CN107235738A - A kind of preparation method of fiber reinforced refractory material - Google Patents

A kind of preparation method of fiber reinforced refractory material Download PDF

Info

Publication number
CN107235738A
CN107235738A CN201710526853.2A CN201710526853A CN107235738A CN 107235738 A CN107235738 A CN 107235738A CN 201710526853 A CN201710526853 A CN 201710526853A CN 107235738 A CN107235738 A CN 107235738A
Authority
CN
China
Prior art keywords
refractory material
fiber reinforced
dry
preparation
reinforced refractory
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710526853.2A
Other languages
Chinese (zh)
Inventor
佘建锋
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Changxing Hongkuang Furnace Burden Co Ltd
Original Assignee
Changxing Hongkuang Furnace Burden Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Changxing Hongkuang Furnace Burden Co Ltd filed Critical Changxing Hongkuang Furnace Burden Co Ltd
Priority to CN201710526853.2A priority Critical patent/CN107235738A/en
Publication of CN107235738A publication Critical patent/CN107235738A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/66Monolithic refractories or refractory mortars, including those whether or not containing clay
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3206Magnesium oxides or oxide-forming salts thereof
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/3205Alkaline earth oxides or oxide forming salts thereof, e.g. beryllium oxide
    • C04B2235/3208Calcium oxide or oxide-forming salts thereof, e.g. lime
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/48Organic compounds becoming part of a ceramic after heat treatment, e.g. carbonising phenol resins
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/02Composition of constituents of the starting material or of secondary phases of the final product
    • C04B2235/50Constituents or additives of the starting mixture chosen for their shape or used because of their shape or their physical appearance
    • C04B2235/52Constituents or additives characterised by their shapes
    • C04B2235/5208Fibers
    • C04B2235/5216Inorganic
    • C04B2235/524Non-oxidic, e.g. borides, carbides, silicides or nitrides
    • C04B2235/5248Carbon, e.g. graphite
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2235/00Aspects relating to ceramic starting mixtures or sintered ceramic products
    • C04B2235/70Aspects relating to sintered or melt-casted ceramic products
    • C04B2235/96Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance

Landscapes

  • Engineering & Computer Science (AREA)
  • Chemical & Material Sciences (AREA)
  • Ceramic Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Materials Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Oxide Ceramics (AREA)

Abstract

The invention belongs to technical field of refractory materials.The invention discloses a kind of preparation method of fiber reinforced refractory material, it includes getting the raw materials ready, batch mixing, preliminary granulation, the again step such as granulation, toughening modifying, dry-pressing formed and sintering.Prepared in the present invention during fiber reinforced refractory material, obtained green compact have preferable mechanical performance, the problems such as being not susceptible to broken, yields is higher, ensure that the efficient progress of refractory material preparation process;Fiber reinforced refractory material has higher fracture toughness obtained by being made, and the service life of refractory material is ensure that, while also can guarantee that the use reliability of refractory material.

