CN107128930A - The method of comprehensive utilization of flyash - Google Patents
The method of comprehensive utilization of flyash Download PDFInfo
- Publication number
- CN107128930A CN107128930A CN201710370404.3A CN201710370404A CN107128930A CN 107128930 A CN107128930 A CN 107128930A CN 201710370404 A CN201710370404 A CN 201710370404A CN 107128930 A CN107128930 A CN 107128930A
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- China
- Prior art keywords
- flyash
- chloride
- comprehensive utilization
- chlorination
- flotation
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- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/08—Compounds containing halogen
- C01B33/107—Halogenated silanes
- C01B33/1071—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof
- C01B33/10715—Tetrachloride, trichlorosilane or silicochloroform, dichlorosilane, monochlorosilane or mixtures thereof prepared by reacting chlorine with silicon or a silicon-containing material
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/56—Chlorides
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/10—Halides
Abstract
The invention discloses a kind of method of comprehensive utilization of flyash, including step：S1, flyash mixed and pelletizing or briquetting with carbon source, obtain chlorizated raw material；S2, by chlorizated raw material in chlorination 10min~10h at 500 DEG C~1300 DEG C, obtain gaseous state chlorizate and chlorination tailings；The gaseous state chlorizate is condensed to be reclaimed, and obtains the chloride of the chloride, the chloride of silicon and aluminium of iron；S3, chlorination tailings is subjected to flotation after crushing and filtered, obtain charcoal flotation thing, alkali metal/alkaline earth metal chloride waste liquid and flotation tailings；S4, flotation tailings is calcined, obtains silica flour.According to the method for comprehensive utilization of the present invention, the various valuable resources in flyash separation and recovery is subjected to respectively and recycled, have been that the higher value application of flyash opens new approach, the purpose for improving comprehensive resource utilization rate, reducing environmental pollution is reached；And during the comprehensive reutilization of flyash, almost produced without poisonous and harmful waste residue, waste water, environmental friendly, technically reliable.
Description
Technical field
The invention belongs to industrial waste technical field of comprehensive utilization, specifically, it is related to a kind of comprehensive utilization of flyash
Method.
Background technology
Flyash is the dust and bottom slag collected in fire coal boiler fume, and produced in coal-burning power plant's production process
Desulphurization and denitration lime-ash, is mainly derived from the using coal enterprises such as thermal power plant, smeltery, chemical plant.In recent years, the coal-fired electricity of China
Factory's flyash yield is huge and rapid development, and thermal power plant's flyash total emission volumn in 2011 is 4.96 hundred million tons, flyash in 2012
Discharge capacity reaches 5.70 hundred million tons, and 5.78 hundred million tons have been reached by 2014, it is contemplated that total volume of cargo in storage to the year two thousand twenty flyash is up to
More than 30 hundred million tons.The a large amount of of flyash store up the arable land for not only taking up sheet, destruction ecological environment, can also cause a large amount of in flyash
The waste of valuable resource, thus seek suitable processing or very necessary using the method for flyash.But at present, domestic flyash
Utilization ways be mainly used for building materials, build the road, engineering backfill etc., utilization rate is less than 70%, and aluminum oxide therein, titanium dioxide
The valuable resources such as silicon, iron oxide do not play maximum value, low in economic efficiency, therefore develop what Ash Utilization was utilized
The flyash spin-off of new way and preparation high added value is significant.
The content of the invention
, should the invention provides a kind of method of comprehensive utilization of flyash to solve the problem of above-mentioned prior art is present
Method of comprehensive utilization opens new approach for the higher value application of flyash, reaches raising comprehensive resource utilization rate, reduces ring
The purpose of border pollution.
In order to reach foregoing invention purpose, present invention employs following technical scheme：
A kind of method of comprehensive utilization of flyash, including step：
S1, flyash mixed and pelletizing or briquetting with carbon source, obtain chlorizated raw material；
S2, by the chlorizated raw material in chlorination 10min~10h at 500 DEG C~1300 DEG C, obtain gaseous state chlorizate and chlorine
Change tailings；Wherein, the gaseous state chlorizate is condensed reclaims, and obtains chloride, the chlorination of the chloride and aluminium of silicon of iron
Thing；
S3, the chlorination tailings is subjected to flotation after crushing and filtered, obtain charcoal flotation thing, alkali metal/alkaline-earth metal
Chloride waste liquid and flotation tailings；
S4, the flotation tailings is calcined, obtains silica flour.
