CN109650842A - A kind of preparation method of inorganic combination ceramic fibre material - Google Patents
A kind of preparation method of inorganic combination ceramic fibre material Download PDFInfo
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- CN109650842A CN109650842A CN201811594994.9A CN201811594994A CN109650842A CN 109650842 A CN109650842 A CN 109650842A CN 201811594994 A CN201811594994 A CN 201811594994A CN 109650842 A CN109650842 A CN 109650842A
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B30/00—Compositions for artificial stone, not containing binders
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/24—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing alkyl, ammonium or metal silicates; containing silica sols
- C04B28/26—Silicates of the alkali metals
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/20—Mortars, concrete or artificial stone characterised by specific physical values for the density
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Nonwoven Fabrics (AREA)
Abstract
The invention belongs to Material Field more particularly to a kind of preparation methods of inorganic combination ceramic fibre material, method includes the following steps: a) being beaten ceramic fibre in water, dehydration forming, obtains wet base later；B) inorganic bonding agent is impregnated into wet base, impregnates pH adjusting agent into wet base again later, stood, form wet gel base；The inorganic bonding agent is alkaline silica sol and/or waterglass, and the pH adjusting agent is acid solution；Or, the inorganic bonding agent is acidic silicasol, the pH adjusting agent is lye；C) wet gel base is dried, obtains inorganic combination ceramic fibre material.In the present invention, by successively impregnating inorganic bonding agent and pH adjusting agent into wet base, the inorganic bonding agent being impregnated into ceramic fiber body can be promoted to be condensed into Silica hydrogel in advance, to make it that can be securely bonded together with ceramic fibre, it avoids inorganic bonding agent in subsequent drying process from migrating with moisture evaporation, guarantees that intensity is consistent inside and outside material.
Description
Technical field
The invention belongs to Material Field more particularly to a kind of preparation methods of inorganic combination ceramic fibre material.
Background technique
Ceramic fibre material has excellent heat-insulating property and mechanical property, is the heat-insulated preferred material of kiln backing.Tradition
Ceramic fibre material usually passes through the organic bonds such as addition starch, cellulose and improves intensity, and organic bond is in hot conditions
Under can be carbonized, burn, and generate with peculiar smell, cause damages to environment and human health.As every profession and trade energy conservation drops in country
The increasing of consumption, safety and environmental protection etc. working dynamics, the ceramic fibre that market prepares use inorganic material as bonding agent
The demand of material just gradually increases, and this fibrous material is free of any organic matter, smokeless, tasteless under high temperature.
Inorganic combination ceramic fibre material generally goes through the processes such as ingredient, molding, drying and is made, due to that can make material when drying
Moisture inside material can evaporate outward, to inevitably cause the inorganic bonding agent of material internal along with moisture to moving outside
It moves, and then the inorganic combination ceramic fibre material obtained after drying is made the hard intermediate soft phenomenon in surface layer easily occur.Therefore, how to mention
The uniformity of hardness of high inorganic combination ceramic fibre material is field technical problem urgently to be resolved at present.
Summary of the invention
In view of this, being used the purpose of the present invention is to provide a kind of preparation method of inorganic combination ceramic fibre material
Hardness uniformity inside and outside the ceramic fibre material of the method for the present invention preparation.
The present invention provides a kind of preparation methods of inorganic combination ceramic fibre material, comprising the following steps:
A) ceramic fibre is beaten, later dehydration forming in water, obtains wet base；
B) inorganic bonding agent is impregnated into the wet base, impregnates pH adjusting agent into the wet base again later, stood, shape
At wet gel base；
The inorganic bonding agent is alkaline silica sol and/or waterglass, and the pH adjusting agent is acid solution；
Or, the inorganic bonding agent is acidic silicasol, the pH adjusting agent is lye；
C) the wet gel base is dried, obtains inorganic combination ceramic fibre material.
Preferably, in step a), the diameter of the ceramic fibre is 2~5 μm.
Preferably, in step a), the revolving speed of the mashing is 500~1000r/min；The time of the mashing be 15~
20min。
Preferably, in step a), the mode of the dehydration forming is vacuum suction filter；
The vacuum degree of the vacuum suction filter is 400~550mmHg；The time of the vacuum suction filter is 5~10s.