Description

A kind of preparation method of fiber reinforced refractory material
Technical field
The present invention relates to technical field of refractory materials, more particularly, to a kind of preparation method of fiber reinforced refractory material.
Background technology
In traditional sense, refractory material refers to that refractoriness is not less than 1580 DEG C of inorganic non-metallic material, and it is for height The basic material of temperature technique service, is used as the structural material of the Thermal Equipments such as high temperature kiln, and industrial high temperature container and portion The material of part, and corresponding physicochemical change and mechanism can be born.
Most of refractory material is with natural crystal(Such as fire clay, silica, magnesite, dolomite)Manufactured for raw material , using some raw materials of industry and artificial-synthetic material(Such as commercial alumina, carborundum, mullite synthesizing, synthetic spinel Deng)Also increasing, therefore, the species of refractory material is a lot.Refractory material can be divided into the siliceous, silicon of oxidation according to mineral composition Sour aluminum, magnesia, dolomite matter, olivine matter, spinel, containing carbonaceous, containing zirconia refractory and special refractory;Press It can be divided into natural crystal and artifact according to manufacture method;It can be divided into block elements and unshape refractory by its mode; It can be divided into not burned product, burnt product and melt-cast products according to heat treatment mode;It can be divided into common, senior and spy according to refractoriness Level refractory product;It can be divided into acid, neutral and basic refractory according to chemical property;It can be divided into lightweight and again according to its density Fire resistant materials;Shape and size according to its product can be divided into standard brick, special shaped brick, special special shaped brick, pipe and flame ware;Also Blast furnace use, cement kiln use, glass furnace use, ceramic kiln refractory etc. can be divided into by its application.
It is a problem of generally existing in inorganic non-metallic and material that the mechanical tenacity of inorganic non-metallic material is poor, is made To belong to the refractory material of inorganic non-metallic material together, its mechanical tenacity is also poor, although refractory material is almost in use It need not move, but thermal shock resistance of its poor mechanical tenacity when also having had influence on its high temperature, it is anxious in chilling Heat and the gap used are resistance to because the influences such as cracking, peeling easily occur under the effect of expanding with heat and contract with cold for larger temperature difference refractory material The situation of fiery material integrity, reduces the service life of refractory material;Simultaneously for those need often to move it is resistance to Fiery material product, its poor mechanical tenacity can then greatly increase the spoilage of refractory product, influence its routine use.
The content of the invention
To solve the above problems, the invention provides a kind of preparation method of fiber reinforced refractory material, passing through this method The raw material for refractory compatibility being prepared is reasonable, and can be before the performance such as higher fire resistance and more excellent fracture toughness is realized Put and minimize cost.
To achieve the above object, the technical solution adopted by the present invention is as follows:
A kind of preparation method of fiber reinforced refractory material, comprises the following steps:
a)Get the raw materials ready:Prepare raw material by following parts by weight:40 parts of magnesia, 90~100 parts of calcium oxide, 6~7 parts of toughened fiber is made 1~3 part of binding agent of grain, 0.5~1.5 part of molding adhesive;
b)Batch mixing:Magnesia and calcium oxide ball milling is dry-mixed well mixed;
c)Preliminary granulation:Sprayed water into magnesia and oxidation calcium compound, while simultaneously continuous vibrating prilling;
d)Granulate again:Add adhesive for granulating into the mixture after preliminary granulation, and dry-mixed 20~30 minutes of ball milling;
e)Toughening modifying:Toughened fiber is added in the mixture after granulating again, and dry-mixed 10~20 minutes of ball milling, do Fiber reinforced refractory material powder is made after dry;
f)It is dry-pressing formed:Molding adhesive simultaneously dry-mixed 15~30 minutes of ball milling are added into fiber reinforced refractory material powder, so It is dry-pressing formed under 10~25Mpa pressure afterwards, refractory material green compact are made;
g)Sintering:Refractory material green compact after shaping are sintered 4~8 hours at 1700~1800 DEG C, natural cooling acquisition afterwards Fiber reinforced refractory material.
In refractory material, dolomite series refractory material is the important refractory material of a class.Magnesia and calcium oxide are one Certainty ratio mixes and can obtain the refractory material of dolomite matter after sintered, when magnesia and calcium oxide mol ratio are 0.25: 0.75 or so is that can generate most dolomite phases, with best fire resistance, in magnesia and two kinds of components of calcium oxide, The cost of calcium oxide is more cheap, and more calcium oxide are added in appropriate scope to minimize cost, but oxygen The reduction that the dolomite of the stabilization generated after the too high levels for changing calcium is met drastically, the refractoriness of obtained refractory material also can Decline to a great extent accordingly, therefore the mol ratio of magnesia and calcium oxide is positioned 0.3:0.7 or so, and carry out according to actual needs Corresponding adjustment, can so realize can reduce cost as far as possible, also can guarantee that refractoriness within tolerance interval.
