CN103011890B - Method for preparing light wall material by microwave baking of chromic slag - Google Patents
Method for preparing light wall material by microwave baking of chromic slag Download PDFInfo
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- CN103011890B CN103011890B CN201210589168.1A CN201210589168A CN103011890B CN 103011890 B CN103011890 B CN 103011890B CN 201210589168 A CN201210589168 A CN 201210589168A CN 103011890 B CN103011890 B CN 103011890B
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Abstract
The invention relates to a method for preparing light wall material by microwave baking of chromic slag. The method comprises the following steps of: respectively metering the chromic slag, coal ash and sodaclase according to weight ratios of 55-65%, 20-30% and 15-25%, and uniformly mixing the chromic slag, the coal ash and the sodaclase, thus obtaining a batch mixture; weighing a reducing agent according to the weight ratio of 5-10% of the chromic slag, and adding water in a weight of 2-4 times of the weight of the reducing agent into the reducing agent to obtain a water solution; mixing the water solution with the batch mixture to obtain a mixture, and pressing the mixture into green bricks; and conveying the green bricks into an industrial microwave oven after drying, thus obtaining the light wall material by microwave high-temperature sintering. According to the method for preparing light wall material by the microwave baking of the chromic slag, hexavalent chromium in the microwave baking is converted into trivalent chromium by the reducing agent under industrial microwaves, then a glassy state molten mass is formed by the high-temperature sintering, and the light wall material is further prepared. When the chromic slag is subjected to detoxifying and innocent treatment, the chromic slag is subjected to recycling comprehensive utilization and changed from waste material into things of value; and the industrial microwave heating is adopted, the heating speed is quick and free of pollution, meanwhile, the microwave heating can be precisely controlled, the heat treatment time is shortened, the energy source is saved, and the environmental protection is benefitted.
Description
Technical field
The present invention relates to a kind of method of preparing light wall material, particularly relate to a kind of chromium slag that utilizes and through microwave thermal, process the method for manufacturing standby light wall material.
Background technology
Chromium slag is a kind of solid waste producing in chromium metal and chromium salt production process, because its water-solubility Cr that contains excess (VI) has strong toxicity, is one of internationally recognized 47 kinds of refuses the most dangerous.In China, containing chromium refuse, be put into the Hazardous Waste List > > of < < country.Objectionable constituent in chromium slag are mainly the hexavalent chromiums such as solubility chromic acid sodium, solubility in acid yellow ultramarine, and hexavalent chromium is very large to the murder by poisoning of HUMAN HEALTH.Cr(VI in chromium slag) can to ecotope, cause severe contamination with rainwater infiltration.Chromium slag contaminated harm has potentiality, disguise and chronicity, once cause the environmental pollutions such as water body, soil, even if drop into, is greatly also difficult to recover again original appearance.The chromium slag that accumulate in the whole nation at present surpasses 2,500,000 tons, and annual also by the speed increase with few hundred thousand tonnes of.The correlative study of administering and fully utilize chromium slag is both at home and abroad more, mainly contains the four large classes such as solidification method, reduction method, complexometry and biological process.It is reductive agent that high temperature solid-state reduction method be take powdered carbon, wood chip, rice husk, coal gangue and metallurgical slag etc., utilizing the excessive C wherein containing to carry out high-temperature fusion with chromium slag reacts, make the Cr (VI) in chromium slag be reduced into Cr (III), finally with vitreous state or spinel form, exist.The method removing toxic substances is thorough, stable, is the prefered method of chromium slag recycling treatment.But the method chromium slag is not fully utilized, and production efficiency is lower, and energy consumption is higher.
A large amount of non-baked light-weight materials for walls that use mainly contain concrete hollow block and air-entrained concrete building block in the market, but the need of production of gas concrete consumes cement, consume energy larger, and the water-intake rate of gas concrete is higher, easily cracks, and volume stability is poor, ubiquity is built wall crazing, in harsh climate environment, the problems such as freeze injury occur, its use is restricted, and also has influence on use function and the visual appearance of buildings.
