CN108947546A - A kind of fire bond and its preparation method and application - Google Patents
A kind of fire bond and its preparation method and application Download PDFInfo
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- CN108947546A CN108947546A CN201810804402.5A CN201810804402A CN108947546A CN 108947546 A CN108947546 A CN 108947546A CN 201810804402 A CN201810804402 A CN 201810804402A CN 108947546 A CN108947546 A CN 108947546A
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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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/626—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
- C04B35/63—Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
- C04B35/632—Organic additives
- C04B35/634—Polymers
- C04B35/63448—Polymers obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- C04B35/63472—Condensation polymers of aldehydes or ketones
- C04B35/63476—Phenol-formaldehyde condensation polymers
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- 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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
- C04B35/10—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on aluminium oxide
- C04B35/101—Refractories from grain sized mixtures
- C04B35/103—Refractories from grain sized mixtures containing non-oxide refractory materials, e.g. carbon
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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
- C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
- C04B35/622—Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G14/00—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00
- C08G14/02—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes
- C08G14/04—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols
- C08G14/06—Condensation polymers of aldehydes or ketones with two or more other monomers covered by at least two of the groups C08G8/00 - C08G12/00 of aldehydes with phenols and monomers containing hydrogen attached to nitrogen
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- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3205—Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
- C04B2235/3206—Magnesium oxides or oxide-forming salts thereof
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- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/32—Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
- C04B2235/3217—Aluminum oxide or oxide forming salts thereof, e.g. bauxite, alpha-alumina
- C04B2235/3222—Aluminates other than alumino-silicates, e.g. spinel (MgAl2O4)
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- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/02—Composition of constituents of the starting material or of secondary phases of the final product
- C04B2235/30—Constituents and secondary phases not being of a fibrous nature
- C04B2235/42—Non metallic elements added as constituents or additives, e.g. sulfur, phosphor, selenium or tellurium
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Abstract
The invention discloses a kind of fire bonds and its preparation method and application, wherein, the preparation method of fire bond, include the following steps: after mixing phenol and formalin, using ammonium hydroxide as catalyst, after reacting 1~3h at 70~80 DEG C, 1~3h is reacted at 90~100 DEG C, obtains the binder that solid content is 66~72wt%.The mass ratio of formaldehyde is 100:35~50 in the phenol and formalin.The mass fraction of the ammonium hydroxide is 19~22%, and the mass ratio of phenol and ammonium hydroxide is 100:5~8.Fire bond provided by the invention keeps the polymer molecular weight to be formed moderate, narrow molecular weight distribution, for that can significantly improve the ontology of three-major-items product, the intensity of slag lining in refractory material by controlling necleophilic reaction rate.
Description
Technical field
The present invention relates to technical field of refractory materials, and in particular to a kind of fire bond and preparation method thereof and answers
With.
Background technique
Continuous-casting three-main-product includes long nozzle, integral column of sagger and submersed nozzle, is that the functionality in continuous-casting steel-making technique is resistance to
Fiery material.Their effect is connecting ladle, tundish and crystallizer three in one, flow control and water conservancy diversion molten steel, is prevented
Only secondary oxidation of steel.Continuous-casting three-main-product mainly makees bonding agent using resin, after granulation, isostatic pressing, baking and firing
With higher-strength and good thermal shock resistance.
Ammonia catalytic resin is the catalytic action polymerization with phenolic compound and aldehyde compound through ammonia and manufactured one kind is closed
At resin, phenolic compound mainly has phenol, cresols, xylenol etc., and aldehyde compound mainly has formaldehyde, furfural, paraformaldehyde
Deng.Three-major-items mainly pass through addition and polycondensation two using formaldehyde and phenol as raw material with resin under a certain amount of ammonia catalytic action
The resin with certain molecular weight formed after a reaction.It is adjacent since there are a hydroxyls in Benzene Molecule structure for phenol
Hydrogen atom activity with higher on position and contraposition, to make have 3 active function groups in molecule, in certain environmental condition
Under, the hydrogen atom of phenyl ring hydroxyl ortho position and contraposition easily occurs addition reaction with the carbonyl in formaldehyde molecule and forms methylolation benzene
Phenol, with the further progress of reaction, the methylolated phenol of generation due to containing active function groups, can in phenol molecule
Active function groups polymerize again, while can also continue to be condensed into macromolecular between hydroxymethylphenol, with polymerization reaction
Lasting to carry out, final polymerization forms the phenolic resin with certain molecular weight.
