CN104230170B - A kind of preparation method of sintering process foaming micro crystal material product - Google Patents
A kind of preparation method of sintering process foaming micro crystal material product Download PDFInfo
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- CN104230170B CN104230170B CN201310349128.4A CN201310349128A CN104230170B CN 104230170 B CN104230170 B CN 104230170B CN 201310349128 A CN201310349128 A CN 201310349128A CN 104230170 B CN104230170 B CN 104230170B
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- 238000005187 foaming Methods 0.000 title claims abstract description 32
- 239000000463 material Substances 0.000 title claims abstract description 28
- 238000000034 method Methods 0.000 title claims abstract description 24
- 239000013081 microcrystal Substances 0.000 title claims abstract description 18
- 230000008569 process Effects 0.000 title claims abstract description 17
- 238000005245 sintering Methods 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- 239000011521 glass Substances 0.000 claims abstract description 20
- 239000002245 particle Substances 0.000 claims abstract description 19
- 239000002241 glass-ceramic Substances 0.000 claims abstract description 15
- 239000002994 raw material Substances 0.000 claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- 239000007787 solid Substances 0.000 claims abstract description 11
- 239000000203 mixture Substances 0.000 claims abstract description 10
- 239000002667 nucleating agent Substances 0.000 claims abstract description 9
- 238000002425 crystallisation Methods 0.000 claims abstract description 6
- 230000008025 crystallization Effects 0.000 claims abstract description 6
- 239000004088 foaming agent Substances 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 5
- 239000000047 product Substances 0.000 claims description 24
- 238000001816 cooling Methods 0.000 claims description 20
- 238000002156 mixing Methods 0.000 claims description 13
- 239000011819 refractory material Substances 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 9
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 8
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical group [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 7
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims description 6
- 235000011941 Tilia x europaea Nutrition 0.000 claims description 6
- 239000004571 lime Substances 0.000 claims description 6
- 229910010271 silicon carbide Inorganic materials 0.000 claims description 6
- 229910021532 Calcite Inorganic materials 0.000 claims description 5
- 239000006004 Quartz sand Substances 0.000 claims description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 5
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 5
- 239000006260 foam Substances 0.000 claims description 5
- 229910052664 nepheline Inorganic materials 0.000 claims description 5
- 239000010434 nepheline Substances 0.000 claims description 5
- 229910052656 albite Inorganic materials 0.000 claims description 4
- 229910052593 corundum Inorganic materials 0.000 claims description 4
- 239000010433 feldspar Substances 0.000 claims description 4
- 230000004907 flux Effects 0.000 claims description 4
- 229910001845 yogo sapphire Inorganic materials 0.000 claims description 4
- 238000010304 firing Methods 0.000 claims description 3
- 239000007795 chemical reaction product Substances 0.000 claims description 2
- 239000002184 metal Substances 0.000 claims description 2
- 229910052751 metal Inorganic materials 0.000 claims description 2
- 239000010814 metallic waste Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 238000009413 insulation Methods 0.000 abstract description 7
- 238000010276 construction Methods 0.000 abstract 1
- 238000002560 therapeutic procedure Methods 0.000 abstract 1
- 238000005516 engineering process Methods 0.000 description 9
- 239000000919 ceramic Substances 0.000 description 7
- 238000009837 dry grinding Methods 0.000 description 6
- 239000012071 phase Substances 0.000 description 6
- 230000006835 compression Effects 0.000 description 5
- 238000007906 compression Methods 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000012856 packing Methods 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 238000002791 soaking Methods 0.000 description 5
- 238000003860 storage Methods 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- 235000017550 sodium carbonate Nutrition 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000007767 bonding agent Substances 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 239000012774 insulation material Substances 0.000 description 2
- 229910052742 iron Inorganic materials 0.000 description 2
- 239000004014 plasticizer Substances 0.000 description 2
- 238000007493 shaping process Methods 0.000 description 2
- FUJCRWPEOMXPAD-UHFFFAOYSA-N Li2O Inorganic materials [Li+].[Li+].[O-2] FUJCRWPEOMXPAD-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000013459 approach Methods 0.000 description 1