Preferably, in step b), the concentration of the inorganic bonding agent is 20~40wt%.
Preferably, the mass ratio of the inorganic bonding agent and the ceramic fibre is (20~40): (60~80).
Preferably, in step b), H in the acid solution+Concentration be 0.1~1mol/L；OH in the lye-Concentration be
0.1~1mol/L；
The inorganic bonding agent and the mass ratio of pH adjusting agent are 100:(1~3).
Preferably, in step b), the acid solution includes acetum, oxalic acid solution, phosphoric acid solution, nitric acid solution, hydrochloric acid
One of solution and sulfuric acid solution are a variety of；
The lye includes ammonium hydroxide and/or sodium hydroxide solution.
Preferably, in step b), the temperature of the standing is 15~35 DEG C；The time of the standing is 10~20min.
Preferably, in step c), the temperature of the drying is 80~120 DEG C；The time of the drying be 10~for 24 hours.
Compared with prior art, the present invention provides a kind of preparation methods of inorganic combination ceramic fibre material.The present invention
Ceramic fibre the following steps are included: a) be beaten by the preparation method of offer in water, and dehydration forming, obtains wet base later；B) will
Inorganic bonding agent is impregnated into the wet base, impregnates pH adjusting agent into the wet base again later, is stood, and wet gel base is formed；
The inorganic bonding agent is alkaline silica sol and/or waterglass, and the pH adjusting agent is acid solution；Or, the inorganic bonding agent is
Acidic silicasol, the pH adjusting agent are lye；C) the wet gel base is dried, obtains inorganic combination ceramic fibre material
Material.In the present invention, by successively impregnating inorganic bonding agent and pH adjusting agent into wet base, can promote to be impregnated into ceramic fibre base
Inorganic bonding agent in body is condensed into Silica hydrogel in advance, to make it that can be securely bonded together with ceramic fibre, after avoiding
Inorganic bonding agent is migrated with moisture evaporation in continuous drying process, guarantees that intensity is consistent inside and outside material.The results showed that using this
The surface hardness of the inorganic combination ceramic fibre material of inventive method preparation is consistent with section hardness.
Specific embodiment
The technical scheme in the embodiments of the invention will be clearly and completely described below, it is clear that described implementation
Example is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field is common
Technical staff's every other embodiment obtained without making creative work belongs to the model that the present invention protects
It encloses.
The present invention provides a kind of preparation methods of inorganic combination ceramic fibre material, comprising the following steps:
A) ceramic fibre is beaten, later dehydration forming in water, obtains wet base；
B) inorganic bonding agent is impregnated into the wet base, impregnates pH adjusting agent into the wet base again later, stood, shape
At wet gel base；
The inorganic bonding agent is alkaline silica sol and/or waterglass, and the pH adjusting agent is acid solution；
Or, the inorganic bonding agent is acidic silicasol and/or acidic water glass, the pH adjusting agent is lye；
C) the wet gel base is dried, obtains inorganic combination ceramic fibre material.
In preparation method provided by the invention, ceramic fibre is beaten in water first.Wherein, the ceramic fibre packet
Include but be not limited to plain edition ceramic fibre, high-purity type ceramic fibre, high aluminium profiles ceramic fibre, the ceramic fibre of type containing zirconium and mullite
One of type ceramic fibre is a variety of；The diameter of the ceramic fibre is preferably 2~5 μm, concretely 2 μm, 2.5 μm, 3 μ
M, 3.5 μm, 4 μm, 4.5 μm or 5 μm；The mass ratio of the ceramic fibre and water is preferably (60~80): (3000~5000), tool
Body can be 60:3000,70:4500 or 80:5000；The revolving speed of the mashing is preferably 500~1000r/min, concretely
500r/min、550r/min、600r/min、650r/min、700r/min、750r/min、800r/min、850r/min、900r/
Min, 950r/min or 1000r/min；The time of the mashing is preferably 15~20min, concretely 15min, 15.5min,
16min, 16.5min, 17min, 17.5min, 18min, 18.5min, 19min, 19.5min or 20min；The mashing preferably exists
It is carried out in volt beater.After mashing, dehydration forming is carried out to fibre stuff is obtained.Wherein, the side of the dehydration forming
Formula is preferably vacuum suction filter；The vacuum degree of the vacuum suction filter is preferably 400~550mmHg, concretely 400mmHg,
410mmHg、420mmHg、430mmHg、440mmHg、450mmHg、460mmHg、470mmHg、480mmHg、490mmHg、
500mmHg, 510mmHg, 520mmHg, 530mmHg, 540mmHg or 550mmHg；The time of the vacuum suction filter is preferably 5~
10s, concretely 5s, 5.5s, 6s, 6.5s, 7s, 7.5s, 8s, 8.5s, 9s, 9.5s or 10s；What the vacuum suction filter used sets
Standby preferably Roots vaccum pump.After dehydration forming, wet base is obtained.
