CN103172253B - A kind of method of utilizing the spontaneous brewed standby froth inorganic stock of gangue cenosphere - Google Patents
A kind of method of utilizing the spontaneous brewed standby froth inorganic stock of gangue cenosphere Download PDFInfo
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- CN103172253B CN103172253B CN201310132817.XA CN201310132817A CN103172253B CN 103172253 B CN103172253 B CN 103172253B CN 201310132817 A CN201310132817 A CN 201310132817A CN 103172253 B CN103172253 B CN 103172253B
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Abstract
The invention discloses a kind of method of utilizing the spontaneous brewed standby froth inorganic stock of gangue cenosphere that belongs to light material preparing technical field. Gangue microballon of the present invention is primary raw material, the method of reacting spontaneous brewed standby froth inorganic stock by it with glass dust, is characterized in not needing additionally adding blowing agent, utilizes the at high temperature generated reactive gas foaming certainly of gangue microballon and glass dust, technical process is simple, and preparation cost is low. Froth inorganic stock prepared by the inventive method has that intensity is high, density is low, non-combustible, heat-proof quality good, sqouynd absorption lowering noise, integrated cost are low, utilize the features such as solid waste in a large number, has broad application prospects.<!--1-->
Description
Technical field
The invention belongs to light material preparing technical field, particularly one utilizes gangue hollow micro-The method of the spontaneous brewed standby froth inorganic stock of pearl and glass dust generated reactive gas.
Background technology
Gangue is the solid waste producing in coal mining, dressing of coal by washing process, annual dischargeAmount is equivalent to 10% left and right of coal production then. According to incompletely statistics, whole nation accumulation over the years at presentApproximately 4,500,000,000 tons of the gangues of stacking, larger hillock has more than 1600, takes up an area approximately1.5 ten thousand hectares, and accumulating amount is also with the speed increase of annual 1.5～200,000,000 tons, is currentOne of industrial solid castoff of China's discharge capacity maximum. Gangue is stored up for a long time, takies a large amount ofSoil, easily causes spontaneous combustion, atmosphere pollution and groundwater quality. Although gangue is coal industryDiscarded object, is simultaneously again available natural resources, fully excavate gangue application prospect,The application of widening gangue is the important component part of coal resources comprehensive utilization.
The main component of gangue is A2O3、SiO2(average content is more than 50%), Fe2O3、CaThe compound of O, MgO and potassium and phosphorus etc., and micro heavy. In gangue organic withChange (generally in 20% left and right) containing coal amount, mainly comprise the elements such as C, H, O, N, S,Wherein C is main component. The moisture of various gangues is all less than 5%. Gangue routine mainChemical composition is in table 1.
The conventional chemical composition of table 1 gangue
China has carried out the work of gangue comprehensive utilization from 20 century 70s, has opened up oneSeries gangue utilize approach. But due to the restriction of resource qualitative factor, economic condition,The gap of technical equipment and the impact of turn of the market, at present the utilization rate of gangue be 10%～30%, gap is still larger compared with developed countries.
At present, the research of China's gangue and application mainly concentrate on coal gangue power generation, extract chemical industry productProduct, directly utilization (as roadbed, ground, soil improvement and shaped coal additive) and production building materialsEtc. aspect. The gangue that phosphorus content is lower can be used for producing brick and tile, cement, lightweight aggregate, slagThe construction materials such as cotton and engineering plastics; The few gangue of phosphorus content can be used for filling out hole, make ground,Backfill opencut and as roadbed material; Gangue after spontaneous combustion, can through broken, screeningPreparation Binder Materials. Some colliery powders also can be used to improve soil, doFertilizer and farm chemical carrier. The gangue that alumina content is high, can extract polymeric aluminum, aluminium chloride andThe chemical products such as aluminum sulfate.
Although the research of gangue classification application caused extensive attention and carried out corresponding research work,But generally acknowledged scientific classification index is not yet formulated, main cause is various places gangue complicated components,Physicochemical characteristic is different. In addition, the change of different gangue processing and utilization directions to gangueStudy point and physicochemical characteristics requires differently, this is also that classification and the name of gangue is difficult to reachBecome consistent reason. As can be seen here, gangue complicated component is the weight of its large-scale application of restrictionWant reason.