Further, in the step S1, additive is also included in the chlorizated raw material；Wherein, the additive
The ratio between quality sum of quality and the flyash and the carbon source is no more than 10%.
Further, the additive is selected from sodium carboxymethylcellulose, water soluble starch, pre-gelatinized starch, potassium chloride, chlorine
Change at least one of sodium, diboron trioxide, borax.
Further, the mass ratio of the flyash and the carbon source is 10:4~10:1.
Further, the carbon source in coke, bituminous coal, anthracite, charcoal, activated carbon, graphite, bamboo charcoal at least one
Kind.
Further, in the step S3, during flotation collecting agent used be kerosene or diesel oil, foaming agent be fusel,
At least one of sec-octyl alcohol, No. two oil；Wherein, the consumption of the collecting agent is 500g/t~5000g/t, the foaming agent
Consumption is 20g/t~2000g/t.
Further, in the step S4, sintering temperature during roasting is 1000 DEG C~1300 DEG C, and roasting time is
5min~60min.
Further, in the step S2, chlorinating agent during chlorination is chlorine.
Further, in the step S2, chloridizing unit during chlorination is shaft furnace or rotary kiln.
Further, in the step S2, the specific method for condense recovery by the gaseous state chlorizate is：Will
The gaseous state chlorizate is condensed at 200 DEG C~260 DEG C, obtains the chloride and the first condensing gaseous product of the iron；
The first condensing gaseous product is condensed at 60 DEG C~180 DEG C, the chloride and the second condensing gaseous of the aluminium is obtained
Product；The second condensing gaseous product is condensed below 55 DEG C, the chloride of the silicon is obtained.
Beneficial effects of the present invention：
(1) flyash reacts through carbon thermal chlorination, directly obtains anhydrous gaseous aluminium, iron, the chloride of silicon, later separation
Purifying technique is simple, can efficiently reclaim the resources such as aluminium, iron, silicon in flyash, and be easily achieved itself and chlorination tailings
Separation；
(2) quartz, the chloride of alkali and alkaline earth metal ions and unreacted carbon residue etc. are mainly contained in chlorination tailings,
The separation of quartz mineral and soluble chloride and most of charcoal can be realized by floatation process, an one-step baking is then passed through again
Carbon removal, can obtain the higher quartz sand of purity；
(3) according to the method for comprehensive utilization of the present invention, the wherein process of the comprehensive reutilization of flyash does not almost have
The harmful waste residue of poison, waste water are produced, environmental friendly, technically reliable.
Embodiment
Hereinafter, embodiments of the invention are described in detail in the future.However, it is possible to implement this hair in many different forms
It is bright, and the specific embodiment of the invention that should not be construed as limited to illustrate here.It is opposite there is provided these embodiments be for
The principle and its practical application of the present invention is explained, so that others skilled in the art are it will be appreciated that the present invention's is various
Embodiment and the various modifications for being suitable for specific intended application.
Although it will be appreciated that can be used term " first ", " second " etc. to describe various materials herein, these
Material should not be limited by these terms.These terms are only used for making a distinction a material and another material.
The invention provides a kind of method of comprehensive utilization of flyash, the method for comprehensive utilization can be to each in flyash
Plant valuable resource and carry out sufficiently separation and recycling, be a kind of approach of brand-new flyash higher value application.Should
Method of comprehensive utilization specifically includes following steps：
Step S1：Flyash is mixed and pelletizing or briquetting with carbon source, chlorizated raw material is obtained.
Specifically, the mass ratio of flyash and carbon source is 10:4~10:1, and the carbon source may be selected from coke, bituminous coal,
In anthracite, charcoal, activated carbon, graphite, bamboo charcoal any one or at least two mixing；Carbon source is served follow-up herein
The effect that catalysis and promotion chlorination reaction in chlorination process are carried out, therefore when using many kinds of substance mixing as carbon source,
Usage ratio without specifically controlling each component.
