CN107540355A - A kind of preparation method of lightweight refracrory - Google Patents
A kind of preparation method of lightweight refracrory Download PDFInfo
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Abstract
The present invention relates to a kind of preparation method of lightweight refracrory, belong to field of material technology.Take polyvinylpyrrolidone, absolute ethyl alcohol, deionized water and styrene to add into three-necked flask, be passed through nitrogen, stir；Divinylbenzene, absolute ethyl alcohol and deionized water are prepared into mixed solution, are added dropwise in three-necked flask, continues to react after being added dropwise, filters, obtains polystyrene microsphere；Bauxite and mica ball milling are taken, obtains ball-milled powder；It will be placed in ball-milled powder and hydrogen peroxide in beaker, filtered after sonic oscillation, obtain modified ball-milled powder；Polystyrene microsphere, ethanol, deionized water and surfactant are poured into beaker and stirred, ball-milled powder and sulfuric acid solution is added, is filtered after stirring, washing it is dry aluminum oxide hollow microsphere；Aluminum oxide hollow microsphere, alumina silicate, dispersant, perlite and deionized water are stirred, obtained stirring slurry is filled into mould, is freeze-dried, is sintered and produce a kind of lightweight refracrory.
Description
Technical field
The present invention relates to a kind of preparation method of lightweight refracrory, belong to field of material technology.
Background technology
Today's society, the energy and environmental problem have been to be concerned by more and more people.Base of the refractory material as hot industry
Plinth material, development energy-saving and environmental protection, the green refractory material of Eco-friendly are also an important side of refractory material future development
To.Lightweight unshape refractory both has good thermal insulation function, can effectively reduce the loss of the energy, while can
To burn till direct use without high temperature, meet the theory of green refractory material.With the development of society and the progress of science and technology, thermal technology
The species of equipment is more and more, also more next more to the requirement of lightweight refracrory, therefore meets the height of Special use environment
The lightweight refracrory of performance is extremely urgent.Refractory material is the important foundation of the hot industries such as steel, cement, ceramics, glass
Material, there is important influence to hot industry production, converted products.Steel industry is the consumption rich and influential family of refractory material, and it is consumed
Amount accounts for more than half of refractory material total amount.Therefore, refractory material is one of important leverage of development of iron ＆ steel industry progress, and
The quality and performance of refractory material produce to steel and are machined with important influence.Now, global refractories industry change
It is huge.With the progress of industrial technology, production technology is increasingly advanced with production equipment, along with refractory quality with
Updating and improving for performance, makes the consumption of refractory material decline year by year.It is continuous with the degree of globalization of world economy
Deepening, the competition between global refractory material enterprise, refractory material enterprise needs to improve constantly research and development of products ability,
So that the species of refractory material is more and more, quality, the performance of the product of resistance to material improve constantly, and are better able to the use for meeting user
It is required that.Refractory material enterprise enables itself to have stronger also in the continuous consciousness and ability strengthened as customer service simultaneously
Competitiveness, occupied a tiny space in keen competition.Under present Circumstances of Market Economy, many scale is smallers, product
The medium-sized and small enterprises that quality is relatively low, lacks competitiveness can gradually be eliminated.Now, global refractory material enterprise gradually realizes enterprise
The optimum combination of industry, the Optimum utilization of market resource can be so more beneficial for, promote the development of refractories industry.In the whole world
It is energy-saving to turn into the problem of hot industry is to be solved under the situation for advocating development " low-carbon economy " energetically.Refractory material conduct
The basic material of hot industry, development energy-saving and environmental protection, the green refractory material of Eco-friendly are extremely important,
It is related to the sustainable development of China's refractories industry at present and in the future.The total yield of China's refractory material and product category are all
It is the first in the world.In recent years, Chinese refractory material is quickly grown, and not only product category is complete, and quality also have it is very big
Improve, China has turned into one of important refractory base in the world.The industrial refractory material such as steel, coloured, chemical industry is main
It is satisfied with domestic demand, some also export many developed countries compared with high grade refractory product.In addition, China or the world are important
Refractory raw material base, occupied an important position in global refractories industry.But compared with developed country's refractory material, I
Be present very big gap in state's refractory material development, be mainly shown as：The average consumption of steel and iron industry refractory material is far above state
There is certain gap in border advanced level, quality and the life-span of refractory material；High-performance, the refractory material of long-life are less, mainly
It is with low content of technology based on primary product, high energy consumption；The waste of resource is very serious, and depletion rate is too fast, causes raw material resources
Missing, the utilization of resources are unreasonable；Environmental pollution and waste reclamation problem.The refractory raw material that does not utilize, using rear fire proofed wood
The stacking of the material desert in air pollution and soil, the also harm of Cr2O3-containing refractories to environment and people's body all caused by meeting
Etc..The recycling rate of waste material caused by production and used refractory is relatively low, serious waste of resources.Therefore, China is resistance to
Fiery materials industry should develop towards energy-conservation, ecological, environmentally friendly and low useless direction." green refractory material " may be summarized to be：Resource,
Energy conservation, kind, superior in qualityization are innoxious using process, production process environmental protection." greenization " development is exactly that collection is more
, the development of all advanced, scientific and rational theory, management and technologies to refractory material is all favourable to kind benefit.Gently
One of the important component of fire resistant materials as refractory material, there is good thermal insulation function, it is possible to reduce thermal technology
The thermal losses of equipment in use, reduces the waste of the energy, while reduces waste gas caused by the burning of the energy, meets green
The theory of color refractory material energy-saving and environmental protection Eco-friendly.
