrylic acid
23.4g acrylic acid is added in 46.7g water and is uniformly mixed, 100g carbonic acid is gradually added after being warming up to 55 DEG C
Zirconium, continues to stir to the transparent clarification of material, obtains final product the poly- zirconium solution of acrylic acid and (zirconium oxide in reaction system, water and acrylic acid rubs
You are than being 1:8:1)；Zirconium oxide crystalline phase stabilizer yttrium nitrate 21.6g and organic addition are added in the poly- zirconium solution of gained acrylic acid
Agent acetic acid 39g, citric acid 6.2g, continue the stirring at 55 DEG C and are concentrated by evaporation, and progressively moisture content unnecessary in removing system, works as system
When middle zirconium oxide mass concentration reaches 50%, that is, the poly- zirconium colloidal sol spinning solution of acrylic acid is obtained；
2nd, the shaping of gelatinous fibre
The poly- zirconium colloidal sol spinning solution of acrylic acid that step 1 is obtained is placed in high speed centrifugation tumbling machine, with 11000 turns per second
Speed gets rid of silk into fibre, obtains gelatinous fibre containing zirconium；
3rd, it is heat-treated
The gelatinous fibre containing zirconium that step 2 is obtained is warming up to 550 DEG C and is incubated 1h with the heating rate of 1.0 DEG C/min, with
It is warming up to 1100 DEG C with the heating rate of 2 DEG C/min afterwards and is incubated 1h, a diameter of 3-6 microns is obtained by being cooled to after room temperature
Zirconium oxide fibre.Using SEM sem tests its average diameters be 4.0 μm, fibre diameter it is uniform and apparent smooth, compared with
The Zirconium oxide fibre of 4-15 μm of filament diameter prepared by ZL200410024264.7 is thinner, performance more preferably, according to ISO11566-
1996 test its average monofilament tensile strength, its average monofilament tensile strength is up to 1200MPa.
Embodiment 3：
The preparation method of Zirconium oxide fibre is as follows in the present embodiment：
1st, the preparation of the poly- zirconium colloidal sol spinning solution of acrylic acid
46.8g acrylic acid is added in 70g water and is uniformly mixed, 100g carbonic acid is gradually added after being warming up to 65 DEG C
Zirconium, continues to stir to the transparent clarification of material, obtains final product the poly- zirconium solution of acrylic acid and (zirconium oxide in reaction system, water and acrylic acid rubs
You are than being 1:12:2)；Zirconium oxide crystalline phase stabilizer yttrium nitrate 21.6g and organic addition are added in the poly- zirconium solution of gained acrylic acid
Agent acetic acid 19.5g, continues the stirring at 65 DEG C and is concentrated by evaporation, progressively moisture content unnecessary in removing system, when zirconium oxide in system
When mass concentration reaches 55%, that is, the poly- zirconium colloidal sol spinning solution of acrylic acid is obtained；
2nd, the shaping of gelatinous fibre
The poly- zirconium colloidal sol spinning solution of acrylic acid that step 1 is obtained is placed in high speed centrifugation tumbling machine, with 12000 turns per second
Speed gets rid of silk into fibre, obtains gelatinous fibre containing zirconium；
3rd, it is heat-treated
The gelatinous fibre containing zirconium that step 2 is obtained is warming up to 550 DEG C and is incubated 1h with the heating rate of 1.2 DEG C/min, with
It is warming up to 1200 DEG C with the heating rate of 3.5 DEG C/min afterwards and is incubated 1h, a diameter of 3-6 microns is obtained by being cooled to after room temperature
Zirconium oxide fibre.Using SEM sem tests its average diameters be 4.5 μm, fibre diameter it is uniform and apparent smooth, compared with
The Zirconium oxide fibre of 4-15 μm of filament diameter prepared by ZL200410024264.7 is thinner, performance more preferably, according to ISO11566-
1996 test its average monofilament tensile strength, its average monofilament tensile strength is up to 1100MPa.
Embodiment 4：
The preparation method of Zirconium oxide fibre is as follows in the present embodiment：
1st, the preparation of the poly- zirconium colloidal sol spinning solution of acrylic acid
70.2g acrylic acid is added in 87.5g water and is uniformly mixed, 100g carbonic acid is gradually added after being warming up to 75 DEG C
Zirconium, continues to stir to the transparent clarification of material, obtains final product the poly- zirconium solution of acrylic acid and (zirconium oxide in reaction system, water and acrylic acid rubs
You are than being 1:15:3)；Zirconium oxide crystalline phase stabilizer yttrium nitrate 13.1g and organic addition are added in the poly- zirconium solution of gained acrylic acid
Agent acetic acid 9.75g, citric acid 18.6g, continue the stirring at 75 DEG C and are concentrated by evaporation, progressively moisture content unnecessary in removing system, when
When zirconium oxide mass concentration reaches 60% in system, that is, the poly- zirconium colloidal sol spinning solution of acrylic acid is obtained；
2nd, the shaping of gelatinous fibre
The poly- zirconium colloidal sol spinning solution of acrylic acid that step 1 is obtained is placed in high speed centrifugation tumbling machine, with 13000 turns per second
Speed gets rid of silk into fibre, obtains gelatinous fibre containing zirconium；
3rd, it is heat-treated
The gelatinous fibre containing zirconium that step 2 is obtained is warming up to 550 DEG C and is incubated 1h with the heating rate of 1.5 DEG C/min, with
It is warming up to 1600 DEG C with the heating rate of 5 DEG C/min afterwards and is incubated 1h, a diameter of 3-6 microns is obtained by being cooled to after room temperature
Zirconium oxide fibre.Using SEM sem tests its average diameters be 5.5 μm, fibre diameter it is uniform and apparent smooth, compared with
The Zirconium oxide fibre of 4-15 μm of filament diameter prepared by ZL200410024264.7 is thinner, performance more preferably, according to ISO11566-
1996 test its average monofilament tensile strength, its average monofilament tensile strength is up to 350MPa.