Flyash as a kind of industrial residue and carbon source belong to agglomerate body, coarse grain footpath material, therefore generally require by
Chlorizated raw material carries out the operation such as broken, ball milling, so that each material mixing is more uniformly distributed；Again with modes such as pelletizing or briquettings after mixing
Processing obtains chlorizated raw material, to facilitate the operation in follow-up chlorination process.
Preferably, in order to reduce the degree of the fragmentation procedure of flyash and carbon source before mixing, in chlorizated raw material also
May include additive, i.e., flyash, carbon source and additive be mixed to form chlorizated raw material, in this way, can need not by flyash with
And the particle diameter of carbon source be crushed to it is too small；And the quality of control additive is no more than flyash and the 10% of carbon source gross mass, addition
Agent specifically may be selected from sodium carboxymethylcellulose, water soluble starch, pre-gelatinized starch, potassium chloride, sodium chloride, diboron trioxide, boron
In sand any one or at least two mixing.
Step S2：By chlorizated raw material in chlorination 10min~10h at 500 DEG C~1300 DEG C, gaseous state chlorizate and chlorine are obtained
Change tailings.
Specifically, the general chloridizing unit for using shaft furnace or rotary kiln as chlorizated raw material, and preferably with chlorine
It is used as chlorinating agent；Chlorizated raw material is placed in chlorine atmosphere and carries out chlorination.
More specifically, the condensed chlorination reclaimed, obtain the chloride, silicon of iron of gaseous state chlorizate obtained through chlorination
The chloride of thing and aluminium.Usually, chloride, the chloride of silicon of separation iron can be reached by way of fractional condensation is reclaimed
And the purpose of the chloride of aluminium, referring in particular to following step：(1) gaseous state chlorizate is condensed at 200 DEG C~260 DEG C,
Obtain the chloride and the first condensing gaseous product of iron；(2) the first condensing gaseous product is condensed at 60 DEG C~180 DEG C,
Obtain the chloride and the second condensing gaseous product of aluminium；(3) the second condensing gaseous product is condensed below 55 DEG C, obtains silicon
Chloride.
In this way, be to realize the purpose for being separated and recovered the aluminium in flyash, iron, silicon by step S2, and
During above-mentioned substance is reclaimed, its elder generation escapes in gaseous chloride form, is also convenient for more sufficient with the progress of chlorination tailings
Separation.What deserves to be explained is, it will be appreciated by those skilled in the art that the aluminium, iron, the separation and recovery of silicon in above-mentioned flyash are
A kind of preliminary processing, does not represent all aluminium, iron, silicon and is reclaimed, and not only there was only iron in regenerant yet
The chloride of chloride, the chloride of aluminium or silicon, three is only the main component in regenerant.
Step S3：Chlorination tailings is carried out to flotation after crushing and filtered, charcoal flotation thing, alkali metal/alkaline-earth metal is obtained
Chloride waste liquid and flotation tailings.
Chlorination tailings after crushing, carries out flotation under the double action of collecting agent and foaming agent, obtains charcoal flotation thing,
The alkali metal of mixing/alkaline earth metal chloride waste liquid and flotation tailings are separated by filtering again；In this way, i.e. by charcoal,
Alkali metal/alkaline earth metal chloride waste liquid and flotation tailings are separated, and can carry out recycling to charcoal.
Specifically, collecting agent used during flotation is kerosene or diesel oil, and foaming agent is in fusel, sec-octyl alcohol, No. two oil
At least one；And it is general in order to save reagent and rationally control flotation effect, the consumption for preferably controlling collecting agent is 500g/t
~5000g/t, the consumption of foaming agent is 20g/t~2000g/t, i.e., per ton to treat that flotation material correspondence is caught using 500g~5000g
Receive agent and 20g~2000g foaming agents.
The time of flotation and ore dressing system are specifically determined according to the content of charcoal in correspondence chlorination tailings.
Step S4：Flotation tailings is calcined 5min~60min at 1000 DEG C~1300 DEG C, silica flour is obtained.