The method that secondary granulation is used in the present invention, for the first time granulation is the granulation for raw material calcium oxide and magnesia, Using the granulation mode of water spray, in order to allow calcium oxide and magnesia to be well mixed and big of certain particle diameter can be formed Grain, the order of magnitude of the particle diameter of the bulky grain formed after granulation at 0.01 millimeter, so beneficial to follow-up technique, while after being also beneficial to Toughener can be preferably distributed in the gap of magnesia calcium oxide powder in continuous step;Second of granulation is using first first time The mode for granulating addition binding agent in obtained powder is granulated, and is the other grain granulation shape of 0.01 grade by original particle diameter Into the powder particles that particle diameter is 0.1 millimeter of quantity, and it is that next step toughener can be stablized uniformly to superscribe binding agent in powder The surface for being attached to particle;In the present invention, first secondary granulation adds toughener rather than added at the very start thereto again to be increased Tough dose of purpose is the integrated distribution for making toughener form small range in powder;Because the addition of toughener is seldom, if Toughener is equally distributed in powder, is produced in refractory material obtained by firing behind crack, toughener is difficult to prevent more at least The extension in crack, by the method in the present invention, the concentration for making toughener relative in small range is to have when crack is spread to Enough abilities prevent spreading for crack, it is ensured that the fracture toughness of refractory material.
Preferably, toughened fiber is hollow acetate fibre, its length is 5~15 microns.
Acetate fiber is that one kind is raw material by cellulose, and the chemistry fibre that acetyl cellulose is made is changed into method through chemistry Dimension, with higher carbon content, results in excellent carbon fiber after reducing atmosphere pyroreaction;In the system of acetate fiber 0.5wt% titanium dioxide is often added as delustering agent during standby.Therefore, acetate fiber has following two features, 1. With higher carbon content, it can generate and contain in excellent carbon fiber, 2. acetate fibers after reducing atmosphere pyroreaction There is 0.5wt% titanium dioxide, after reducing atmosphere high-temperature calcination, titanium dioxide can be enriched with the specific limits, and be given birth to Long, the acetate fiber most crossed afterwards through reducing atmosphere high-temperature process, which can become a kind of surface, has small titanium dioxide branch fork Carbon fiber, although these titanium dioxide branch fork is shorter for the diameter of carbon fiber, but it also increases carbon fiber Surface area, adds the binding ability between carbon fiber and refractory material powder.Hollow acetate fiber is passing through reproducibility gas After atmosphere high-temperature process, a kind of carbon fiber pipe with hollow pipeline structure can be formed accordingly, its inwall and outer surface also can phases The generation titanium dioxide branch fork answered, improves the specific surface area of hollow carbon fiber, and also greatly increase hollow carbon fiber is resistance to other Binding ability between fiery material powder, in refractory material sintering process, can reduce the sintering difficulty of refractory material, simultaneously As a kind of fiber, thought with corresponding toughness reinforcing, and can also increase the fracture toughness of refractory material.
It it is 5~15 microns from length, the shorter acetate fiber of length can preferably combine refractory material powder Together, draw ratio can be being generated after pyroreaction small carbon fiber, the hollow carbon pitched with titanium dioxide branch of generation Fibre pipe, is evenly distributed in refractory material, refractory material can closely link together, be used in refractory material Occur crackle in journey, the propagation of crackle can be also blocked in time, it is ensured that refractory material will not be broken.
Preferably, adhesive for granulating is 5wt% Kynoar 1-METHYLPYRROLIDONE solution, described shaping is bonded Agent is 5wt% polyvinylpyrrolidone ethanol solutions.
Kynoar 1-METHYLPYRROLIDONE solution refers to that Kynoar is dissolved in what is obtained in 1-METHYLPYRROLIDONE Solution, polyvinylpyrrolidone ethanol solution refers to being dissolved in polyvinylpyrrolidone into the solution obtained in ethanol.
In the prior art, binding agent typically uses polyvinyl alcohol(PVA)The aqueous solution, but polyvinyl alcohol be one kind intolerant to height The organic high molecular compound of temperature, its fusing point is relatively low, and decomposition temperature is relatively low, is added to as binding agent in powder, in sintering Stage needs to carry out dumping processing at a lower temperature, at a lower temperature dumping, easily causes after binding agent decomposition Holdup time process of the product in powder, or even long period lasting impact is produced to powder, cause obtained fire proofed wood Expect the decline of mechanical property;Kynoar is a kind of organic high molecular compound with high-temperature stability, compared to poly- second Enol, there is relatively higher fusing point, relatively higher decomposition temperature, therefore the temperature of powder dumping can also rise accordingly for it Height, after dump temperature rise, catabolite also can be discharged quickly from powder, reduced the time for being detained powder, reduced to system Obtain the influence of refractory material mechanical property.