In the present invention, after obtaining wet base, inorganic bonding agent is impregnated into the wet base.Wherein, the inorganic combination
Agent is alkaline silica sol and/or waterglass, or is acidic silicasol；The concentration of solute is preferably 20 in the inorganic bonding agent
~40wt%, concretely 20wt%, 21wt%, 22wt%, 23wt%, 24wt%, 25wt%, 26wt%, 27wt%,
28wt%, 29wt%, 30wt%, 31wt%, 32wt%, 33wt%, 34wt%, 35wt%, 36wt%, 37wt%, 38wt%,
39wt% or 40wt%；The inorganic bonding agent with prepare ceramic fibre used in the wet base mass ratio preferably (20~
40): (60~80), concretely 20:80,30:70 or 40:60.In the present invention, the mode for impregnating the inorganic bonding agent is excellent
It is selected as: drenching inorganic bonding agent on wet base surface, inorganic bonding agent is to wet base internal penetration later, and is distributed evenly in wet base
Each position.
In the present invention, after inorganic bonding agent dipping, then into the wet base pH adjusting agent is impregnated.Wherein, if it
The inorganic bonding agent of preceding dipping is alkaline silica sol and/or waterglass, then the pH adjusting agent impregnated is acid solution；If impregnate before
Inorganic bonding agent is acidic silicasol, then the pH adjusting agent impregnated is lye.In the present invention, the acid solution includes but is not limited to
One of acetum, oxalic acid solution, phosphoric acid solution, nitric acid solution, hydrochloric acid solution and sulfuric acid solution are a variety of；The acid solution
Middle H+Concentration be preferably 0.1~1mol/L, concretely 0.1mol/L, 0.2mol/L, 0.3mol/L, 0.4mol/L,
0.5mol/L, 0.6mol/L, 0.7mol/L, 0.8mol/L, 0.9mol/L or 1mol/L；The lye includes but is not limited to ammonium hydroxide
And/or sodium hydroxide solution；OH in the lye-Concentration be preferably 0.1~1mol/L, concretely 0.1mol/L,
0.2mol/L, 0.3mol/L, 0.4mol/L, 0.5mol/L, 0.6mol/L, 0.7mol/L, 0.8mol/L, 0.9mol/L or
1mol/L.In the present invention, the mass ratio of the pH adjusting agent and the inorganic bonding agent is preferably (1~3): 100, specifically may be used
For 1:100,1.5:100,2:100,2.5:100 or 3:100.In the present invention, the mode for impregnating the pH adjusting agent is preferred are as follows:
PH adjusting agent is drenched on wet base surface, pH adjusting agent is to wet base internal penetration later, and is distributed evenly in each position of wet base.
In the present invention, after impregnated of pH adjusting agent, the inorganic bonding agent of dipping before promoting in ceramic fiber body
It is gradually condensed into Silica hydrogel, a period of time is stood, obtains wet gel base.Wherein, the temperature of the standing is preferably 15~35 DEG C,
Concretely 15 DEG C, 16 DEG C, 17 DEG C, 18 DEG C, 19 DEG C, 20 DEG C, 21 DEG C, 22 DEG C, 23 DEG C, 24 DEG C, 25 DEG C (room temperature), 26 DEG C, 27
DEG C, 28 DEG C, 29 DEG C, 30 DEG C, 31 DEG C, 32 DEG C, 33 DEG C, 34 DEG C or 35 DEG C；The time of the standing is preferably 10~20min, tool
Body can be 10min, 11min, 12min, 13min, 14min, 15min, 16min, 17min, 18min, 19min or 20min.