The content of the invention
The technical problems to be solved by the invention：Bad, refractory ability and mechanical property for traditional refractory material uniformity
Can be poor, the problem of high energy consumption, there is provided a kind of preparation method of refractory material.
In order to solve the above technical problems, the technical solution adopted by the present invention is：
（1）10 ~ 20g polyvinylpyrrolidones, 8 ~ 16g absolute ethyl alcohols, 20 ~ 30g deionized waters and 40 ~ 50g styrene is taken to add
Into three-necked flask, temperature is adjusted after being passed through nitrogen, liquid must be stirred after stirring；
（2）In mass ratio 1:1:3, divinylbenzene, absolute ethyl alcohol and deionized water are prepared into mixed solution, are added dropwise to three mouthfuls
In flask, filtered after reaction, obtain polystyrene microsphere；
（3）50 ~ 60g bauxite and 5 ~ 6g mica ball millings are taken, obtains ball-milled powder；
（4）Ball-milled powder and hydrogen peroxide are placed in beaker, filtered after ultrasonic vibration, obtains modified ball-milled powder；
（5）Polystyrene microsphere, 50mL ethanol, 50mL deionized waters and 5mL surfactant are poured into beaker, stirred,
Then addition ball-milled powder and the stirring of 40 ~ 50mL sulfuric acid solutions, filtering, spontaneously dry after being washed repeatedly with deionized water, obtain oxygen
Change aluminium hollow microsphere；
（6）By aluminum oxide hollow microsphere, 10 ~ 20g alumina silicate, 5 ~ 8g dispersants, 15 ~ 20g perlites and 40 ~ 50g deionized waters
It is placed in beaker and stirs, be then filled with into block mold, after being placed in 20 ~ 24h of household freezer freezing, is placed in cold in freeze drier
It is lyophilized dry, obtain solidifying substance；
（7）Solidifying substance is placed in sintering furnace and sintered, produces a kind of lightweight refracrory.
Step（1）The described speed for being passed through nitrogen is 30 ~ 40mL.
Step（2）Described mixed liquor rate of addition 10mL/min.
Step（5）Described sulfuric acid solution is 25%.
Step（6）Described compacting pressure is 30 ~ 40MPa.
Step（7）Described sintering temperature is 600 ~ 800 DEG C.
Compared with other method, advantageous effects are the present invention：
（1）The present invention prepares aluminum oxide hollow microsphere, greatly during lightweight refracrory is prepared by primary raw material of alum clay
Amplitude improves the refractory ability and mechanical strength of material, while can also make the density of material of preparation smaller.
（2）The present invention burns the stirring slurry elder generation cryogenic freezing re-dry of preparation during lightweight refracrory is prepared
Knot, makes that energy consumption can be reduced to a certain extent in this way, while the use of this method can be that the material percent opening prepared increases, drop
Low density of material.