Application number is that 201010592512.3 patent application document discloses a kind of glazed self-insulation foamed ceramic composite wall material and preparation method thereof, it is main raw material that the method be take slag, flyash, wilkinite, during preparation, at mould bottom, spread the first tight zone, spread successively thermal insulation layer, the second tight zone, glaze, then press molding obtains green compact again; Green compact are dry, pack kiln high temperature into and burn till.Utilize ceramic waste material to be broken into particle, add tackiness agent and water, press forming becomes firing time 10-12 hour at 1100-1150 ℃ through tunnel klining.This patent application utilizes the raw materials such as slag, flyash, wilkinite, do not relate to the problem of utilizing of chromium slag, and firing time is longer, needs to consume mass energy, and production cost is higher, affects it and applies.
Summary of the invention
The technical problem to be solved in the present invention: overcome in prior art chromic slag harmlessness and process the problems such as insufficient, complex process, cost are higher, provide a kind of and make full use of chromium slag resource, energy consumption is low, efficiency is high, the microwave thermal of utilizing of energy-conserving and environment-protective is processed the method that chromium slag is prepared light wall material.
technical scheme of the present invention:
Microwave thermal is processed the method that chromium slag is prepared light wall material, comprises the following steps:
1) chromium slag, flyash, albite are measured respectively by the weight ratio of 55-65%, 20-30%, 15-25%, and pulverize;
2) chromium slag, flyash and albite are together added in mixer, mix, obtain admixtion;
3) weight ratio of pressing chromium slag 5-10% weighs reductive agent, to adding water in reductive agent, is made into the aqueous solution, amount of water be reductive agent weight 2-4 doubly; This aqueous solution is mixed and obtains compound with described admixtion, then compound is pressed into adobe;
4) by sending into industrial microwave oven after brick bat drying, through microwave high-temperature sintering, obtain light wall material.
Described reductive agent is one or more the mixture in glucose, sucrose, oxalic acid and citric acid.
The power of described industrial microwave oven is 30-60KW, and temperature rise rate during microwave high-temperature sintering is per minute 5-15 ℃, is warming up to 900-1100 ℃, and is incubated 15-35min at this temperature.
The granularity of the chromium slag of described pulverizing, flyash, albite is 0.074-0.3mm; Pressure during pressing unfired brick is 5-20MPa.
positive beneficial effect of the present invention:
(1) the present invention be take chromium slag, flyash, albite and reductive agent as main raw material, adopt reduction curing legal system for light wall material, under reductive agent, by microwave thermal, process sexavalent chrome poisonous in chromium slag is converted into the trivalent chromium that toxicity is less, through high-temperature fusion sintering, prepare light wall material, trivalent chromium is further solidified and sealed.The present invention completes chromium residue detoxifying, preparation one step curing and light wall material, work simplification, and production cost is lower, and the materials for wall obtaining is vitreous structure and porous nickel, and product quality is better.Micro-structure diagram 2-Fig. 5 referring to product.
The technical indicator of product of the present invention: density: 800 ~ 1000 kg/m
3, ultimate compression strength: 5 ~ 13 MPa; Thermal conductivity: 0.1 ~ 0.2 W/ (mK).
(2) the at high temperature volatilization in microwave thermal treating processes of the reductive agent in the present invention, reductive agent, in reduced chromium slag, also plays the effect of pore-forming material; When high temperature burns till, in product, form micropore, thereby the product obtaining has light porous feature.