- 229910001570 bauxite Inorganic materials 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004035 construction material Substances 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- XUCJHNOBJLKZNU-UHFFFAOYSA-M dilithium;hydroxide Chemical compound [Li+].[Li+].[OH-] XUCJHNOBJLKZNU-UHFFFAOYSA-M 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 230000005496 eutectics Effects 0.000 description 1
- 235000013312 flour Nutrition 0.000 description 1
- 239000010881 fly ash Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 229910003480 inorganic solid Inorganic materials 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910021645 metal ion Inorganic materials 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 239000006259 organic additive Substances 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 239000010970 precious metal Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000010791 quenching Methods 0.000 description 1
- 230000000171 quenching effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
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- 238000005728 strengthening Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 229920001187 thermosetting polymer Polymers 0.000 description 1
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- Compositions Of Oxide Ceramics (AREA)
Abstract
The present invention relates to a kind of preparation method of sintering process foaming micro crystal material product.It is primary raw material that its raw material for being technically characterized in that sintering process foaming micro crystal material product is inorganic non-metallic solid discarded object, is mixed with the addO-on therapy such as the glass ceramics frit water particle containing Nucleating Agent.In production process, the batch containing Nucleating Agent and foaming agent is prepared using mix grinding mode first, secondly in the foaming of sintering process high temperature, then the crystallization of glass phase in its product is controlled by adjusting the method for temperature lowering curve, the glass phase remained in sintering process foaming micro crystal material is greatly lowered, so that its material product has enough intensity.Obtained sintering process foaming micro crystal material, with the characteristic such as light body, heat-insulated, sound-absorbing, high intensity, can be widely applied to the insulation needs of construction wall and industrial equipment, it is possible to achieve industrialized production.
Description
Technical field：
The invention belongs to building material field, and in particular to using the manufacture sintering process foaming of inorganic non-metallic solid discarded object
The preparation method of micro crystal material product.
Background technology：
Inorganic foamed micro crystal material due to it is non-ignitable, insulation the characteristics of, there is wide application in building energy saving field
Prospect.
Since the product invention, foamed glass has had substantial amounts of public technology and patented technology, mainly uses glass
Glass foams, and manufactures light heat insulation material, and its foam process principle is foundation of the invention, and ceramic production technology is base of the invention
Plinth.
Sintering process foamed ceramic is typically ceramic batch and a series of physical and chemical reaction occurs in sintered kind, makes
Ceramic particle is bonded and produces certain glass phase, is formed due to the effect of foaming agent at high temperature with ceramic crystalline phase and glass
The porous material that glass is mixed.Because amount of glassy phase is few compared with foamed glass, thus, the table of resulting expanded material after foaming
Density is seen to be difficult that 200kg/m can be accomplished as foamed glass3Below.And with apparent density reduction, intensity significantly drops
It is low.
Foaming devitrified glass is by by the vitreum melt foaming containing Nucleating Agent, then controlling it crystallization, and manufacture is brilliant
Phase content expanded material high, has good effect in terms of insulation material mechanical property is improved.But foaming devitrified glass by
It is primary raw material in the devitrified glass water quenching material containing Nucleating Agent is used completely, manufacturing cost is higher, limits it in building work
The extensive application of industry.
A kind of " crystallite foaming ceramic composition and its manufacture method " of application number 200710105769.X is with specific porcelain
Soil is primary raw material, the various raw materials such as chemical addition agent, plasticizer, bonding agent need to be added, using the anhydrous mixing of chemical thermosetting
Recipe, but also need to be sintered after mud processed, shaping.The process of its control crystallization is not described.Nucleator is precious metal ion
(Li2O)。
The content of the invention：
According to the deficiencies in the prior art, the technical problem to be solved in the present invention is：There is provided a kind of high intensity, low cost it is new
Type safety heat-preserving construction material, while the sintering process foaming micro crystal material product of the inorganic non-metallic solid discarded object that can largely dissolve
And preparation method thereof.