Embodiment
10 ~ 20g polyvinylpyrrolidones, 8 ~ 16g absolute ethyl alcohols, 20 ~ 30g deionized waters and 40 ~ 50g styrene is taken to add
Into the three-necked flask equipped with agitator, thermometer and nitrogen tube, 15 ~ 20min of nitrogen is passed through with 30 ~ 40mL/min speed
Afterwards, by temperature adjustment to 55 ~ 65 DEG C, and 1 ~ 2h is stirred with 120 ~ 150r/min rotating speed, obtains stirring liquid；In mass ratio 1:1:3,
Divinylbenzene, absolute ethyl alcohol and deionized water are prepared into mixed solution, three-necked flask is added dropwise to 10mL/min speed
In, continue 18 ~ 22h of reaction after being added dropwise, filter, obtain polystyrene microsphere；50 ~ 60g bauxite and 5 ~ 6g micas are taken, is put
With 200 ~ 300r/min rotating speed 1 ~ 2h of ball milling in ball grinder, ball-milled powder is obtained；Ball-milled powder is placed in the quality with 500mL
Fraction is to be placed in 20% hydrogen peroxide in beaker, beaker is placed in 180~220W sonic oscillation instrument, after 8 ~ 9h of sonic oscillation
Filtering, obtains modified ball-milled powder；By polystyrene microsphere, 50mL mass fractions be 55% ethanol, 50mL deionized water and
5mL surfactant is poured into beaker, stirs 20 ~ 30min, then adds ball-milled powder and 40 ~ 50mL mass fraction is
25% sulfuric acid solution, filter, be washed with deionized 3 ~ 4 times after stirring 3 ~ 4h with 100 ~ 120r/min rotating speed, it is naturally dry
It is dry, obtain aluminum oxide hollow microsphere；By aluminum oxide hollow microsphere, 10 ~ 20g alumina silicate, 5 ~ 8g dispersants, 15 ~ 20g perlites and 40
~ 50g deionized waters are placed in beaker stirs 20 ~ 30min with 120 ~ 150r/min rotating speed, by obtained stirring slurry 30 ~
Filling is placed in 20 ~ 24h in -10 ~ -5 DEG C of household freezer, is subsequently placed at freeze drier into block mold under 40MPa pressure
In, it is freeze-dried at a temperature of -40 ~ -50 DEG C, obtains solidifying substance；Solidifying substance is placed in sintering furnace, 600 ~ 800 DEG C of sintering 2 ~
3h, produce a kind of lightweight refracrory.Described surfactant is CTAB.Described dispersant is
N, N- ethylene bis stearamide.
Example 1
10g polyvinylpyrrolidones, 8g absolute ethyl alcohols, 20g deionized waters and 40g styrene is taken to add to equipped with agitator, temperature
In degree meter and the three-necked flask of nitrogen tube, after being passed through nitrogen 15min with 30mL/min speed, by temperature adjustment to 55 DEG C, and
1h is stirred with 120r/min rotating speed, obtains stirring liquid；In mass ratio 1:1:3, by divinylbenzene, absolute ethyl alcohol and deionized water
Mixed solution is prepared into, is added dropwise to 10mL/min speed in three-necked flask, continues to react 18h after being added dropwise, filters,
Obtain polystyrene microsphere；50g bauxite and 5g micas are taken, is placed in ball grinder with 200r/min rotating speed ball milling 1h, obtains ball milling
Powder；Ball-milled powder is placed in 500mL mass fractions to be placed in 20% hydrogen peroxide in beaker, beaker is placed in 180W
In sonic oscillation instrument, filtered after sonic oscillation 8h, obtain modified ball-milled powder；It is 55% by polystyrene microsphere, 50mL mass fractions
Ethanol, 50mL deionized water and 5mL CTAB pour into beaker, stir 20min, then add
Ball-milled powder and 40mL mass fraction are 25% sulfuric acid solution, to be filtered after 100r/min rotating speed stirring 3h, use deionization
Water washing 3 times, spontaneously dry, obtain aluminum oxide hollow microsphere；Aluminum oxide hollow microsphere, 10g alumina silicate, 5gN, N- ethylenes is double hard
Acyl amine, 15g perlites and 40g deionized waters are placed in beaker and stir 20min with 120r/min rotating speed, by obtained stirring
Slurry filling under 30MPa pressure into block mold, is placed in 20h in -10 DEG C of household freezer, is subsequently placed at freeze drier
In, it is freeze-dried at a temperature of -40 DEG C, obtains solidifying substance；Solidifying substance is placed in sintering furnace, 600 DEG C of sintering 2h, produces one kind
Lightweight refracrory.