Hebei YL-inno Co., Ltd. do not considering on the basis of gangue complicated component,Gangue is prepared into the functional material with special construction---micron order cenosphere (middle promulgated by the State CouncilBright patent: 200910131051.7). The unique texture of cenosphere makes it have more high-strengthIn degree time,, have again that bulk density is low, quality is light, and thermal conductivity factor is little, good heat insulating,The characteristics such as sound insulation, wear-resisting, high dispersive, electrical insulating property and Heat stability is good, can be used as a kind of highBy force, lightweight, the excellent infant industry basic material of property, there is wide market application foreground.
Froth inorganic stock be a kind of porosity between 40-95%, in structure, show bubble is inorganic manyHole material, the aperture size of foamed material from nanometer to micron until millimeter. Foamed material hasThe advantages such as density is little, the porosity is high, specific area is large, low-thermal conductivity, are used as molten stateMetal filtration, purifying vehicle exhaust material, sewage disposal, heat-insulating sound-insulating, catalyst carrier,Electrolyte membrane and separation disperse original paper etc., are widely used in industrial circle, aviation field, electronicsField, building field, field of medicaments and biochemical field etc.
Directly foaming is to prepare a kind of most important method of the porous material such as foamed ceramics and foam glass, direct foaming is divided into again high temperature foaming and room temperature foams two kinds, and wherein room temperature foaming is mainly answeredFor the preparation of foamed ceramics, in ceramic size, introduce a large amount of bubbles, form stable potteryPorcelain foamed slurry, drying and sintering after moulding; High temperature foaming is used for the preparation of foam glass,Together with glass dust is pre-mixed with blowing agent, be heated certain temperature, rely on and send outInfusion self produces gas or blowing agent and glass dust generated reactive gas, forms gas in glassHole, obtains foam glass after cooling. This patent utilizes gangue cenosphere and glass dust at heightTemperature issues biochemical generated reactive gas from foaming, prepares gangue hollow without interpolation blowing agentMicroballon foamed material.
Before inventor herein, once propose two and prepared inorganic foamed insulation with gangue hollow ball microballonThe patent of invention of material, comprise a kind of inorganic cellular insulant with secondary hole-closing structure andIts preparation method (application number: 201210282748.6), taking gangue cenosphere as major ingredient, taking cement as Binder Materials, add animal blowing agent and at room temperature foam and prepare foam mortar,Be poured into die for molding, then obtain foamed material, another patent of invention through maintenance, after dryBe: a kind of inorganic heat insulation material and preparation thereof with three grades of pore structuresMethod (application number: 201210592778.7), first by gangue cenosphere, glass dust,High-temperature foaming agent, foam stabilizer are mixed to form premix, then by water-soluble to premix and epoxy resinLiquid mixes, then adds surfactant foaming agent, stirs and obtains foamed slurry, and foamed slurry watersNote, in mould, obtains base substrate after cold curing, through super-dry, binder removal, and high temperature foaming, fixedType, foamed material is provided in cooling preparation. Compared with above-mentioned two patents, this patent is maximum with itBe not both, do not need additionally to add blowing agent, significantly reduce manufacturing cost, do not need preparationThis step of foamed slurry, reduced simultaneously foamed slurry moulding, solidify, the operation such as dry, it is more simple and easy to do that preparation technology becomes.
Summary of the invention
The object of the invention is the present situation for Coal Gangue Resource comprehensive utilization, propose one and utilize bastard coalThe method of reacting spontaneous brewed standby froth inorganic stock between stone cenosphere and glass dust, thisIt is a kind of approach of the gangue product of producing high added value.
To achieve these goals, the present invention has adopted following technical scheme:
A method of utilizing the spontaneous brewed standby froth inorganic stock of gangue cenosphere, comprises followingStep:
Step 1: feed coal spoil cenosphere, glass dust, foam stabilizer are mixed, obtain pre-Batch mixing;
Step 2: above-mentioned premix is put into the crucible that scribbles releasing agent, and be placed in Elema resistanceIn stove;
Step 3: resistance furnace is heated to 400 ° of C with the rate of heat addition of 5 ~ 10 ° of C/min from room temperature, protectsTemperature 0 ~ 120min, continues to be heated to 700 ° of C with the rate of heat addition of 5 ~ 10 ° of C/min, insulation 5 ~ 120min, is warming up to 900 ~ 1100 ° of C with 10 ~ 15 ° of C/min rates of heat addition, insulation 10 ~ 120miN foaming, after foaming finishes, is cooled to 800 ° with the cooldown rate of 15 ~ 20 ° of C/min by sampleC, cools to room temperature afterwards with the furnace, obtains froth inorganic stock.