The present invention is different from closest to prior art：
Raw materials used is based on inorganic non-metallic solid discarded object, to be equipped with the glass ceramics frit water containing Nucleating Agent broken
Material and other inorganic raw materials, mixing dry grinding is then charged into sintered and foamed in refractory-material dies, and control crystallization, cooling are come out of the stove.Match somebody with somebody
Close and be not required to add chemical organic additive, plasticizer, bonding agent etc. in expecting, sintered after being not required to mud processed and shaping.The present invention be
Grow up on the basis of existing foamed glass, sintering process foamed ceramic, foaming devitrified glass.Solution technology of the present invention is asked
Inscribing used technical scheme is：The glass ceramics frit water particle containing Nucleating Agent is introduced in composition of raw materials, batch is controlled
Intercrystalline glass phase crystallite turns to core technology, and manufacture is cheap, high intensity, the sintering process of low bulk density foaming micro crystal material,
Can be used for the fields such as industry and building energy conservation.
1st, composition of raw materials of the invention is：Inorganic non-metallic solid discarded object=30~85%, feldspar, quartz sand=0~
60%, nepheline, Al2O3=0~30%, calcite, CaCO3, lime=0~30%, flux 0~10%, glass ceramics frit
Water particle 5~40%, foaming agent 0~5%.
Wherein：
1) the inorganic non-metallic solid discarded object is any gangue, metal tailings, factory's inorganic non-metallic waste residue etc.
One kind, or the inorganic non-metallic solid discarded object that two kinds and two or more arbitrary proportions mix.
2) the glass ceramics frit water particle described in is containing Nucleating Agent 0.5%~10%.
3) feldspar, quartz sand described in are two kinds of one of which or arbitrary proportion mixing.
4) nepheline, Al described in2O3It is two kinds of one of which or arbitrary proportion mixing.
5) calcite, CaCO described in3, lime be one of which, two kinds of arbitrary proportion mixing or arbitrary proportion it is mixed
Three kinds for closing.
6) flux described in is calcined soda for industry or albite.
7) foaming agent described in is carborundum powder, CaCO3Or one kind of lime.
2nd, production technology is comprised the following steps：
1) raw material is prepared into batch using dry method mix grinding mode.
2) batch is fitted into and is placed on kiln car in the refractory-material dies with demoulding material.
3) refractory-material dies that will install batch transport into kiln heating by kiln car, and high temperature foaming firing is formed,
The crystallization of glass phase in its product is controlled in sintering procedure.
4) end product cooling, the demoulding, you can obtain the micro crystal material product that foams.
Wherein：
Step 1) in, the granularity of cooperation material granularity≤120 mesh after the mixed grinding.
Step 2) in, the thickness that loads of the batch is the 1/5~1/2 of cavity body of mould height, the height of cavity body of mould
Less than 400mm.
Step 3) in, the heating rate of the kiln is 1~5 DEG C/min, the foaming burn till maximum temperature for 1000~
1200℃。
Step 4) in, 950 DEG C of rate of temperature fall is cooled to for 5-10 DEG C/min after burning till foaming, 950~550 DEG C of cooling
0.5-1 DEG C of speed/min, less than 550 DEG C of 1-5 DEG C of rate of temperature fall/min.
It is of the invention compared with present technology, have the positive effect that：
It is main material production sintering process foaming micro crystal material product with non-metal inorganic solid discarded object, can be advised with maximum
The big comprehensive solid waste of dissolving of mould, not only contributes to the protection of environment, also for the second development and utilization of resource have found effectively
Approach.
By the use of the glass ceramics frit water particle containing Nucleating Agent as addition raw material, multinomial technique effect is can reach：It is first
First, because the strengthening action of microcrystal crystal grain and microcrack evolution equation effect, so that product strength is improved.Secondly because
The complexity of microcrystal reduces the thermal conductivity factor of product the optimization of convection conduct heat phonon free path.Meanwhile, firing
Cheng Zhong, makes the eutectic being dispersed in batch be initially formed hybrid glass liquid phase with glass ceramics frit water flour material, favorably
It is that base substrate foaming creates conditions, than using glass ceramics frit or glass dust completely in the bonding for promoting batch particle raw material
Material produces crystallite foaming product as raw material, can reduce a large amount of production costs.
Therefore, the present invention is using the manufacture sintering process foaming of inorganic non-metallic solid discarded object micro crystal material and its making side
Method, is a new and high technology that is simultaneous and having energy-conservation and environmentally friendly double effect, and prepared foaming micro crystal material product has strong
The low advantage of degree height, toughness high, low cost, thermal conductivity factor.There is novelty in thinking, there is novelty on technical operation
Property, there is good application prospect and practical value in building field and industrial heat preservation field.