Claims (6)
1. a kind of preparation method of Zirconium oxide fibre, it is characterised in that comprise the steps：
(1) preparation of the poly- zirconium colloidal sol spinning solution of acrylic acid
Acrylic acid is added to the water and is uniformly mixed, zirconium carbonate is added after being warming up to 45-75 DEG C, continue to stir saturating to material
Bright clarification, obtains final product the poly- zirconium solution of acrylic acid；Zirconium oxide crystalline phase stabilizer is added in the poly- zirconium solution of gained acrylic acid and organic is added
Plus agent, continue the stirring at 45-75 DEG C and be concentrated by evaporation, progressively moisture content unnecessary in removing system, when zirconium oxide quality in system
When concentration reaches 45-60%, that is, the poly- zirconium colloidal sol spinning solution of acrylic acid is obtained；
(2) shaping of gelatinous fibre
The poly- zirconium colloidal sol spinning solution of acrylic acid that step (1) is obtained is placed in high speed centrifugation tumbling machine, in high speed centrifugation active force
Under by getting rid of wire tray aperture by obtain gelatinous fibre containing zirconium into fine；
(3) it is heat-treated
The gelatinous fibre containing zirconium that step (2) is obtained is warming up to 550 DEG C and is incubated 1h, 1000-1600 DEG C is then raised temperature to and is protected
Warm 1h, obtains the Zirconium oxide fibre of a diameter of 3-6 microns by being cooled to after room temperature.
2. preparation method according to claim 1, it is characterised in that：
In step (1), the mol ratio fed intake according to zirconium oxide, water and acrylic acid in reaction system is 1:5-15:The ratio of 0.5-3
Example, weighs zirconium carbonate, water and the acrylic acid of corresponding weight.
3. preparation method according to claim 1, it is characterised in that：
In step (1), the zirconium oxide crystalline phase stabilizer is yttrium nitrate, according to zirconium oxide in reaction system and Y2O3What is fed intake rubs
You are than being 90-95:The ratio of 10-5, weighs the zirconium carbonate and yttrium nitrate of corresponding weight.
4. preparation method according to claim 1, it is characterised in that：
In step (1), the organic additive is one or two in acetic acid, citric acid, according to zirconium oxide in reaction system
It is 1 with the mol ratio that acetic acid feeds intake:The mol ratio that 0.5-2.5, zirconium oxide and citric acid feed intake is 1:The ratio of 0.1-0.3, claims
Take zirconium carbonate, acetic acid and the citric acid of corresponding weight.
5. preparation method according to claim 1, it is characterised in that：
In step (2), the rotating speed of high speed centrifugation tumbling machine turns for 10000-13000 per second.
6. preparation method according to claim 1, it is characterised in that：
In step (3), the heating rate for being warming up to 550 DEG C is 0.5-1.5 DEG C/min；It is warming up to 1000-1600 DEG C of intensification speed
Rate is 1-5 DEG C/min.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108467549A (en) * | 2018-03-29 | 2018-08-31 | 平顶山学院 | A kind of Electric insulation material and preparation method thereof that high temperature resistant is anti-aging |
| CN111792933A (en) * | 2020-07-30 | 2020-10-20 | 安徽同和晶体新材料股份有限公司 | Method for preparing environment-friendly zirconia crystal fiber by alkaline process |
| CN113023775A (en) * | 2021-04-08 | 2021-06-25 | 齐鲁工业大学 | Preparation method of ligand-modified zirconia sol and zirconia polycrystalline fiber |
| CN113620705A (en) * | 2021-08-17 | 2021-11-09 | 山东鲁阳浩特高技术纤维有限公司 | Zirconia fiber and preparation method thereof, zirconia fiber filter material and preparation method thereof |
| CN113716970A (en) * | 2021-09-23 | 2021-11-30 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of zirconia fiber heat insulation product |
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| CN113716970A (en) * | 2021-09-23 | 2021-11-30 | 中钢集团洛阳耐火材料研究院有限公司 | Preparation method of zirconia fiber heat insulation product |
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| CN106637510B (en) | 2018-12-11 |
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