The reaction system of ammonia catalytic resin is complex, still not fully aware of to its reaction mechanism mechanism of reaction at present, raw when ammonia is catalyzed
At resin almost lose water solubility immediately, the molecular weight of generation is larger；It, which generates intermediate product, dihydroxy benzylamine, three hydroxyl benzylamines
Deng forming complicated intermediate product with phenol in addition, ammonia and formaldehyde are readily generated hexamethylenetetramine.
Summary of the invention
The present invention provides a kind of fire bonds and its preparation method and application, pass through control necleophilic reaction speed
Rate keeps the polymer molecular weight to be formed moderate, narrow molecular weight distribution, for that can significantly improve three-major-items system in refractory material
The intensity of the ontologies of product, slag lining.
A kind of preparation method of fire bond, includes the following steps:
After phenol and formalin are mixed, using ammonium hydroxide as catalyst, after reacting 1~3h at 70~80 DEG C,
1~3h is reacted at 90~100 DEG C, obtains the binder that solid content is 66~72wt%.
The intermediate product methylol that the present invention is reacted with ammonia water by control reaction temperature and reaction time, control formaldehyde
Ammonia, and the further ratio of the intermediate product dihydroxy benzylamine, three hydroxyl benzylamines of polymerization generation, make the polymer molecular structure to be formed
It is moderate, narrow molecular weight distribution.
The solid content of the fire bond is 66~72wt%, can guarantee three-major-items product during making material
Granulation outcome.
The fire bond can significantly improve the intensity of three-major-items for three-major-items product, in order to guarantee that three is big
Part product has better intensity, it is preferable that the mass ratio of formaldehyde is 100:35~50 in the phenol and formalin.
Preferably, the mass fraction of the ammonium hydroxide is 19~22%, the mass ratio of phenol and ammonium hydroxide is 100:5~8.
Preferably, the mass fraction of the formalin is 37%, the mass ratio of phenol and formalin is
100:100~130.
The present invention also provides a kind of fire bonds, are prepared using the refractory material preparation method.
The present invention also provides application of the binder described in one kind in refractory material, include the following steps: fire resisting
Aggregate, refractory powder and binder as claimed in claim 5 carry out high speed mixing granulator, then successively mixed through ageing mixture,
Refractory material is prepared in molding, baking, firing.
Preferably, the refractory aggregate is corundum, the refractory powder is made of spinelle fine powder and graphite, each component
Weight it is as follows:
The grain size distribution of the corundum is as follows:
2-1mm 30~40
1-0.5mm 30~40
< 0.5mm 30~40.
The spinelle fine powder is 170 mesh~200 mesh, and graphite particle size is that -198 (i.e. the graphite of 98% mass fraction can be with
It is logical to sieve with 100 mesh sieve).
The three-major-items refractory material prepared using binder provided by the invention, intensity is high, rises in continuous-casting steel pouring process
To water conservancy diversion, the effect for preventing secondary oxidation of steel, controlling molten steel flow speed, service life can be greatly prolonged.
Specific embodiment
Below with reference to embodiment, the present invention will be further described, not limiting of its scope.
Embodiment 1
A kind of preparation method of fire bond, includes the following steps:
(1) formalin that phenol and mass fraction are 37% is placed in reaction kettle and is stirred evenly, phenol and formaldehyde
The mass ratio of aqueous solution is 100:105；
(2) mass fraction is added into reaction kettle as 20% ammonium hydroxide, the mass ratio of phenol and ammonium hydroxide is 100:6；
(3) 2h is stirred under the conditions of 75 DEG C；
(4) 2h is stirred under the conditions of 95 DEG C；
(5) solvent alcohol is added in decompression dehydration, and the fire bond that solid content is 68wt% is made.
The process that three-major-items refractory material is prepared using the binder, is included the following steps:
A, 60% refractory aggregate corundum, 20% spinelle fine powder, 10% graphite are added in muller；
Mass fraction is calculated on the basis of material total weight, corundum granularity is 2-1mm accounting 20%, and corundum granularity is 1-
0.5mm accounting 20%, corundum granularity are 0.5-0mm accounting 20%；Spinelle powder particle size is 180 mesh；Graphite is -198；
B, bonding agent prepared by addition 10% carries out high speed and is kneaded granulation；
C, pug is granulated through ageing mixture mixed use after for 24 hours；
D, mixed pug be added mold through etc. static pressure 120MPa pressure forming；
E, after molding green body through 180 DEG C baking, 900 DEG C firing, sharp processing and three-major-items product is made.