Specific embodiment
Example 1,
By gold mine tailings 60kg, glass ceramics frit water particle 10kg, nepheline 24kg, soda ash 5kg, carborundum 1.0kg, mix
Close the granularity of dry grinding to powder particles≤120 mesh.These batches for processing are seated in the container of refractory material, then
In kiln, 1160 DEG C of thermal insulation foamings, soaking time 40 minutes are heated to by the heating rate of 2~4 DEG C/min；Then with 10
DEG C/cooling rate of min reduced the temperature to 950 DEG C, then after reduced the temperature to 550 DEG C, most with the cooling rate of 1 DEG C/min
Room temperature is reduced the temperature to the cooling rate of 1~3 DEG C/min afterwards, is come out of the stove.
Obtained product apparent density is 310g/m3, compression strength is 3.0Mpa, and thermal conductivity factor is≤0.10w/m.k.Cut
It is cut into standard-sized finished product packing storage.
Example 2,
By flyash 50kg, glass ceramics frit water particle 20kg, quartz sand 25kg, soda ash 4kg, carborundum 1.0kg, mix
Close the granularity of dry grinding to powder particles≤120 mesh.These batches for processing are seated in the container of refractory material, then
In kiln, 1150 DEG C of thermal insulation foamings, soaking time 40 minutes are heated to by the heating rate of 2~4 DEG C/min；Then with 10
DEG C/cooling rate of min reduced the temperature to 950 DEG C, then reduced the temperature to 550 DEG C, finally with the cooling rate of 1 DEG C/min
Room temperature is reduced the temperature to the cooling rate of 1~3 DEG C/min, is come out of the stove.
Obtained product apparent density is 230g/m3, compression strength is 2.0Mpa, and thermal conductivity factor is≤0.08w/m.k.Cut
It is cut into standard-sized finished product packing storage.
Example 3,
By gangue 50kg, glass ceramics frit water particle 25kg, albite 24kg, carborundum 1.0kg, mixing dry grinding is extremely
The granularity of powder particles≤120 mesh.These batches for processing are seated in the container of refractory material, then in kiln
In, it is heated to 1170 DEG C of thermal insulation foamings, soaking time 40 minutes by the heating rate of 2~4 DEG C/min；Then with 10 DEG C/min's
Cooling rate is reduced the temperature to 950 DEG C, then is reduced the temperature to 550 DEG C, finally with 1~3 with the cooling rate of 1 DEG C/min
DEG C/cooling rate of min reduces the temperature to room temperature, come out of the stove.
Obtained product apparent density is 280g/m3, compression strength is 2.8Mpa, and thermal conductivity factor is≤0.09w/m.k.Cut
It is cut into standard-sized finished product packing storage.
Example 4,
By iron ore mine 50kg, glass ceramics frit water particle 36kg, alundum (Al2O3) 10kg, soda ash 3kg, carborundum
1.0kg, the granularity of mixing dry grinding to powder particles≤120 mesh.These batches for processing are seated in the appearance of refractory material
In device, then in kiln, 1150 DEG C of thermal insulation foamings, soaking time 40 minutes are heated to by the heating rate of 2~4 DEG C/min；
Then reduced the temperature to 950 DEG C with the cooling rate of 10 DEG C/min, then with the cooling rate of 1 DEG C/min reduce the temperature to
550 DEG C, room temperature is finally reduced the temperature to the cooling rate of 1~3 DEG C/min, come out of the stove.
Obtained product apparent density is 200g/m3, compression strength is 1.5Mpa, and thermal conductivity factor is≤0.07w/m.k.Cut
It is cut into standard-sized finished product packing storage.
Example 5,
Bauxite red mud is carried the slag 40kg after iron, glass ceramics frit water particle 30kg, albite 20kg, calcite
10kg, the granularity of mixing dry grinding to powder particles≤120 mesh.These batches for processing are seated in the container of refractory material
In, then in kiln, 1130 DEG C of thermal insulation foamings, soaking time 40 minutes are heated to by the heating rate of 2~4 DEG C/min；So
Reduced the temperature to 950 DEG C with the cooling rate of 10 DEG C/min afterwards, then reduced the temperature to 550 with the cooling rate of 1 DEG C/min
DEG C, room temperature is finally reduced the temperature to the cooling rate of 1~3 DEG C/min, come out of the stove.