Adhesive for granulating in the present invention is being entirely located in inside particle after preparation, it is difficult to realized between preferable particle Bond, need adding molding adhesive for this, due to need to only play the cementation between particle, consumption need not be too many, adds Plus 0.1wt% or so can be achieved intergranular cementation, and can meet will for conventional polyvinylpyrrolidonesolution solution Ask.
Preferably, in step c, the amount of water spray is aluminum oxide and 2~5wt% of magnesia gross weight, and water spray process is 10 Uniform completion in~12 minutes.
In prilling of spraying water, the purpose of water spray be in order to allow powder surface wetting, then with certain adhesive property, Therefore the speed of water spray is slow, uniform.
Preferably, in the temperature-rise period of step g sintering, being first warming up to by room temperature with 1~3 DEG C/min heating rate 900~1000 DEG C and be incubated 1~2 hour, 1500~1600 DEG C of progress are warming up to 3~5 DEG C/min heating rate again afterwards Sintering.
Whole refractory material sintering process is mainly two steps, and the first step is dumping, will prepare and adds during powder and green compact Plus organic binder bond decompose and exclude in ejection body, the heating rate in dumping stage is unsuitable too fast, and heating too quickly is easily made Decompose too fast into binding agent, produce the too fast damage base substrate of gas;Second stage is sintering stage, and this stage is viscous due to not having Tie agent and decompose the problem of producing gas, therefore heating rate can also so accelerate efficiency with slightly faster;Although of the invention In whole sintering stage carried out under reducing atmosphere, be narrowly that the dumping stage is not present, but sintered Still there can be binding agent in journey and occur the process that decomposed becomes carbon particle, therefore there is also deposited during the reaction of such as dumping in fact Gas generation process, although the gas of generation is less, but also to control heating rate reduce aerogenesis rate guarantee base substrate not The gas that can be generated is damaged.
Preferably, whole step g is carried out under nitrogen reducing environment, sintering end is cooled to room temperature recession and removes nitrogen.
In order to allow carbon fiber of the hollow acetate fibre formation with special construction, it is necessary to be carried out under reducing atmosphere, nitrogen Compression ring border is best reducing atmosphere, while the quality in order to ensure refractory material, need to cool to after room temperature and remove reduction Property environment.
Therefore, the invention has the advantages that:
(1)Prepared in the present invention during fiber reinforced refractory material, obtained green compact have preferable mechanical performance, be difficult hair Raw broken the problems such as, yields is higher, ensure that the efficient progress of refractory material preparation process;
(2)Fiber reinforced refractory material obtained by the present invention is obtained has higher fracture toughness, ensure that refractory material Service life, while also can guarantee that the use reliability of refractory material.
Embodiment
Technical scheme is further described with reference to embodiment.
Obviously, described embodiment is only a part of embodiment of the present invention, rather than whole embodiments.Based on this Embodiment in invention, all other reality that those of ordinary skill in the art are obtained under the premise of creative work is not made Example is applied, the scope of protection of the invention is belonged to.
Embodiment 1
A kind of preparation method of fiber reinforced refractory material, comprises the following steps:
a)Get the raw materials ready:Prepare raw material by following parts by weight:40 parts of magnesia, 90 parts of calcium oxide, 6 parts of toughened fiber, adhesive for granulating 1 Part, 0.5 part of molding adhesive;Toughened fiber is hollow acetate fibre, and its length is 5 microns, and adhesive for granulating is 5wt% poly- inclined PVF 1-METHYLPYRROLIDONE solution, described molding adhesive is 5wt% polyvinylpyrrolidone ethanol solutions;
b)Batch mixing:Magnesia and calcium oxide ball milling is dry-mixed well mixed;
c)Preliminary granulation:Sprayed water into magnesia and oxidation calcium compound, while simultaneously continuous vibrating prilling;The amount of water spray is oxidation The 2wt% of aluminium and magnesia gross weight, water spray process is uniform at 10 minutes to be completed;
d)Granulate again:Add adhesive for granulating into the mixture after preliminary granulation, and dry-mixed 20 minutes of ball milling;
e)Toughening modifying:Toughened fiber is added in the mixture after granulating again, and dry-mixed 10 minutes of ball milling, after drying Fiber reinforced refractory material powder is made;
f)It is dry-pressing formed:Molding adhesive simultaneously dry-mixed 15 minutes of ball milling, Ran Hou are added into fiber reinforced refractory material powder It is dry-pressing formed under 10Mpa pressure, refractory material green compact are made;