The three-major-items product of preparation is cut into 40 × 40 × 40mm bulk sample, the strength at normal temperature for detecting sample is
25MPa。
Embodiment 2
A kind of preparation method of fire bond, includes the following steps:
(1) formalin that phenol and mass fraction are 37% is placed in reaction kettle and is stirred evenly, phenol and formaldehyde
The mass ratio of aqueous solution is 100:115；
(2) mass fraction is added into reaction kettle as 21% ammonium hydroxide, the mass ratio of phenol and ammonium hydroxide is 100:6；
(3) 2h is stirred under the conditions of 75 DEG C；
(4) 2h is stirred under the conditions of 95 DEG C；
(5) solvent alcohol is added in decompression dehydration, and the fire bond that solid content is 68wt% is made.
Three-major-items product is prepared using method described in embodiment 1, the three-major-items product of preparation is cut into 40 ×
40 × 40mm bulk sample, the strength at normal temperature for detecting sample is 27MPa.
Embodiment 3
A kind of preparation method of fire bond, includes the following steps:
(1) formalin that phenol and mass fraction are 37% is placed in reaction kettle and is stirred evenly, phenol and formaldehyde
The mass ratio of aqueous solution is 100:125；
(2) mass fraction is added into reaction kettle as 22% ammonium hydroxide, the mass ratio of phenol and ammonium hydroxide is 100:6；
(3) 2h is stirred under the conditions of 75 DEG C；
(4) 2h is stirred under the conditions of 95 DEG C；
(5) solvent alcohol is added in decompression dehydration, and the fire bond that solid content is 68wt% is made.
Three-major-items product is prepared using method described in embodiment 1, the three-major-items product of preparation is cut into 40 ×
40 × 40mm bulk sample, the strength at normal temperature for detecting sample is 26MPa.
Embodiment 4
A kind of preparation method of fire bond, includes the following steps:
(1) formalin that phenol and mass fraction are 37% is placed in reaction kettle and is stirred evenly, phenol and formaldehyde
The mass ratio of aqueous solution is 100:105；
(2) mass fraction is added into reaction kettle as 20% ammonium hydroxide, the mass ratio of phenol and ammonium hydroxide is 100:6；
(3) 2h is stirred under the conditions of 75 DEG C；
(4) 2h is stirred under the conditions of 95 DEG C；
(5) solvent alcohol is added in decompression dehydration, and the fire bond that solid content is 71wt% is made.
Three-major-items product is prepared using method described in embodiment 1, the three-major-items product of preparation is cut into 40 ×
40 × 40mm bulk sample, the strength at normal temperature for detecting sample is 26MPa.
Embodiment 5
A kind of preparation method of fire bond, includes the following steps:
(1) formalin that phenol and mass fraction are 37% is placed in reaction kettle and is stirred evenly, phenol and formaldehyde
The mass ratio of aqueous solution is 100:115；
(2) mass fraction is added into reaction kettle as 21% ammonium hydroxide, the mass ratio of phenol and ammonium hydroxide is 100:6；
(3) 2h is stirred under the conditions of 75 DEG C；
(4) 2h is stirred under the conditions of 95 DEG C；
(5) solvent alcohol is added in decompression dehydration, and the fire bond that solid content is 71wt% is made.
Three-major-items product is prepared using method described in embodiment 1, the three-major-items product of preparation is cut into 40 ×
40 × 40mm bulk sample, the strength at normal temperature for detecting sample is 29MPa.
Embodiment 6
A kind of preparation method of fire bond, includes the following steps:
(1) formalin that phenol and mass fraction are 37% is placed in reaction kettle and is stirred evenly, phenol and formaldehyde
The mass ratio of aqueous solution is 100:125；
(2) mass fraction is added into reaction kettle as 22% ammonium hydroxide, the mass ratio of phenol and ammonium hydroxide is 100:6；
(3) 2h is stirred under the conditions of 75 DEG C；
(4) 2h is stirred under the conditions of 95 DEG C；
(5) solvent alcohol is added in decompression dehydration, and the fire bond that solid content is 71wt% is made.
Three-major-items product is prepared using method described in embodiment 1, the three-major-items product of preparation is cut into 40 ×
40 × 40mm bulk sample, the strength at normal temperature for detecting sample is 27MPa.