Obtained product apparent density is 170g/m3, and compression strength is 1.0Mpa, and thermal conductivity factor is≤0.06w/m.k.Cut
It is cut into standard-sized finished product packing storage.
Claims (1)
1. a kind of sintering process foams the preparation method of micro crystal material product, it is characterised in that：
Composition of raw materials is：Inorganic non-metallic solid discarded object=30~85%, feldspar, quartz sand=0~60%, nepheline, Al2O3
=0~30%, calcite, CaCO3, lime=0~30%, flux 0~10%, glass ceramics frit water particle 5~40%,
Foaming agent 0~5%；
1) raw material is prepared the batch for meeting technical recipe using dry method mix grinding mode；
2) batch is fitted into and is placed on kiln car in the refractory-material dies with release materials；
3) refractory-material dies that will install batch transport into kiln heating by kiln car, and high temperature foaming firing is formed, fired
During control the crystallization of glass phase in its product；
4) end product cooling, the demoulding, you can obtain the micro crystal material product that foams；
Wherein：
Step 1) in, the granularity of cooperation material granularity≤120 mesh after mixed grinding；
Step 2) in, the thickness that loads of the batch is the 1/5~1/2 of cavity body of mould height, and the height of cavity body of mould is less than
400mm；
Step 3) in, the heating rate of the kiln is 1~5 DEG C/min, and it is 1000~1200 that maximum temperature is burnt till in the foaming
℃；
Step 4) in, after burning till foaming, 950 DEG C of rate of temperature fall is cooled to for 5-10 DEG C/min, 950~550 DEG C of cooling speed
0.5-1 DEG C of rate/min, less than 550 DEG C of 1-5 DEG C of rate of temperature fall/min；
Described inorganic non-metallic solid discarded object be gangue, metal tailings, factory inorganic non-metallic waste residue any one, or
The inorganic non-metallic solid discarded object of two or more arbitrary proportion mixing；
Described feldspar, quartz sand are two kinds of one of which or arbitrary proportion mixing；
Described nepheline, Al2O3It is two kinds of one of which or arbitrary proportion mixing；
Described calcite, CaCO3, lime be one of which, or two kinds of arbitrary proportion mixing or arbitrary proportion mixing three
Kind；
Described glass ceramics frit water particle is containing Nucleating Agent 0.5%~10%；
Described flux is calcined soda for industry or albite；
Described foaming agent is carborundum powder, CaCO3Or one kind of lime.
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| CN201310349128.4A CN104230170B (en) | 2013-06-07 | 2013-08-13 | A kind of preparation method of sintering process foaming micro crystal material product |
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| CN106747615A (en) * | 2017-03-09 | 2017-05-31 | 咸阳陶瓷研究设计院 | A kind of method that utilization molybdenum tailing produces ceramic thermal insulation plate |
| CN109180143A (en) * | 2018-09-03 | 2019-01-11 | 岑金涛 | The composite foamed ceramic assembled building wall material of nano microcrystalline and its manufacturing method |
| CN112876214B (en) * | 2021-01-22 | 2022-07-19 | 北京科技大学 | Microcrystalline foamed ceramic and preparation method and application thereof |
| CN112679224B (en) * | 2021-01-27 | 2022-09-16 | 辽宁罕王绿色建材有限公司 | Micro-crystallized porous ceramic plate and preparation method thereof |
| CN115108726B (en) * | 2022-08-12 | 2023-05-12 | 西南科技大学 | Porous microcrystalline glass using coal gangue as raw material and preparation method thereof |
| CN115557703A (en) * | 2022-09-14 | 2023-01-03 | 沈阳环境科学研究院 | Preparation method of high-added-value microporous foamed glass ceramics made of coal gangue |
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| CN102633426A (en) * | 2011-12-13 | 2012-08-15 | 淄博钰晶新型材料科技有限公司 | Method for producing microcrystal foam heat-insulation plate by aid of industrial red mud |
| CN103102076A (en) * | 2012-11-14 | 2013-05-15 | 张文知 | Method for manufacturing microcrystalline glass water-quenched material by adopting amorphous graphite ore surrounding rock spontaneous combustion method |
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