Reaction principle: utilize C in reductive agent and the CaCrO in chromium slag
4under microwave high-temperature sintering, react, after reaction, chromium slag is reduced removing toxic substances.Principal reaction formula is as follows:
3C(s) + 2CaCrO
4 (s) = 2CaO (s) + Cr
2 O
3 (s)+ 3CO(g) ①
3CO (g) + 2CaCrO
4 (s) = 2CaO (s) + Cr
2O
3 (s)+ 3CO
2 (g) ②
C(s) + CO
2 (g) = 2CO(g) ③
C in reaction mainly comes from reductive agent as glucose, and the fusing point of glucose is 146 ℃, starts to decompose when melting.Along with temperature raises, glucose is constantly carrying out carbonization process, and the gas phase small molecules of generation is overflowed in carbonization, at carbon surface, takes the lead in producing one deck CO air film.Because glucose is to mix with chromium slag with the form of the aqueous solution, it is very even that reductive agent mixes with chromium slag, and be combined closely with chromium slag, can accelerate like this reaction that carbon surface generates CO, is conducive to the carrying out of reduction reaction.
(3) the present invention detoxifies and harmless treatment to chromium slag when producing light wall material, make chromium slag obtain second stage employ, can turn waste into wealth, energy-conserving and environment-protective, greatly reduce the pollution and harm of chromium slag to environment, realized the comprehensive utilization to chromium slag.
(4) the present invention adopts industrial microwave oven to heat in high-temperature sintering process, industrial microwave heating can make material self integral body heat up simultaneously, microwave heating rate of heating is fast, pollution-free, sufficient reacting, and raw material forms vitreum after by microwave high-temperature sintering, and product structure is even; And microwave heating process can accurately be controlled, and reduction efficiency is high, shorten heat-up time, save energy; In microwave field, there is non-thermal effect, reduction reaction is easily carried out, compare with the obvious advantage with other heating means.
(5) in the present invention, materials for wall base substrate becomes crude pottery after oversintering, its inside becomes Solid solution structure, there is no gelling material, this structure can not cause because of the migration of free water in its hole comparatively large vol distortion, can effectively solve in wall crazing, severe cold environment the problems such as freeze injury occur, can extend the body of wall life-span, maintenance cost is lower, safe and reliable, outer decoration can be diversified; This structure need to not reach under the prerequisite of identical energy-saving heat preserving and effect of heat insulation at the tectonic systems such as the nonweight-bearing heat insulating of inside and outside increase of main body walling, has good economic benefit.
Accompanying drawing explanation
The process flow diagram of Fig. 1 light wall material of the present invention;
The SEM image of Fig. 2 light wall material of the present invention under 35 multiplying powers;
The SEM image of Fig. 3 light wall material of the present invention under 200 multiplying powers;
The SEM image of Fig. 4 light wall material of the present invention under 2000 multiplying powers;
The SEM image of Fig. 5 light wall material of the present invention under 3000 multiplying powers.
Scale in Fig. 2～Fig. 5 is respectively 500 μ m, 100 μ m, 10 μ m, 5 μ m.
Embodiment
Embodiment 1: a kind of method of preparing light wall material with microwave thermal processing chromium slag, comprises the following steps:
1) measure respectively 55Kg chromium slag, 30Kg flyash, 15Kg albite, pulverize, then together add in mixer and mix, obtain admixtion;
2) weight ratio of pressing chromium slag 5% weighs glucose, to adding water in glucose, is made into the aqueous solution, and amount of water is 4 times of glucose weight; This aqueous solution is joined in above-mentioned admixtion, in mixer, mix and obtain compound;
3) compound is added in mould, through vibrations hydropress, under 5MPa pressure, be pressed into adobe;
4) will after brick bat drying, send in the industrial microwave oven of power 30KW, industrial microwave oven is warming up to 1100 ℃ with the temperature rise rate of 15 ℃ of per minutes and carries out high temperature sintering, and is incubated 30min at this temperature, obtains light wall material of the present invention.
Technical target of the product: density 820 kg/m
3, ultimate compression strength 6.5 MPa, thermal conductivity 0.12 W/ (mK).