Example 2
15g polyvinylpyrrolidones, 12g absolute ethyl alcohols, 25g deionized waters and 45g styrene is taken to add to equipped with agitator, temperature
In degree meter and the three-necked flask of nitrogen tube, after being passed through nitrogen 17min with 35mL/min speed, by temperature adjustment to 60 DEG C, and
1h is stirred with 135r/min rotating speed, obtains stirring liquid；In mass ratio 1:1:3, by divinylbenzene, absolute ethyl alcohol and deionized water
Mixed solution is prepared into, is added dropwise to 10mL/min speed in three-necked flask, continues to react 20h after being added dropwise, filters,
Obtain polystyrene microsphere；55g bauxite and 5.5g micas are taken, is placed in ball grinder with 250r/min rotating speed ball milling 1.5h, obtains
Ball-milled powder；Ball-milled powder is placed in 500mL mass fractions to be placed in 20% hydrogen peroxide in beaker, beaker is placed in
In 200W sonic oscillation instrument, filtered after sonic oscillation 8h, obtain modified ball-milled powder；By polystyrene microsphere, 50mL mass fractions
CTAB for 55% ethanol, 50mL deionized water and 5mL is poured into beaker, stirs 25min, with
The mass fraction for adding ball-milled powder and 45mL afterwards is 25% sulfuric acid solution, to be filtered after 110r/min rotating speed stirring 3h, is used
Deionized water is washed 3 times, is spontaneously dried, is obtained aluminum oxide hollow microsphere；By aluminum oxide hollow microsphere, 15g alumina silicate, 7gN, N- second
Support bis-stearamides, 17g perlites and 45g deionized waters are placed in beaker stirs 25min with 135r/min rotating speed, will be made
Stirring slurry filled under 35MPa pressure into block mold, be placed in 22h in -7 DEG C of household freezer, it is dry to be subsequently placed at freezing
In dry machine, it is freeze-dried at a temperature of -45 DEG C, obtains solidifying substance；Solidifying substance is placed in sintering furnace, 700 DEG C of sintering 2h, produced
A kind of lightweight refracrory.
Example 3
20g polyvinylpyrrolidones, 16g absolute ethyl alcohols, 30g deionized waters and 50g styrene is taken to add to equipped with agitator, temperature
In degree meter and the three-necked flask of nitrogen tube, after being passed through nitrogen 20min with 40mL/min speed, by temperature adjustment to 65 DEG C, and
2h is stirred with 150r/min rotating speed, obtains stirring liquid；In mass ratio 1:1:3, by divinylbenzene, absolute ethyl alcohol and deionized water
Mixed solution is prepared into, is added dropwise to 10mL/min speed in three-necked flask, continues to react 22h after being added dropwise, filters,
Obtain polystyrene microsphere；60g bauxite and 6g micas are taken, is placed in ball grinder with 200 ~ 300r/min rotating speed ball milling 2h, obtains
Ball-milled powder；Ball-milled powder is placed in 500mL mass fractions to be placed in 20% hydrogen peroxide in beaker, beaker is placed in
In 220W sonic oscillation instrument, filtered after sonic oscillation 9h, obtain modified ball-milled powder；By polystyrene microsphere, 50mL mass fractions
CTAB for 55% ethanol, 50mL deionized water and 5mL is poured into beaker, stirs 30min, with
The mass fraction for adding ball-milled powder and 50mL afterwards is 25% sulfuric acid solution, to be filtered after 120r/min rotating speed stirring 4h, is used
Deionized water is washed 4 times, is spontaneously dried, is obtained aluminum oxide hollow microsphere；By aluminum oxide hollow microsphere, 20g alumina silicate, 8gN, N- second
Support bis-stearamides, 20g perlites and 50g deionized waters are placed in beaker stirs 30min with 150r/min rotating speed, will be made
Stirring slurry filled under 40MPa pressure into block mold, be placed in 24h in -5 DEG C of household freezer, it is dry to be subsequently placed at freezing
In dry machine, it is freeze-dried at a temperature of -50 DEG C, obtains solidifying substance；Solidifying substance is placed in sintering furnace, 800 DEG C of sintering 3h, i.e.,
Obtain a kind of lightweight refracrory.
A kind of lightweight refracrory being prepared into and Zichuan District of Zibo City Xinghua refractory material are detected, specific detection
It is as follows：
（1）The measure of surface elasticity
It is disposed vertically with diameter=1.5mm mould draw point and withstands pin bottom down, with thumb in the surface of sample, needle point
Portion, pressed down with natural force, go out to insert the depth of sample with vernier caliper measurement, according to depth come the table of intuitive judgment sample
Surface elastic is good and bad.
（2）The measure of apparent density
Sample after the demoulding is put in 120 DEG C of baking oven, dried to constant weight, it is standby to be cooled to room temperature.Take three pieces of test specimens point of preparation
Do not polish and claim quality, be accurate to lg.Distinguished in order with Steel Ruler in test specimen two ends away from the mm of side 20 and centre position
Its length and width is measured, is accurate to lm m, takes the average value of 3 measurement data.With slide measure on any one side of test specimen
Both ends measure thickness respectively far from the mm of edge 20 and centre position, are measured more than relative another side repetition, are accurate to 0.
lmm.The average value of 6 measurement data is taken, so as to try to achieve the quality of each test specimen and volume.Dry density is calculated as follows：
ρ=m /v
In formula：
ρ --- dry density/g/cm3, m --- test specimen quality/g, v --- test specimen volume/cm3。
Calculate the arithmetic mean of instantaneous value of three test specimen dry densities, specific test result such as table 1.