g)Sintering:Refractory material green compact after shaping are sintered 4 hours at 1700 DEG C, natural cooling acquisition afterwards is fiber reinforced resistance to Fiery material;In the temperature-rise period of sintering, first it is warming up to 900 DEG C with 1 DEG C/min heating rate by room temperature and is incubated 1 hour, it 1500 DEG C are warming up to again with 3 DEG C/min heating rate afterwards to be sintered;Whole sintering step is carried out under nitrogen reducing environment, Sintering end is cooled to room temperature recession and removes nitrogen.
Embodiment 2
A kind of preparation method of fiber reinforced refractory material, comprises the following steps:
a)Get the raw materials ready:Prepare raw material by following parts by weight:40 parts of magnesia, 95 parts of calcium oxide, 6.5 parts of toughened fiber, granulation is bonded 2 parts of agent, 1.0 parts of molding adhesive;Toughened fiber is hollow acetate fibre, and its length is 10 microns, and adhesive for granulating is 5wt% Kynoar 1-METHYLPYRROLIDONE solution, described molding adhesive is 5wt% polyvinylpyrrolidone ethanol solutions;
b)Batch mixing:Magnesia and calcium oxide ball milling is dry-mixed well mixed;
c)Preliminary granulation:Sprayed water into magnesia and oxidation calcium compound, while simultaneously continuous vibrating prilling;The amount of water spray is oxidation The 3.5wt% of aluminium and magnesia gross weight, water spray process is uniform at 11 minutes to be completed;
d)Granulate again:Add adhesive for granulating into the mixture after preliminary granulation, and dry-mixed 25 minutes of ball milling;
e)Toughening modifying:Toughened fiber is added in the mixture after granulating again, and dry-mixed 15 minutes of ball milling, after drying Fiber reinforced refractory material powder is made;
f)It is dry-pressing formed:Molding adhesive simultaneously dry-mixed 25 minutes of ball milling, Ran Hou are added into fiber reinforced refractory material powder It is dry-pressing formed under 15Mpa pressure, refractory material green compact are made;
g)Sintering:Refractory material green compact after shaping are sintered 6 hours at 1750 DEG C, natural cooling acquisition afterwards is fiber reinforced resistance to Fiery material;In the temperature-rise period of sintering, first it is warming up to 950 DEG C with 2 DEG C/min heating rate by room temperature and is incubated 1.5 hours, 1550 DEG C are warming up to again with 4 DEG C/min heating rate afterwards to be sintered;Whole sintering step enters under nitrogen reducing environment OK, sintering end is cooled to room temperature recession and removes nitrogen.
Embodiment 3
A kind of preparation method of fiber reinforced refractory material, comprises the following steps:
a)Get the raw materials ready:Prepare raw material by following parts by weight:40 parts of magnesia, 100 parts of calcium oxide, 7 parts of toughened fiber, adhesive for granulating 3 parts, 1.5 parts of molding adhesive;Toughened fiber is hollow acetate fibre, and its length is 15 microns, and adhesive for granulating is poly- for 5wt% Vinylidene 1-METHYLPYRROLIDONE solution, described molding adhesive is 5wt% polyvinylpyrrolidone ethanol solutions;
b)Batch mixing:Magnesia and calcium oxide ball milling is dry-mixed well mixed;
c)Preliminary granulation:Sprayed water into magnesia and oxidation calcium compound, while simultaneously continuous vibrating prilling;The amount of water spray is oxidation The 5wt% of aluminium and magnesia gross weight, water spray process is uniform at 12 minutes to be completed;
d)Granulate again:Add adhesive for granulating into the mixture after preliminary granulation, and dry-mixed 30 minutes of ball milling;
e)Toughening modifying:Toughened fiber is added in the mixture after granulating again, and dry-mixed 20 minutes of ball milling, after drying Fiber reinforced refractory material powder is made;
f)It is dry-pressing formed:Molding adhesive simultaneously dry-mixed 30 minutes of ball milling, Ran Hou are added into fiber reinforced refractory material powder It is dry-pressing formed under 25Mpa pressure, refractory material green compact are made;
g)Sintering:Refractory material green compact after shaping are sintered 8 hours at 1800 DEG C, natural cooling acquisition afterwards is fiber reinforced resistance to Fiery material;In the temperature-rise period of sintering, first it is warming up to 1000 DEG C with 3 DEG C/min heating rate by room temperature and insulation 1~2 is small When, it is warming up to 1600 DEG C with 3~5 DEG C/min heating rate again afterwards and is sintered;Whole sintering step reduces ring in nitrogen Carried out under border, sintering end is cooled to room temperature recession and removes nitrogen.
Measure of merit:
Fiber reinforced refractory material in above-described embodiment is subjected to correlated performance test;
Refractoriness test is carried out using the GB/T 7322-2007 methods recorded, and apparent porosity is recorded using GB/T 5071-2013 Method carry out, cold crushing strength is carried out using the GB/T 5072-2008 methods recorded, and refractoriness under load uses GB/T The method that 5989-2008 is recorded is carried out, and fracture toughness is tested using SENB methods well known in the art.
Test effect:
1. refractoriness >=1960 DEG C, maximum temperature in use >=1900 DEG C;
2. apparent porosity≤4%;
3. cold crushing strength >=125MPa;
4. refractoriness under load >=1920 DEG C;
5. fracture toughness >=2.0MPam1/2
It should be appreciated that to those skilled in the art, can according to the above description be improved or be become Change, and all these modifications and variations should all belong to the protection domain of appended claims of the present invention.

