CN110423128A - A kind of preparation method of the high refractoriness fire clay of anti-shrink - Google Patents
A kind of preparation method of the high refractoriness fire clay of anti-shrink Download PDFInfo
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- CN110423128A CN110423128A CN201910719391.5A CN201910719391A CN110423128A CN 110423128 A CN110423128 A CN 110423128A CN 201910719391 A CN201910719391 A CN 201910719391A CN 110423128 A CN110423128 A CN 110423128A
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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
- C04B35/66—Monolithic refractories or refractory mortars, including those whether or not containing clay
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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
- 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
- C04B2235/38—Non-oxide ceramic constituents or additives
- C04B2235/3817—Carbides
- C04B2235/3826—Silicon carbides
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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
- 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
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/443—Nitrates or nitrites
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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
- 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
- C04B2235/44—Metal salt constituents or additives chosen for the nature of the anions, e.g. hydrides or acetylacetonate
- C04B2235/447—Phosphates or phosphites, e.g. orthophosphate, hypophosphite
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Abstract
The invention discloses a kind of preparation methods of the high refractoriness fire clay of anti-shrink, belong to technical field of fire-resistant material preparation.The present invention is first using river sand as raw material, it is pulverized and sieved to obtain river sand powder, then dried object is dried to obtain after mixing river sand powder and brown sugar water, dried object carbonize simultaneously high temperature sintering again, silicon carbide is prepared, mixing fines is made in oriental topaz and kyanite mixing and ball milling again, then with potassium carbonate, zirconium oxide and diammonium hydrogen phosphate are raw material, it carries out solid-phase sintering and Potassium dizirconium phosphate powder is prepared, finally with silicon carbide, mix fines, Potassium dizirconium phosphate and strontium nitrate are powder, phenolic resin and ethylene glycol are that the high refractoriness fire clay of anti-shrink is prepared in bonding agent.
Description
Technical field
The invention discloses a kind of preparation methods of the high refractoriness fire clay of anti-shrink, belong to refractory material technology of preparing neck
Domain.
Background technique
Fire clay is also known as chamotte or joint filler (powder dress object).Puzzle joint material as refractory product masonry.It can divide by material
For clay matter, High-Alumina, siliceous and magnesite refractory etc..It is made of refractory powder, bonding agent and additive.It is almost all of resistance to
Fiery raw material can be made for preparing powder used in fire clay.With grog refractory powder add appropriate plastic clay make bonding agent and
Plasticizer and it is manufactured claim common fire clay, normal temperature strength is lower, and Ceramic bond is formed under high temperature just has higher-strength.With
The hydraulicity, air-setting or thermohardening bond material are chemically combined fire clay as the title of bonding agent, form Ceramic bond being lower than
It generates certain chemical reaction before temperature and hardens.
The granularity of fire clay is according to requirements different, and Limit Grain Size is generally less than 1mm, and some is less than 0.5mm or more
Carefully.The material for selecting refractory wass, is considered as consistent with the material of the refractory product of masonry.Fire resisting Fender is made outside puzzle joint material,
The protective coating of liner body can also be used as using semar technique or gunite.
Refractory material is many kinds of, is usually divided into common refractory (1580~1770 DEG C), advanced by refractoriness height
Refractory material (1770~2000 DEG C) and superrefractory (2000 DEG C or more)；By chemical characteristic be divided into acid refractory,
Neutral refractory and basic refractory.In addition, there are also the refractory materials for being used for special occasions.
Fire clay according to composition material difference can be divided into clay matter fire clay, High-Alumina fire clay, silica fireclay,
Magnesite refractory etc..Fire clay and can be divided into following three classes according to the difference of bonding agent: Ceramic bond fire clay it be by fire resisting
The mixture of fine aggregate and vitrified bond composition.Hydraulicity combined fire resistant mud it be by fire resisting fine aggregate and mainly in combination with work
The mixture of hydraulicity bonding agent composition.The mixing that chemical bonding fire clay is made of fire resisting fine aggregate and chemical bond
Material.The condition of delivery can be dry shape either pulpous state, lower than hardening below Ceramic bond temperature.Fire clay is divided into product
With two kinds of semi-finished product.