Embodiment 2: a kind of method of preparing light wall material with microwave thermal processing chromium slag, comprises the following steps:
1) 60Kg chromium slag, 20Kg flyash, 20Kg albite are pulverized, then together added in mixer and mix, obtain admixtion;
2) weight ratio of pressing chromium slag 8% weighs sucrose, to adding water in sucrose, is made into the aqueous solution, and amount of water is 3 times of sucrose weight; This aqueous solution is joined in above-mentioned admixtion, in mixer, mix and obtain compound;
3) compound is added in mould, on 15MPa vibrations hydropress, be pressed into adobe;
4) will after brick bat drying, send in the industrial microwave oven that power is 40KW, microwave oven is warming up to 950 ℃ with the speed of 10 ℃ of per minutes, is incubated 35min and carries out high temperature sintering at this temperature, obtains light wall material of the present invention.
The technical indicator of product: density 990kg/m
3, ultimate compression strength 7.6 MPa, thermal conductivity 0.16 W/ (mK).
Embodiment 3: a kind of method of preparing light wall material with microwave thermal processing chromium slag, comprises the following steps:
1) 60Kg chromium slag, 25Kg flyash, 15Kg albite in powder are broken into the particulate material that granularity is 0.074-0.3mm; Above-mentioned raw materials is together added in mixer and mixed, obtain admixtion;
2) weight ratio of pressing chromium slag 7% weighs citric acid, to adding water in citric acid, is made into the aqueous solution, and amount of water is 2 times of citric acid weight; This aqueous solution is joined in above-mentioned admixtion, in mixer, mix and obtain compound;
3) compound is added in mould, on 8MPa vibrations hydropress, be pressed into light wall material base substrate;
4) by sending into power after body drying, be that the industrial microwave oven of 60KW carries out high temperature sintering, industrial microwave oven is warming up to 1000 ℃ with the speed of 8 ℃ of per minutes, and keeps 25min at this temperature, obtains light wall material of the present invention.
The technical indicator of product: density 980 kg/m
3, pressure resistance 8.2 MPa, thermal conductivity 0.13 W/ (mK).
Embodiment 4: a kind of method of preparing light wall material with microwave thermal processing chromium slag, comprises the following steps:
1) 65Kg chromium slag, 20Kg flyash, 15Kg albite are pulverized, together added in mixer and mix, obtain admixtion; After pulverizing, the granularity of chromium slag, flyash, albite is 0.074-0.3mm;
2) weight ratio of pressing chromium slag 10% weighs oxalic acid, to adding water in oxalic acid, is made into the aqueous solution, and amount of water is 2.5 times of oxalic acid weight; This aqueous solution is joined in above-mentioned admixtion, in mixer, mix and obtain compound;
3) compound is added in mould, on 20MPa vibrations hydropress, be pressed into adobe;
4) by sending into industrial microwave oven after brick bat drying, carry out high temperature sintering, industrial microwave oven is warming up to 1100 ℃ with the speed of 5 ℃ of per minutes, and is incubated 30min at this temperature, obtains light wall material of the present invention.
Technical target of the product: density 880 kg/m
3, ultimate compression strength 12.9 MPa, thermal conductivity 0.189 W/ (mK).
Embodiment 5: a kind of method of preparing light wall material with microwave thermal processing chromium slag, comprises the following steps:
1) 55Kg chromium slag, 20Kg flyash, 25Kg albite in powder being broken into granularity is 0.074-0.3mm particulate material, then together adds in mixer and mixes, and obtains admixtion;
2) by the weight ratio of chromium slag 5%, weigh respectively sucrose and citric acid, sucrose, citric acid are mixed, add wherein the water of 2 times of the two gross weights, obtain the mixed solution of sucrose, citric acid; This mixed solution and above-mentioned admixtion are mixed, then in mixer, mix and obtain compound;
3) compound is added in mould, on 12MPa vibrations hydropress, be pressed into adobe;
4) by sending into industrial microwave oven after brick bat drying, carry out high temperature sintering, microwave oven is warming up to 1050 ℃ with the speed of 12 ℃ of per minutes, and is incubated 20min at this temperature, obtains light wall material of the present invention.
Technical target of the product: density 950 kg/m
3, ultimate compression strength 10.4 MPa, thermal conductivity 0.152 W/ (mK).