Claims (6)

1. a kind of preparation method of fiber reinforced refractory material, it is characterised in that comprise the following steps:
a)Get the raw materials ready:Prepare raw material by following parts by weight:40 parts of magnesia, 90~100 parts of calcium oxide, 6~7 parts of toughened fiber is made 1~3 part of binding agent of grain, 0.5~1.5 part of molding adhesive;
b)Batch mixing:Magnesia and calcium oxide ball milling is dry-mixed well mixed;
c)Preliminary granulation:Sprayed water into magnesia and oxidation calcium compound, while simultaneously continuous vibrating prilling;
d)Granulate again:Add adhesive for granulating into the mixture after preliminary granulation, and dry-mixed 20~30 minutes of ball milling;
e)Toughening modifying:Toughened fiber is added in the mixture after granulating again, and dry-mixed 10~20 minutes of ball milling, do Fiber reinforced refractory material powder is made after dry;
f)It is dry-pressing formed:Molding adhesive simultaneously dry-mixed 15~30 minutes of ball milling are added into fiber reinforced refractory material powder, so It is dry-pressing formed under 10~25Mpa pressure afterwards, refractory material green compact are made;
g)Sintering:Refractory material green compact after shaping are sintered 4~8 hours at 1700~1800 DEG C, natural cooling acquisition afterwards Fiber reinforced refractory material.
2. a kind of preparation method of fiber reinforced refractory material according to claim 1, it is characterised in that:
Described toughened fiber is hollow acetate fibre, and its length is 5~15 microns.
3. a kind of preparation method of fiber reinforced refractory material according to claim 1, it is characterised in that:
Described adhesive for granulating is 5wt% Kynoar 1-METHYLPYRROLIDONE solution, and described molding adhesive is 5wt% Polyvinylpyrrolidone ethanol solution.
4. a kind of preparation method of fiber reinforced refractory material according to claim 1, it is characterised in that:
In described step c, the amount of water spray is aluminum oxide and 2~5wt% of magnesia gross weight, and water spray process is at 10~12 points Clock is uniformly completed.
5. a kind of preparation method of fiber reinforced refractory material according to claim 1, it is characterised in that:
In the temperature-rise period of the step g sintering, first 900~1000 DEG C are warming up to by room temperature with 1~3 DEG C/min heating rate And 1~2 hour is incubated, it is warming up to 1500~1600 DEG C with 3~5 DEG C/min heating rate again afterwards and is sintered.
6. a kind of preparation method of fiber reinforced refractory material according to claim 1 or 5, it is characterised in that:
The whole step g is carried out under nitrogen reducing environment, and sintering end is cooled to room temperature recession and removes nitrogen.
CN201710526853.2A 2017-06-30 2017-06-30 A kind of preparation method of fiber reinforced refractory material Pending CN107235738A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710526853.2A CN107235738A (en) 2017-06-30 2017-06-30 A kind of preparation method of fiber reinforced refractory material