Anode carbon product used in aluminium cell is made of firing in roaster, to roast roaster used,
Flue wall part refractory brick build to use fire clay, due to the maturing temperature of roaster to be generally more than 1200 DEG C even more
Height, therefore fire clay needs adhesion strength with higher and higher refractoriness in low temperature, medium temperature, high temperature.Currently, big portion
The clayey fire clay that the fire clay of the baking furnace flame path wall divided is all made of, Al2O3Content is between 45~48%, and silicon carbide
Content only has 5~15%, during applied at elevated temperature, shrinks greatly, makes to generate gap between furnace body and refractory material, cause leakage fire
It leaks out, and clay fire clay adhesion strength and refractoriness are lower, it is poor to the impermeability of molten metal.
Therefore, inventing the fire clay that a kind of anti-contracility is good and refractoriness is high is to have very much to technical field of fire-resistant material preparation
It is necessary.
Summary of the invention
Present invention mainly solves the technical issues of, for the clayey fire clay that common fire clay is all made of at present,
Al2O3Content is between 45~48%, and carborundum content only has 5~15%, during applied at elevated temperature, shrink it is big, make furnace body and
Gap is generated between refractory material, leakage fire is caused to leak out, and clay fire clay adhesion strength and refractoriness are lower, to melting gold
The defect of the impermeability difference of category, provides a kind of preparation method of high refractoriness fire clay of anti-shrink.
In order to solve the above-mentioned technical problem, the technical scheme adopted by the invention is that:
A kind of high refractoriness fire clay of anti-shrink the preparation method comprises the following steps:
According to parts by weight, 40~50 parts are weighed from preparing silicon carbide, 10~15 parts of mixing fineves, 3~5 parts of Potassium dizirconium phosphate powder, 1
It is put into slurry mixer, is stirred after~2 parts of strontium nitrates, 4~5 parts of phenolic resin and 13~15 parts of ethylene glycol mixing to obtain the final product
The high refractoriness fire clay of anti-shrink；
From the preparation of preparing silicon carbide:
(1) weigh river sand and be put into pulverizer and crush and sieve with 100 mesh sieve, obtain sieving river sand powder, will sieving river sand powder and
It is fitted into beaker after brown sugar and water mixing, moves into baking oven after being stirred 15~20min, dry at 105~110 DEG C to perseverance
Weight, obtains dried object；
(2) above-mentioned dried object is put into retort, is obtained under nitrogen protection with 300~400 DEG C of 1~2h of temperature charing process
To carbide, carbide is moved into resistance furnace, under protection of argon gas, high temperature sintering reaction；
(3) after to above-mentioned sintering reaction, under air atmosphere, continue high-temperature calcination, product is taken out after sintering, successively
It is rinsed 3~5 times with hydrofluoric acid and water, it is dry to get from preparing silicon carbide after the completion of rinsing；
Mix the preparation of fines:
Oriental topaz and kyanite are weighed, is first put into pulverizer after crushing 1~2h and obtains coarse fodder, then pressing ball material mass ratio is 10:1
It is put into ball grinder after stainless steel is ground pearl and coarse fodder mixing, 3~5h of ball-milling treatment obtains mixing fines；
The preparation of Potassium dizirconium phosphate powder:
It is fitted into sintering furnace after potassium carbonate, zirconium oxide and diammonium hydrogen phosphate are mixed, under protection of argon gas, is heated to 600
It~800 DEG C, discharges after 3~4h of heat preservation sintering, is put into 1~2h of crushing in pulverizer, Potassium dizirconium phosphate is made in cooled to room temperature
Powder.
In the preparation of the high refractoriness fire clay of anti-shrink, according to parts by weight, it is 40~50 parts, mixes carefully from preparing silicon carbide
Material is 10~15 parts, Potassium dizirconium phosphate powder is 3~5 parts, strontium nitrate is 1~2 part, phenolic resin is 4~5 parts, ethylene glycol 13
~15 parts.
From in the preparation of preparing silicon carbide, the mass ratio of be sieved river sand powder and brown sugar and water is 1:1:2.
From in the preparation of preparing silicon carbide, high temperature sintering reaction temperature be 1500~1600 DEG C, high temperature sintering reaction when
Between be 4~6h.
From in the preparation of preparing silicon carbide, the temperature of high-temperature calcination is 800~900 DEG C, and the time of high-temperature calcination is 1~2h.
In the preparation for mixing fines, the mass ratio of oriental topaz and kyanite is 10:1.
In the preparation of Potassium dizirconium phosphate powder, the molar ratio of potassium carbonate, zirconium oxide and diammonium hydrogen phosphate is 1:4:6.