Described in step 1, in raw material, gangue cenosphere mass fraction is 50 ~ 80%, and glass dust quality is dividedNumber is 15 ~ 45%, and foam stabilizer mass fraction is 0.5 ~ 5%.
The bulk density of described gangue cenosphere is 100 ~ 600kg/m3; Diameter is 5 ~ 1000 μ m,Room temperature thermal conductivity factor is less than 0.12W/mK.
Described glass dust is that softening temperature is simple glass powder or the boron glass powder of 500 ~ 700 ° of C.
Described foam stabilizer is one or more in calgon, borax or sodium sulphate.
Froth inorganic stock prepared by the above-mentioned method of preparing froth inorganic stock, unit weight is 0.10 ~ 0.90g/cm3, compression strength is 0.3-20MPa, the porosity is 50 ~ 95%.
Beneficial effect of the present invention is: taking gangue cenosphere as primary raw material, by itself and glass dustBetween the spontaneous brewed standby froth inorganic stock of generated reactive gas, regulate blowing temperature can make materialMaterial has a large amount of stableThe pore of sealing. The froth inorganic stock making by the present invention, have lightweight, high-strength, everyHeat, insulation, fire prevention, durable feature, can be widely used in building, industrial energy saving insulation neckTerritory. Produce, preparation method is simple and convenient, be suitable for large-scale industrial and produce.
Brief description of the drawings
Fig. 1 is gangue cenosphere microscopic appearance figure.
Fig. 2 is that gangue cenosphere is from foaming sample surface morphology.
Detailed description of the invention
Below in conjunction with specific embodiment, the present invention will be further described in detail:
Prepare the method and apparatus of gangue cenosphere and see that application number is patent 200910131051.7,Its concrete preparation method is:
The ratio taking volume ratio as 1:4 by Coal gangue powder and water, adds simultaneously and accounts for cumulative volume 1vol.%'sBall milling after ammonium citrate mixes, prepares the slurry that solid concentration is 20vol.%; This slurry is addedEnter in the triton x-100 blowing agent of 1vol.%, fully stir, make stable foamed slurry; Stable foamed slurry is added to centrifugal atomizing equipment, make its atomization form hollow slurry drop, and spray in forming room, slurry drop dries out dry fast, forms gangue hollow micro-Pearl base substrate, wherein moulding indoor temperature is 200 ° of C; Gangue cenosphere base substrate is put into backIn rotary kiln stove, 1200 ° of C carry out sintering, make gangue cenosphere;
The bulk density of the gangue cenosphere making is 100 ~ 600kg/m3; Diameter is 5 ~ 1000 μM, room temperature thermal conductivity factor is less than 0.12W/mK.
Embodiment 1
The mass fraction of gangue cenosphere, boron glass powder, foam stabilizer is respectively 50,49,1%,Wherein the microscopic appearance figure of gangue cenosphere as shown in Figure 1, mixes above-mentioned raw materials,Put into the crucible that scribbles releasing agent, be then placed in Elema resistance furnace, by resistance furnace with 5 °The rate of heat addition of C/min is heated to 400 ° of C from room temperature, and insulation 20min, with adding of 8 ° of C/minHot speed continues to be heated to 700 ° of C, and insulation 30min is further with 10 ° of C/min rates of heat additionBe warming up to 900 ° of C, insulation 30min foaming, when foaming finishes, with the cooling speed of 20 ° of C/minSample is cooled to 800 ° of C by rate, cools to afterwards room temperature with the furnace, for obtaining froth inorganic stock; Fig. 2 is gangue cenosphere from foaming sample surface morphology, froth inorganic stock physicalCan be in table 2.