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710526853.2A CN107235738A (en) 2017-06-30 2017-06-30 A kind of preparation method of fiber reinforced refractory material

Publications (1)

Publication Number Publication Date
CN107235738A true CN107235738A (en) 2017-10-10

Family

ID=59991673

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710526853.2A Pending CN107235738A (en) 2017-06-30 2017-06-30 A kind of preparation method of fiber reinforced refractory material

Country Status (1)

Country Link
CN (1) CN107235738A (en)

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108715545A (en) * 2018-06-21 2018-10-30 华北理工大学 A kind of continuous casting tundish dry material and preparation method thereof
CN108894455A (en) * 2018-08-02 2018-11-27 北京启顺京腾科技有限责任公司 A kind of production method of new and improved decorative panel
CN109987956A (en) * 2019-04-15 2019-07-09 宋志成 A kind of refractory material enhancing toughness
CN110668833A (en) * 2019-10-28 2020-01-10 刘晓慧 Preparation method of magnesium-calcium-carbon composite material
CN112321310A (en) * 2020-11-04 2021-02-05 黑龙江冠瓷科技有限公司 Preparation method of nanoparticle toughened high-toughness SiC product
CN116063087A (en) * 2023-01-09 2023-05-05 宜兴市金其节能科技有限公司 Lining compact material for plasma furnace and preparation method thereof

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101269980A (en) * 2007-12-14 2008-09-24 内蒙古科技大学 Generating method for crassitude carbon nano-tube and carbon nano-fibre in carbon composite refractory material
CN104725031A (en) * 2015-03-16 2015-06-24 上海交通大学 Method for growing carbon nano fibers on ceramic hollow microsphere surface in situ
CN105130457A (en) * 2015-07-09 2015-12-09 长兴泓矿炉料有限公司 Magnesium-calcium-carbon refractory material and preparation method thereof
CN106587938A (en) * 2016-11-14 2017-04-26 江苏科技大学 Spinel powder with high temperature conductivity and synthesis method and application thereof
CN106587937A (en) * 2016-12-07 2017-04-26 苏州洛特兰新材料科技有限公司 High-strength carbon fiber based composite ceramic material and preparation method thereof