The method have the benefit that:
(1) present invention is pulverized and sieved to obtain river sand powder, then by river sand powder and brown sugar water first using river sand as raw material
Be dried to obtain dried object after mixing, then dried object carbonize and high temperature sintering, be prepared silicon carbide, then by oriental topaz and
Mixing fines is made in kyanite mixing and ball milling, then using potassium carbonate, zirconium oxide and diammonium hydrogen phosphate as raw material, carries out solid-phase sintering
Potassium dizirconium phosphate powder is prepared, finally using silicon carbide, mixing fines, Potassium dizirconium phosphate and strontium nitrate as powder, phenolic resin and
Ethylene glycol is that bonding agent is prepared the high refractoriness fire clay of anti-shrink, the present invention using rich silica containing river sand as raw material,
It is pulverized and sieved and powder is made, then using brown sugar as carbon source and river sand admixture of powder, silicon carbide is prepared, then again with richness
Mixing fines is made for raw material and kyanite co-grinding in salic oriental topaz, then with potassium carbonate, zirconium oxide and phosphoric acid hydrogen
Diammonium is raw material, carries out solid-phase sintering and Potassium dizirconium phosphate powder is prepared, and add bonding agent ingredient and fire clay is prepared, this
Since carborundum content is higher than common fire clay in the fire clay of invention, silicon carbide can be with oxygen reaction life under high temperature environment
At silica and charcoal, the silica of generation is the sticky film of one layer of densification, can prevent the infiltration of point molten metal from letting out
Dew；
(2) also containing rich salic oriental topaz powder in fire clay of the present invention, oriental topaz powder can be with the two of silicon carbide life
Silica reacts at high temperature, generates Ceramic bond phase, so that the high temperature bond phase of fire clay is improved, and aquamaine stone powder
It can undergo phase transition at high temperature, the high mullite of refractoriness and adjoint expansion be formed, thus improving the same of fire clay refractoriness
When, the high-temperature shrinkage phenomenon of fire clay is compensated for, avoids and shrinks the generation that generation crack causes leakage fire to be leaked out, and the present invention is resistance to
It also added Potassium dizirconium phosphate and strontium nitrate in chamotte, under the high temperature conditions, Potassium dizirconium phosphate also has high-temperature expansion, further more
The high-temperature shrinkage phenomenon for having mended fire clay avoids and shrinks the generation that generation crack causes leakage fire to be leaked out, in addition, in high temperature action
Under, strontium can enter and replace part zirconium in the lattice of Potassium dizirconium phosphate, to generate basic zirconium phosphate strontium potassium solid solution, the basic zirconium phosphate strontium of generation
Potassium is dissolved volume property and stablizes, and refractoriness is splendid, improves the refractoriness of fire clay again, has broad application prospects.
Specific embodiment
Weigh river sand and be put into pulverizer and crush and sieve with 100 mesh sieve, obtain sieving river sand powder, will sieving river sand powder and
Brown sugar and water are to be fitted into beaker after 1:1:2 mixing in mass ratio, move into baking oven after being stirred 15~20min, 105~
It dries at 110 DEG C to constant weight, obtains dried object；Above-mentioned dried object is put into retort, under nitrogen protection with 300~400
DEG C 1~2h of temperature charing process obtain carbide, by carbide move into resistance furnace in, under protection of argon gas, be heated to
1500~1600 DEG C, high temperature sintering reacts 4~6h；After to above-mentioned sintering reaction, under air atmosphere, it is cooled to 800~
900 DEG C, continue 1~2h of high-temperature calcination, product is taken out after sintering, is successively rinsed 3~5 times, rinsed with hydrofluoric acid and water
At rear drying to get from preparing silicon carbide；Oriental topaz and kyanite are weighed for 10:1 in mass ratio, is first put into pulverizer and crushes 1
Obtain coarse fodder after~2h, then by ball material mass ratio be 10:1 will stainless steel grind pearl and coarse fodder mix after be put into ball grinder, ball milling
3~5h is handled, mixing fines is obtained；It is packed into and burns after in molar ratio mixing potassium carbonate, zirconium oxide and diammonium hydrogen phosphate for 1:4:6
In freezing of a furnace, under protection of argon gas, 600~800 DEG C is heated to, is discharged after 3~4h of heat preservation sintering, is put into pulverizer and crushes
Potassium dizirconium phosphate powder is made in 1~2h, cooled to room temperature；According to parts by weight, 40~50 parts of spare self-control carbonizations are weighed
Silicon, 10~15 parts of mixing fineves, 3~5 parts of Potassium dizirconium phosphate powder, 1~2 part of strontium nitrate, 4~5 parts of phenolic resin and 13~15 parts
It is put into slurry mixer, is stirred up to the high refractoriness fire clay of anti-shrink after ethylene glycol mixing.