The lightweight refracrory performance characterization of table 1
As shown in Table 1, the lightweight refracrory that prepared by the present invention significantly improves the refractory ability and mechanical strength of material, together
When density of material it is smaller.During lightweight refracrory is prepared, the stirring slurry elder generation cryogenic freezing re-dry of preparation is sintered,
Make that energy consumption can be reduced to a certain extent in this way, while the use of this method can be that the material percent opening prepared increases, reduce
Density of material.
Claims (6)
1. a kind of preparation method of lightweight refracrory, its feature are being with specific preparation process：
10 ~ 20g polyvinylpyrrolidones, 8 ~ 16g absolute ethyl alcohols, 20 ~ 30g deionized waters and 40 ~ 50g styrene is taken to add to three
In mouth flask, temperature is adjusted after being passed through nitrogen, liquid must be stirred after stirring；
In mass ratio 1:1:3, divinylbenzene, absolute ethyl alcohol and deionized water are prepared into mixed solution, are added dropwise to three mouthfuls of burnings
In bottle, filtered after reaction, obtain polystyrene microsphere；
50 ~ 60g bauxite and 5 ~ 6g mica ball millings are taken, obtains ball-milled powder；
Ball-milled powder and hydrogen peroxide are placed in beaker, filtered after ultrasonic vibration, obtains modified ball-milled powder；
Polystyrene microsphere, 50mL ethanol, 50mL deionized waters and 5mL surfactant are poured into beaker, stirred, then
Ball-milled powder and the stirring of 40 ~ 50mL sulfuric acid solutions are added, filtering, is spontaneously dried after being washed repeatedly with deionized water, obtains aluminum oxide
Hollow microsphere；
Aluminum oxide hollow microsphere, 10 ~ 20g alumina silicate, 5 ~ 8g dispersants, 15 ~ 20g perlites and 40 ~ 50g deionized waters are placed in
Stir, be then filled with into block mold in beaker, after being placed in 20 ~ 24h of household freezer freezing, be placed in freeze in freeze drier and do
It is dry, obtain solidifying substance；
Solidifying substance is placed in sintering furnace and sintered, produces a kind of lightweight refracrory.
A kind of 2. preparation method of lightweight refracrory according to claim 1, it is characterised in that：Step（1）Described
The speed for being passed through nitrogen is 30 ~ 40mL.
A kind of 3. preparation method of lightweight refracrory according to claim 1, it is characterised in that：Step（2）Described
Mixed liquor rate of addition 10mL/min.
A kind of 4. preparation method of lightweight refracrory according to claim 1, it is characterised in that：Step（5）Described
Sulfuric acid solution is 25%.
A kind of 5. preparation method of lightweight refracrory according to claim 1, it is characterised in that：Step（6）Described
Compacting pressure is 30 ~ 40MPa.
A kind of 6. preparation method of lightweight refracrory according to claim 1, it is characterised in that：Step（7）Described
Sintering temperature is 600 ~ 800 DEG C.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1370136A (en) * | 1999-06-07 | 2002-09-18 | 联合矿物产品公司 | Lightweight dry refractory |
| CN1886350A (en) * | 2003-11-28 | 2006-12-27 | 新型材料莱布尼兹研究所公益性有限责任公司 | Insulation material |
| CN102811973A (en) * | 2010-07-13 | 2012-12-05 | 三井金属矿业株式会社 | Heat insulating refractory and method for producing same |
| CN107021776A (en) * | 2016-01-29 | 2017-08-08 | 阔斯泰公司 | Unsetting refractory body particle |
-
2017
- 2017-09-16 CN CN201710835812.1A patent/CN107540355B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1370136A (en) * | 1999-06-07 | 2002-09-18 | 联合矿物产品公司 | Lightweight dry refractory |
| CN1886350A (en) * | 2003-11-28 | 2006-12-27 | 新型材料莱布尼兹研究所公益性有限责任公司 | Insulation material |
| CN102811973A (en) * | 2010-07-13 | 2012-12-05 | 三井金属矿业株式会社 | Heat insulating refractory and method for producing same |
| CN107021776A (en) * | 2016-01-29 | 2017-08-08 | 阔斯泰公司 | Unsetting refractory body particle |
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