In the present invention, after obtaining wet gel base, the wet gel base is dried.Wherein, the mode of the drying
Preferably dry；The temperature of the drying is preferably 80~120 DEG C, concretely 80 DEG C, 85 DEG C, 90 DEG C, 95 DEG C, 100 DEG C,
105 DEG C, 110 DEG C, 115 DEG C or 120 DEG C；The time of the drying is preferably 10~for 24 hours, concretely 10h, 11h, 12h, 13h,
14h, 15h, 16h, 17h, 18h, 19h, 20h, 21h, 22h, 23h or for 24 hours.After drying, inorganic combination ceramic fibre is obtained
Material.
In the present invention, by successively impregnating inorganic bonding agent and pH adjusting agent into wet base, can promote to be impregnated into ceramics
Inorganic bonding agent in fiber body is condensed into Silica hydrogel in advance, thus be securely bonded together it can with ceramic fibre,
It avoids inorganic bonding agent in subsequent drying process from migrating with moisture evaporation, guarantees that intensity is consistent inside and outside material.The results showed that
Surface hardness using the inorganic combination ceramic fibre material of the method for the present invention preparation is consistent with section hardness.
For the sake of becoming apparent from, it is described in detail below by following embodiment.
In following embodiments of the invention, the fibre diameter of used ceramic fibre is 2~5 μm, is referred specifically to
See Table 1 for details for mark:
The index of the various ceramic fibres of table 1
Embodiment 1
The plain edition ceramic fibre of 60 parts by weight is beaten dispersion by volt beater in 3000 parts by weight water, is beaten
Revolving speed is 500r/min, beating time 20min；Vacuum suction filter dehydration forming is carried out by Roots vaccum pump, vacuum degree is
400mmHg, suction strainer time are 10s；The waterglass that it is 20wt% into 40 parts by weight concentration that wet base surface after molding, which is drenched, makes inorganic
Bonding agent is distributed evenly in each position of wet base, then drenches the oxalic acid solution for being 0.1mol/L into concentration, oxalic acid solution
Drench into amount with drench into waterglass weight ratio be 3:100；After demoulding and placing 10min, dried into drying room, drying temperature 80
DEG C, drying time for 24 hours, obtains the inorganic combined ceramic fiberboard with a thickness of 20mm.
Embodiment 2
The high aluminium profiles ceramic fibre of 70 parts by weight is beaten dispersion by volt beater in 4500 parts by weight water, is beaten
Revolving speed is 800r/min, beating time 18min；Vacuum suction filter dehydration forming is carried out by Roots vaccum pump, vacuum degree is
500mmHg, suction strainer time are 8s；The alkaline silica sol that it is 30wt% into 30 parts by weight concentration that wet base surface after molding, which is drenched, makes
Inorganic bonding agent is distributed evenly in each position of wet base, then drenches the acetum for being 0.5mol/L into concentration, and acetic acid is molten
Liquid drench into amount with drench into silica solution weight ratio be 2:100；It after demoulding and placing 15min, is dried into drying room, drying temperature
100 DEG C of degree, drying time 15h obtains the inorganic combined ceramic fiberboard with a thickness of 25mm.
Embodiment 3
The polymorphic ceramic fibre of 80 parts by weight is beaten dispersion by volt beater in 5000 parts by weight water, is beaten
Revolving speed is 1000r/min, beating time 10min；Vacuum suction filter dehydration forming is carried out by Roots vaccum pump, vacuum degree is
550mmHg, suction strainer time are 5s；The acidic silicasol that it is 40wt% into 20 parts by weight concentration that wet base surface after molding, which is drenched, makes
Inorganic bonding agent is distributed evenly in each position of wet base, then drenches the ammonium hydroxide for being 1mol/L into concentration, and the leaching of ammonium hydroxide enters amount
With drench into silica solution weight ratio be 1:100；It after demoulding and placing 20min, dries, 120 DEG C of drying temperature, dries into drying room
Dry time 10h, obtains the inorganic combined ceramic fiberboard with a thickness of 30mm.