Embodiment 1
From the preparation of preparing silicon carbide:
It weighs river sand and is put into pulverizer and crush and sieve with 100 mesh sieve, obtain sieving river sand powder, by sieving river sand powder and brown sugar
And water is to be fitted into beaker after 1:1:2 is mixed in mass ratio, moves into baking oven after being stirred 15min, dries extremely at 105 DEG C
Constant weight obtains dried object；
Above-mentioned dried object is put into retort, carbide is obtained with 300 DEG C of temperature charing process 1h under nitrogen protection, it will
Carbide moves into resistance furnace, under protection of argon gas, is heated to 1500 DEG C, high temperature sintering reacts 4h；
After to above-mentioned sintering reaction, under air atmosphere, 800 DEG C are cooled to, continues high-temperature calcination 1h, is taken after sintering
Product out is successively rinsed 3 times with hydrofluoric acid and water, dry to get from preparing silicon carbide after the completion of rinsing；
Mix the preparation of fines:
Oriental topaz and kyanite are weighed for 10:1 in mass ratio, is first put into pulverizer after crushing 1h and obtains coarse fodder, then press ball material
Mass ratio is to be put into ball grinder after stainless steel is ground pearl and coarse fodder mixing by 10:1, and ball-milling treatment 3h obtains mixing fines；
The preparation of Potassium dizirconium phosphate powder:
It is fitted into sintering furnace after in molar ratio mixing potassium carbonate, zirconium oxide and diammonium hydrogen phosphate for 1:4:6, is protected in argon gas
Under, 600 DEG C are heated to, is discharged after heat preservation sintering 3h, is put into pulverizer and crushes 1h, phosphorus is made in cooled to room temperature
Sour zirconium potassium powder；
The preparation of impervious high refractoriness fire clay:
According to parts by weight, weigh 40 parts it is spare from preparing silicon carbide, 10 parts of mixing fineves, 3 parts of Potassium dizirconium phosphate powder, 1 part of nitre
It is put into slurry mixer, is stirred up to the high refractoriness of anti-shrink after sour strontium, 4 parts of phenolic resin and 13 parts of ethylene glycol mixing
Fire clay.
Embodiment 2
From the preparation of preparing silicon carbide:
It weighs river sand and is put into pulverizer and crush and sieve with 100 mesh sieve, obtain sieving river sand powder, by sieving river sand powder and brown sugar
And water is to be fitted into beaker after 1:1:2 is mixed in mass ratio, moves into baking oven after being stirred 17min, dries extremely at 107 DEG C
Constant weight obtains dried object；
Above-mentioned dried object is put into retort, carbide is obtained with 350 DEG C of temperature charing process 1.5h under nitrogen protection,
Carbide is moved into resistance furnace, under protection of argon gas, is heated to 1550 DEG C, high temperature sintering reacts 5h；
After to above-mentioned sintering reaction, under air atmosphere, 850 DEG C are cooled to, continues high-temperature calcination 1.5h, after sintering
Product is taken out, is successively rinsed 4 times with hydrofluoric acid and water, it is dry to get from preparing silicon carbide after the completion of rinsing；
Mix the preparation of fines:
Oriental topaz and kyanite are weighed for 10:1 in mass ratio, is first put into pulverizer after crushing 1.5h and obtains coarse fodder, then press ball
Material mass ratio is to be put into ball grinder after stainless steel is ground pearl and coarse fodder mixing by 10:1, and ball-milling treatment 4h obtains mixing fines；
The preparation of Potassium dizirconium phosphate powder:
It is fitted into sintering furnace after in molar ratio mixing potassium carbonate, zirconium oxide and diammonium hydrogen phosphate for 1:4:6, is protected in argon gas
Under, 700 DEG C are heated to, is discharged after heat preservation sintering 3.5h, is put into pulverizer and crushes 1.5h, cooled to room temperature, system
Obtain Potassium dizirconium phosphate powder；
The preparation of impervious high refractoriness fire clay:
According to parts by weight, weigh 45 parts it is spare from preparing silicon carbide, 12 parts of mixing fineves, 4 parts of Potassium dizirconium phosphate powder, 1 part of nitre
It is put into slurry mixer, is stirred up to the high refractoriness of anti-shrink after sour strontium, 4 parts of phenolic resin and 14 parts of ethylene glycol mixing
Fire clay.