Comparative example 1
The preparation method of conventional refractory materials binder, includes the following steps:
(1) formalin that phenol and mass fraction are 37% is placed in reaction kettle and is stirred evenly, phenol and formaldehyde
The mass ratio of aqueous solution is 100:100；
(2) mass fraction is added into reaction kettle as 25% ammonium hydroxide, the mass ratio of phenol and ammonium hydroxide is 100:5；
(3) 1h is stirred under the conditions of 75 DEG C；
(4) 1h is stirred under the conditions of 100 DEG C；
(5) solvent alcohol is added in decompression dehydration, and the fire bond that solid content is 69wt% is made.
Three-major-items product is prepared using method described in embodiment 1, the three-major-items product of preparation is cut into 40 ×
40 × 40mm bulk sample, the strength at normal temperature for detecting sample is 22MPa.
Comparative example 2
The preparation method of conventional refractory materials binder, includes the following steps:
(1) formalin that phenol and mass fraction are 37% is placed in reaction kettle and is stirred evenly, phenol and formaldehyde
The mass ratio of aqueous solution is 100:105；
(2) mass fraction is added into reaction kettle as 25% ammonium hydroxide, the mass ratio of phenol and ammonium hydroxide is 100:4；
(3) 1h is stirred under the conditions of 80 DEG C；
(4) 0.5h is stirred under the conditions of 100 DEG C；
(5) solvent alcohol is added in decompression dehydration, and the fire bond that solid content is 68wt% is made.
Three-major-items product is prepared using method described in embodiment 1, the three-major-items product of preparation is cut into 40 ×
40 × 40mm bulk sample, the strength at normal temperature for detecting sample is 21MPa.
Comparative example 3
The preparation method of conventional refractory materials binder, includes the following steps:
(1) formalin that phenol and mass fraction are 37% is placed in reaction kettle and is stirred evenly, phenol and formaldehyde
The mass ratio of aqueous solution is 100:110；
(2) mass fraction is added into reaction kettle as 25% ammonium hydroxide, the mass ratio of phenol and ammonium hydroxide is 100:3；
(3) 0.5h is stirred under the conditions of 80 DEG C；
(4) 1h is stirred under the conditions of 100 DEG C；
(5) solvent alcohol is added in decompression dehydration, and the fire bond that solid content is 67wt% is made.
Three-major-items product is prepared using method described in embodiment 1, the three-major-items product of preparation is cut into 40 ×
40 × 40mm bulk sample, the strength at normal temperature for detecting sample is 19MPa.
According to the disclosure and teachings of the above specification, those skilled in the art in the invention can also be to above-mentioned embodiment party
Formula carries out change and modification appropriate.Therefore, the invention is not limited to the specific embodiments disclosed and described above, to this
Some modifications and changes of invention should also be as falling into the scope of the claims of the present invention.In addition, although this specification
In use some specific terms, these terms are merely for convenience of description, does not limit the present invention in any way.
Claims (7)
1. a kind of preparation method of fire bond, which comprises the steps of:
After phenol and formalin are mixed, using ammonium hydroxide as catalyst, at 70~80 DEG C after 1~3h of reaction, 90~
1~3h is reacted at 100 DEG C, obtains the binder that solid content is 66~72wt%.
2. the preparation method of fire bond as described in claim 1, which is characterized in that the phenol and formaldehyde are water-soluble
The mass ratio of formaldehyde is 100:35~50 in liquid.
3. the preparation method of fire bond as described in claim 1, which is characterized in that the mass fraction of the ammonium hydroxide
It is 19~22%, the mass ratio of phenol and ammonium hydroxide is 100:5~8.
4. the preparation method of fire bond as described in claim 1, which is characterized in that the matter of the formalin
Measuring score is 37%, and the mass ratio of phenol and formalin is 100:100~130.
5. a kind of fire bond, which is characterized in that using such as the described in any item preparation method systems of Claims 1 to 4
It is standby to obtain.
6. a kind of application of binder as claimed in claim 5 in refractory material, which comprises the steps of:
Refractory aggregate, refractory powder and binder as claimed in claim 5 are subjected to high speed mixing granulator, then successively through tired
Refractory material is prepared in material, mixed, molding, baking, firing.
7. application of the binder as claimed in claim 6 in refractory material, which is characterized in that the refractory aggregate is rigid
Beautiful, the described refractory powder is made of spinelle fine powder and graphite, and the weight of each component is as follows:
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