Comparative example
2Kg silica solution, 0.01kg titanium dioxide and 2kg water are taken, be thoroughly mixed that slurry is made；Then by 500
Alumina silicate fibre after DEG C pre-burning immerses in mixed slurry, while being aided with the vacuum condition of 0.01MPa；Followed by mold to suction
Alumina silicate fibre after starching impregnation carries out Manual pressurizing molding and obtains wet mat；Again by fibre after molding together with mould
Drying and dehydrating is handled tool at 110 DEG C together；Mold is finally taken off, the inorganic combined ceramic fiberboard with a thickness of 30mm is obtained.
Performance test
The inorganic combined ceramic fiberboard number consecutively that the embodiment of the present invention 1~3 is prepared is A, B, C, and comparison is real
The sample number into spectrum for applying example preparation is D.Bulk density, the compressive resistance of test sample respectively, and the production during Statistics Implementation
Efficiency obtains data as shown in table 2:
2 inorganic combined ceramic fiberboard performance data table of table
Data are shown in table, inorganic combined ceramic fiberboard excellent in pressure strength of the present invention, and in hot environment
Basically no attenuation, inside and outside hardness is consistent for lower intensity.The inorfil heat-barrier material compressive resistance that comparative example is prepared is low, this master
If these powder can reunite on alumina silicate fibre surface because containing a large amount of powder in slurry, the infiltration of inorganic bonding agent is influenced
Enter and be uniformly distributed, to influence intensity；In addition the process is more complicated for comparative example, needs pre-burning alumina silicate fibre, needs simultaneously
Manual pressurizing sizing, causes production efficiency relatively low.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (10)
1. a kind of preparation method of inorganic combination ceramic fibre material, comprising the following steps:
A) ceramic fibre is beaten, later dehydration forming in water, obtains wet base；
B) inorganic bonding agent is impregnated into the wet base, impregnates pH adjusting agent into the wet base again later, stood, formed wet
Gel base；
The inorganic bonding agent is alkaline silica sol and/or waterglass, and the pH adjusting agent is acid solution；
Or, the inorganic bonding agent is acidic silicasol, the pH adjusting agent is lye；
C) the wet gel base is dried, obtains inorganic combination ceramic fibre material.
2. preparation method according to claim 1, which is characterized in that in step a), the diameter of the ceramic fibre is 2~
5μm。
3. preparation method according to claim 1, which is characterized in that in step a), the revolving speed of the mashing is 500~
1000r/min；The time of the mashing is 15~20min.
4. preparation method according to claim 1, which is characterized in that in step a), the mode of the dehydration forming is true
Suction filter；
The vacuum degree of the vacuum suction filter is 400~550mmHg；The time of the vacuum suction filter is 5~10s.
5. preparation method according to claim 1, which is characterized in that in step b), the concentration of the inorganic bonding agent is
20~40wt%.
6. preparation method according to claim 5, which is characterized in that the matter of the inorganic bonding agent and the ceramic fibre
Amount is than being (20~40): (60~80).
7. preparation method according to claim 5, which is characterized in that in step b), H in the acid solution+Concentration be 0.1
~1mol/L；OH in the lye-Concentration be 0.1~1mol/L；
The inorganic bonding agent and the mass ratio of pH adjusting agent are 100:(1~3).
8. preparation method according to claim 1, which is characterized in that in step b), the acid solution includes acetum, grass
One of acid solution, phosphoric acid solution, nitric acid solution, hydrochloric acid solution and sulfuric acid solution are a variety of；
The lye includes ammonium hydroxide and/or sodium hydroxide solution.
9. preparation method according to claim 1, which is characterized in that in step b), the temperature of the standing is 15~35
℃；The time of the standing is 10~20min.
10. preparation method according to claim 1, which is characterized in that in step c), the temperature of the drying is 80~
120℃；The time of the drying be 10~for 24 hours.
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| CN111410544A (en) * | 2020-04-29 | 2020-07-14 | 成都天道化工技术有限公司 | Method for manufacturing non-flexible refractory fiber product |
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| CN112523006A (en) * | 2020-11-27 | 2021-03-19 | 山东鲁阳节能材料股份有限公司 | Method for preparing high-density ceramic fiber board by secondary impregnation |
| CN112624721A (en) * | 2020-12-16 | 2021-04-09 | 山东鲁阳节能材料股份有限公司 | High-density ceramic fiber board with built-in embedded part and integrated forming method thereof |
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Application publication date: 20190419 |
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