Embodiment 3
From the preparation of preparing silicon carbide:
It weighs river sand and is put into pulverizer and crush and sieve with 100 mesh sieve, obtain sieving river sand powder, by sieving river sand powder and brown sugar
And water is to be fitted into beaker after 1:1:2 is mixed in mass ratio, moves into baking oven after being stirred 20min, dries extremely at 110 DEG C
Constant weight obtains dried object；
Above-mentioned dried object is put into retort, carbide is obtained with 400 DEG C of temperature charing process 2h under nitrogen protection, it will
Carbide moves into resistance furnace, under protection of argon gas, is heated to 1600 DEG C, high temperature sintering reacts 6h；
After to above-mentioned sintering reaction, under air atmosphere, 900 DEG C are cooled to, continues high-temperature calcination 2h, is taken after sintering
Product out is successively rinsed 5 times with hydrofluoric acid and water, dry to get from preparing silicon carbide after the completion of rinsing；
Mix the preparation of fines:
Oriental topaz and kyanite are weighed for 10:1 in mass ratio, is first put into pulverizer after crushing 2h and obtains coarse fodder, then press ball material
Mass ratio is to be put into ball grinder after stainless steel is ground pearl and coarse fodder mixing by 10:1, and ball-milling treatment 5h obtains mixing fines；
The preparation of Potassium dizirconium phosphate powder:
It is fitted into sintering furnace after in molar ratio mixing potassium carbonate, zirconium oxide and diammonium hydrogen phosphate for 1:4:6, is protected in argon gas
Under, 800 DEG C are heated to, is discharged after heat preservation sintering 4h, is put into pulverizer and crushes 2h, phosphorus is made in cooled to room temperature
Sour zirconium potassium powder；
The preparation of impervious high refractoriness fire clay:
According to parts by weight, weigh 50 parts it is spare from preparing silicon carbide, 15 parts of mixing fineves, 5 parts of Potassium dizirconium phosphate powder, 2 parts of nitre
It is put into slurry mixer, is stirred up to the high refractoriness of anti-shrink after sour strontium, 5 parts of phenolic resin and 15 parts of ethylene glycol mixing
Fire clay.
Comparative example 1: it is essentially identical with the preparation method of embodiment 2, it has only the difference is that lacking from preparing silicon carbide.
Comparative example 2: it is essentially identical with the preparation method of embodiment 2, it has only the difference is that lacking Potassium dizirconium phosphate powder.
Comparative example 3: the preparation method of the high refractoriness fire clay of anti-shrink of Shandong company production.
Refractoriness test is detected by GB/T 7322-2017 standard.
Flexural strength test is detected by GB/T 3002-2017 standard.
Impermeability test: the fire clay in Examples 1 to 3 and comparative example is used in the seam equipped with molten metal, is seen
Whether examine has molten metal infiltration.
Linear shrinkage ratio test is detected by GB/T 14235.4-93 standard.
Table 1: fire clay performance measurement result
| Detection project | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Refractoriness (DEG C) | 1835 | 1840 | 1850 | 1160 | 1035 | 1170 |
| Flexural strength (MPa) (1300 DEG C × for 24 hours) | 7.2 | 7.3 | 7.5 | 4.2 | 4.8 | 4.9 |
| It is impervious | No metal infiltration | No metal infiltration | No metal infiltration | Obvious infiltration | Light percolation | Light percolation |
| Linear shrinkage ratio (%) (1300 DEG C) | -0.015 | -0.012 | -0.009 | -0.041 | -0.052 | -0.038 |
In summary, the high refractoriness fire clay refractoriness of anti-shrink of the invention is high as can be seen from Table 1, and High anti bending strength glues
Knot property is good, and impervious good, no molten metal infiltration, high temperature linear shrinkage ratio is low, has broad application prospects.
The foregoing is merely preferred modes of the invention, are not intended to limit the invention, all in spirit and original of the invention
Within then, any modification, equivalent replacement, improvement and so on be should all be included in the protection scope of the present invention.