Embodiment 6: a kind of method of preparing light wall material with microwave thermal processing chromium slag, comprises the following steps:
1) 55Kg chromium slag, 20Kg flyash, 25Kg albite are pulverized, then together added in mixer and mix, obtain admixtion; After wherein pulverizing, the granularity of chromium slag, flyash, albite is 0.074-0.3mm;
2) in the ratio of above-mentioned chromium slag weight 4%, 3%, weigh respectively glucose and oxalic acid; Glucose and oxalic acid are mixed, add wherein the water of 3 times of the two gross weights, after dissolving, obtain glucose, careless aqueous acid; This aqueous solution and above-mentioned admixtion are mixed in mixer, obtain compound;
3) compound is added in mould, on 6MPa vibrations hydropress, be pressed into adobe;
4) by sending into industrial microwave oven after brick bat drying, carry out high temperature sintering, industrial microwave oven is warming up to 1050 ℃ with the speed of 12 ℃ of per minutes, and is incubated 20min at this temperature, obtains light wall material of the present invention.
The technical indicator of product: density 960 kg/m
3, ultimate compression strength 7.1MPa, thermal conductivity 0.11 W/ (mK).
Claims (4)
1. microwave thermal is processed the method that chromium slag is prepared light wall material, it is characterized in that: the method comprises the following steps:
1) chromium slag, flyash, albite are measured respectively by the weight ratio of 55-65%, 20-30%, 15-25%, and pulverize;
2) chromium slag, flyash and albite are together added in mixer, mix, obtain admixtion;
3) weight ratio of pressing chromium slag 5-10% weighs reductive agent, to adding water in reductive agent, is made into the aqueous solution, amount of water be reductive agent weight 2-4 doubly; This aqueous solution is mixed and obtains compound with described admixtion, then compound is pressed into adobe; Described reductive agent is one or more the mixture in glucose, sucrose, oxalic acid and citric acid;
4) by sending into industrial microwave oven after brick bat drying, through microwave high-temperature sintering, obtain light wall material.
2. microwave thermal is processed the method that chromium slag is prepared light wall material according to claim 1, it is characterized in that: the power of described industrial microwave oven is 30-60kW, temperature rise rate during microwave high-temperature sintering is per minute 5-15 ℃, is warming up to 900-1100 ℃, and is incubated 15-35min at this temperature.
3. microwave thermal is processed the method that chromium slag is prepared light wall material according to claim 1, it is characterized in that: the granularity of the chromium slag of described pulverizing, flyash, albite is 0.074-0.3mm.
4. according to microwave thermal described in claim 1-3 any one, process the method that chromium slag is prepared light wall material, it is characterized in that: pressure during described pressing unfired brick is 5-20MPa.
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| CN107353034A (en) * | 2017-07-27 | 2017-11-17 | 武汉理工大学 | A kind of method for preparing haydite using microwave sintering curing heavy metal chromium |
| CN114394845B (en) * | 2022-01-12 | 2023-08-15 | 湖南国发控股有限公司 | High-chromium slag amount sintering formula and synergistic foaming ceramic production process |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1410393A (en) * | 2002-11-21 | 2003-04-16 | 上海交通大学 | Preparation method of special foamed ceramic filter for magnesium alloy |
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| CN1410393A (en) * | 2002-11-21 | 2003-04-16 | 上海交通大学 | Preparation method of special foamed ceramic filter for magnesium alloy |
Non-Patent Citations (4)
| Title |
|---|
| 叶昌 等.高掺量工业废渣建筑陶瓷锦砖的研制.《中国陶瓷工业》.2010,第17卷(第3期),第1-4页. |
| 微波技术在含铬废渣解毒中的应用;李晓红 等;《压电与声光》;20040831;第26卷(第4期);第334-336页 * |
| 李晓红 等.微波技术在含铬废渣解毒中的应用.《压电与声光》.2004,第26卷(第4期),第334-336页. |
| 高掺量工业废渣建筑陶瓷锦砖的研制;叶昌 等;《中国陶瓷工业》;20100630;第17卷(第3期);第1-4页 * |
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