Embodiment 2
The mass fraction of gangue cenosphere, boron glass powder, foam stabilizer is respectively 65,33,2%,Above-mentioned raw materials is mixed, put into the crucible that scribbles releasing agent, be then placed in Elema electricityIn resistance stove, by resistanceStove is heated to 400 ° of C with the rate of heat addition of 5 ° of C/min from room temperature, and insulation 60min, with 8 ° of C/The rate of heat addition of min continues to be heated to 700 ° of C, and insulation 60min, with 10 ° of C/min rates of heat additionFurther be warming up to 980 ° of C, insulation 30min foaming, when foaming finishes, with 20 ° of C/min'sSample is cooled to 800 ° of C by cooldown rate, cools to afterwards room temperature with the furnace, obtains inorganic foamedMaterial, its physical property is in table 2.
Embodiment 3
The mass fraction of gangue cenosphere, simple glass powder, foam stabilizer is respectively 72,26,2%, above-mentioned raw materials is mixed, put into the crucible that scribbles releasing agent, be then placed in ElemaIn resistance furnace, resistance furnace is heated to 400 ° of C with the rate of heat addition of 5 ° of C/min from room temperature, protectsTemperature 100min, continues to be heated to 700 ° of C with the rate of heat addition of 8 ° of C/min, insulation 45min, with15 ° of C/min rates of heat addition are further warming up to 1050 ° of C, insulation 10min foaming, and foaming finishesTime, with the cooldown rate of 20 ° of C/min, sample is cooled to 800 ° of C, cool to afterwards chamber with the furnaceTemperature, obtains froth inorganic stock, and its physical property is in table 2.
Table 2 embodiment obtains the physical property of insulation material
As can be seen from the above table, the prepared gangue froth inorganic stock product of the embodiment of the present invention 1 ~ 3There is light weight, the feature that high-strength, thermal conductivity factor is low.
Claims (5)
1. a method of utilizing the spontaneous brewed standby froth inorganic stock of gangue cenosphere, is characterized in that,Comprise the following steps:
Step 1: feed coal spoil cenosphere, glass dust, foam stabilizer are mixed, obtain premix;
Step 2: above-mentioned premix is put into the crucible that scribbles releasing agent, and be placed in Elema resistance furnace;
Step 3: resistance furnace is heated to 400 DEG C with the rate of heat addition of 5～10 DEG C/min from room temperature, insulation0～120min, continues to be heated to 700 DEG C with the rate of heat addition of 5～10 DEG C/min, insulation 5～120min, with10～15 DEG C/min rate of heat addition is warming up to 900～1100 DEG C, insulation 10～120min foaming, and after foaming finishes,Sample is cooled to 800 DEG C by cooldown rate with 15～20 DEG C/min, cools to afterwards room temperature with the furnace, obtains nothingMachine foamed material.
2. the gangue cenosphere spontaneous brewed standby froth inorganic stock of utilizing according to claim 1Method, is characterized in that: described in step 1, in raw material, gangue cenosphere mass fraction is 50～80%, glassGlass powder mass fraction is 15～45%, and foam stabilizer mass fraction is 0.5～5%.
3. the gangue cenosphere spontaneous brewed standby froth inorganic stock of utilizing according to claim 1Method, is characterized in that, the bulk density of described gangue cenosphere is 100～600kg/m3; Diameter is5～1000 μ m, room temperature thermal conductivity factor is less than 0.12W/mK.
4. the gangue cenosphere spontaneous brewed standby froth inorganic stock of utilizing according to claim 1Method, is characterized in that, described glass dust is that softening temperature is simple glass powder or the boron glass of 500～700 DEG CPowder.
5. the gangue cenosphere spontaneous brewed standby froth inorganic stock of utilizing according to claim 1Method, is characterized in that, described foam stabilizer be in calgon, borax or sodium sulphate a kind of or a kind of withOn.
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| CN107162391A (en) * | 2017-05-12 | 2017-09-15 | 清华大学 | A kind of preparation method that the regulatable foam glass of micron order air hole structure is prepared by raw material of cullet |
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| CN108499522B (en) * | 2018-03-20 | 2020-08-21 | 清华大学 | Coal gangue cenosphere/aluminosilicate polymer composite adsorbent and preparation method thereof |
| CN108585935B (en) * | 2018-05-15 | 2020-08-21 | 清华大学 | Coal gangue hollow microsphere/foamed aluminosilicate polymer composite material and preparation |
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