Claims (7)
1. a kind of preparation method of the high refractoriness fire clay of anti-shrink, it is characterised in that specific preparation step are as follows:
According to parts by weight, 40~50 parts are weighed from preparing silicon carbide, 10~15 parts of mixing fineves, 3~5 parts of Potassium dizirconium phosphate powder, 1
It is put into slurry mixer, is stirred after~2 parts of strontium nitrates, 4~5 parts of phenolic resin and 13~15 parts of ethylene glycol mixing to obtain the final product
The high refractoriness fire clay of anti-shrink；
The preparation step from preparing silicon carbide are as follows:
(1) weigh river sand and be put into pulverizer and crush and sieve with 100 mesh sieve, obtain sieving river sand powder, will sieving river sand powder and
It is fitted into beaker after brown sugar and water mixing, moves into baking oven after being stirred 15~20min, dry at 105~110 DEG C to perseverance
Weight, obtains dried object；
(2) above-mentioned dried object is put into retort, is obtained under nitrogen protection with 300~400 DEG C of 1~2h of temperature charing process
To carbide, carbide is moved into resistance furnace, under protection of argon gas, high temperature sintering reaction；
(3) after to above-mentioned sintering reaction, under air atmosphere, continue high-temperature calcination, product is taken out after sintering, successively
It is rinsed 3~5 times with hydrofluoric acid and water, it is dry to get from preparing silicon carbide after the completion of rinsing；
The preparation step of the mixing fines are as follows:
Oriental topaz and kyanite are weighed, is first put into pulverizer after crushing 1~2h and obtains coarse fodder, then pressing ball material mass ratio is 10:1
It is put into ball grinder after stainless steel is ground pearl and coarse fodder mixing, 3~5h of ball-milling treatment obtains mixing fines；
The preparation step of the Potassium dizirconium phosphate powder are as follows:
It is fitted into sintering furnace after potassium carbonate, zirconium oxide and diammonium hydrogen phosphate are mixed, under protection of argon gas, is heated to 600
It~800 DEG C, discharges after 3~4h of heat preservation sintering, is put into 1~2h of crushing in pulverizer, Potassium dizirconium phosphate is made in cooled to room temperature
Powder.
2. a kind of preparation method of the high refractoriness fire clay of anti-shrink according to claim 1, it is characterised in that: described anti-
In the specific preparation step for shrinking high refractoriness fire clay, according to parts by weight, it is 40~50 parts, mixes fines from preparing silicon carbide
For 10~15 parts, Potassium dizirconium phosphate powder be 3~5 parts, strontium nitrate is 1~2 part, phenolic resin is 4~5 parts, ethylene glycol be 13~
15 parts.
3. a kind of preparation method of the high refractoriness fire clay of anti-shrink according to claim 1, it is characterised in that: it is described from
In the preparation step (1) of preparing silicon carbide, the mass ratio of be sieved river sand powder and brown sugar and water is 1:1:2.
4. a kind of preparation method of the high refractoriness fire clay of anti-shrink according to claim 1, it is characterised in that: it is described from
In the preparation step (2) of preparing silicon carbide, high temperature sintering reaction temperature be 1500~1600 DEG C, high temperature sintering reaction time be
4~6h.
5. a kind of preparation method of the high refractoriness fire clay of anti-shrink according to claim 1, it is characterised in that: it is described from
In the preparation step (3) of preparing silicon carbide, the temperature of high-temperature calcination is 800~900 DEG C, and the time of high-temperature calcination is 1~2h.
6. a kind of preparation method of the high refractoriness fire clay of anti-shrink according to claim 1, it is characterised in that: described mixed
In the preparation step for closing fines, the mass ratio of oriental topaz and kyanite is 10:1.
7. a kind of preparation method of the high refractoriness fire clay of anti-shrink according to claim 1, it is characterised in that: the phosphorus
In the preparation step of sour zirconium potassium powder, the molar ratio of potassium carbonate, zirconium oxide and diammonium hydrogen phosphate is 1:4:6.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112028648A (en) * | 2020-08-28 | 2020-12-04 | 江苏苏嘉集团新材料有限公司 | Refractory brick with thermal shrinkage effect and preparation process thereof |
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2019
- 2019-08-05 CN CN201910719391.5A patent/CN110423128A/en not_active Withdrawn
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112028648A (en) * | 2020-08-28 | 2020-12-04 | 江苏苏嘉集团新材料有限公司 | Refractory brick with thermal shrinkage effect and preparation process thereof |
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Application publication date: 20191108 |