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101269980A (en) * 2007-12-14 2008-09-24 内蒙古科技大学 Generating method for crassitude carbon nano-tube and carbon nano-fibre in carbon composite refractory material
CN104725031A (en) * 2015-03-16 2015-06-24 上海交通大学 Method for growing carbon nano fibers on ceramic hollow microsphere surface in situ
CN105130457A (en) * 2015-07-09 2015-12-09 长兴泓矿炉料有限公司 Magnesium-calcium-carbon refractory material and preparation method thereof
CN106587938A (en) * 2016-11-14 2017-04-26 江苏科技大学 Spinel powder with high temperature conductivity and synthesis method and application thereof
CN106587937A (en) * 2016-12-07 2017-04-26 苏州洛特兰新材料科技有限公司 High-strength carbon fiber based composite ceramic material and preparation method thereof

Cited By (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108715545A (en) * 2018-06-21 2018-10-30 华北理工大学 A kind of continuous casting tundish dry material and preparation method thereof
CN108894455A (en) * 2018-08-02 2018-11-27 北京启顺京腾科技有限责任公司 A kind of production method of new and improved decorative panel
CN109987956A (en) * 2019-04-15 2019-07-09 宋志成 A kind of refractory material enhancing toughness
CN110668833A (en) * 2019-10-28 2020-01-10 刘晓慧 Preparation method of magnesium-calcium-carbon composite material
CN112321310A (en) * 2020-11-04 2021-02-05 黑龙江冠瓷科技有限公司 Preparation method of nanoparticle toughened high-toughness SiC product
CN116063087A (en) * 2023-01-09 2023-05-05 宜兴市金其节能科技有限公司 Lining compact material for plasma furnace and preparation method thereof
CN116063087B (en) * 2023-01-09 2023-10-24 宜兴市金其节能科技有限公司 Lining compact material for plasma furnace and preparation method thereof

Similar Documents

Publication Publication Date Title
CN107235738A (en) A kind of preparation method of fiber reinforced refractory material
CN106278321B (en) A kind of high tenacity refractory material and its preparation process
CN108424016B (en) High-performance lightweight aggregate for structural engineering
CN106336200B (en) A kind of inorfil toughening refractory material and its preparation process
CN109020449B (en) A kind of jet printing type ardealite base fireproof mortar and its preparation method and application of stalk fibre enhancing
CN108069708A (en) A kind of high thermal shock long-life saggar and preparation method
CN106336227B (en) A kind of mineral products waste refractory material and its preparation process
CN106431434A (en) Closed-pore bauxite based mullite material and preparing method thereof
CN110204323A (en) A kind of energy-saving cordierite zircon composite diphase material and preparation method thereof
CN106431435A (en) Porous periclase-forsterite multiphase material and preparation method thereof
CN111943642A (en) High-strength foamed ceramic and preparation method thereof
CN107337459A (en) A kind of fiber reinforced refractory material raw powder's production technology
CN106336228B (en) A kind of composite fibre toughening refractory material and its preparation process
CN107382337A (en) A kind of preparation method of high tenacity refractory material
CN110002859B (en) Corrosion-resistant ceramic roller and preparation method thereof
CN102659448B (en) Zirconia special foam ceramic filter and preparation method thereof
CN107235740A (en) A kind of fiber reinforced refractory material
CN107311631A (en) A kind of raw powder's production technology for being used to prepare high tenacity refractory material
CN110452009A (en) A kind of preparation method of in-situ preparation magnesium aluminate spinel whisker skeletal porous ceramics
CN109987956A (en) A kind of refractory material enhancing toughness
CN106316426B (en) A kind of Resisting fractre refractory material and its preparation process
CN108675808A (en) A kind of infant industry kiln refractory material and preparation method thereof
CN109369203A (en) Density mullite brick and preparation method thereof in high intensity
CN108530093A (en) A kind of high strength refractory material and preparation method thereof
CN108285350A (en) A kind of tri compound SiC based refractories and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20171010