Main component is quartz and the carbon residue of the non-floated separation in part in flotation tailings, through high-temperature roasting, this part
Carbon residue is converted into the effusion such as carbon dioxide and drained, and residual components are then silica flour, can be with recycling.
In this way, pass through above-mentioned steps S1-S4, it is valuable to the iron in flyash, aluminium, silicon and charcoal and quartz etc. successively
Resource is able to recycling, and realizing the higher value application of flyash, there is provided the new way that flyash synthetical recovery is recycled
Footpath, has reached the purpose for improving comprehensive resource utilization rate, reducing environmental pollution；At the same time, in the comprehensive utilization side of the present invention
In method, almost produced without poisonous and harmful waste residue, waste water, environmental friendly, technically reliable.
What deserves to be explained is, although in the prior art there is also the method for comprehensive utilization of several flyash, it will be clear that often
A kind of method of comprehensive utilization of flyash is all the overall technical architecture that a kind of some products are combined together, and is a continuous place
Chlorination process in the process of reason, such as step S2, if control condition is unreasonable, then iron therein, aluminium, silicon can not be able to
Rational separation, certainly will influence efficiently separating for follow-up charcoal and quartz etc..
The method of comprehensive utilization of the above-mentioned flyash according to the present invention will be illustrated by specific embodiment below, for convenience
The experiment parameter in each embodiment is contrasted, each embodiment is listed in table form.
In embodiments of the invention 1-3, its used flyash comes from Qinghai end of the bridge Lv electricity limited companies, its
Component is as shown in table 1.
The constituent analysis of flyash in the embodiment 1-3 of table 1
The parameter comparison of the method for comprehensive utilization of the embodiment 1-3 of table 2 flyash
Note：In table 2, " the first ratio " refers to the mass ratio of flyash and carbon source；" the second ratio " refers to additive and powder
The mass ratio of the quality sum of coal ash and carbon source.
In above-mentioned steps S1, after being mixed after flyash is mixed with carbon source or with carbon source and additive, broken
Broken, ball milling, briquetting/pelletizing and drying process.In embodiment 1, flyash mixes and is crushed to a 400 mesh left side correspondence with coke
The right side, then be well mixed in ball mill, the ball milling 5min under 300rpm rotating speed finally carries out briquetting using tablet press machine, obtains
Diameter 1cm, high 1cm agglomerate and the drying acquisition chlorizated raw material at 200 DEG C；In example 2, flyash and bituminous coal, solvable
Property starch mix and be crushed to 400 mesh or so, then in ball mill be well mixed, the ball milling 5min under 400rpm rotating speed, most
Pelletizing is carried out using disc balling machine afterwards, average diameter 1cm pelletizing and the drying acquisition chlorizated raw material at 200 DEG C is obtained；
In embodiment 3, flyash and activated carbon, B2O3Mix and be crushed to 200 mesh or so, then be well mixed in ball mill,
Ball milling 5min under 500rpm rotating speed, finally carries out briquetting using tablet press machine, obtain diameter 0.5cm, high 0.5cm agglomerate and
Drying obtains chlorizated raw material at 200 DEG C.
Step S2 effects in the embodiment 1-3 of table 3
Step S3 effects in the embodiment 1-3 of table 4
Although the present invention has shown and described with reference to specific embodiment, it should be appreciated by those skilled in the art that：
In the case where not departing from the spirit and scope of the present invention limited by claim and its equivalent, can carry out herein form and
Various change in details.
Claims (10)
1. a kind of method of comprehensive utilization of flyash, it is characterised in that including step：
S1, flyash mixed and pelletizing or briquetting with carbon source, obtain chlorizated raw material；
S2, by the chlorizated raw material in chlorination 10min~10h at 500 DEG C~1300 DEG C, obtain gaseous state chlorizate and chlorination tail
Slag；Wherein, the gaseous state chlorizate is condensed reclaims, and obtains the chloride of the chloride, the chloride of silicon and aluminium of iron；
S3, the chlorination tailings is subjected to flotation after crushing and filtered, obtain charcoal flotation thing, alkali metal/alkaline-earth metal chlorination
Thing waste liquid and flotation tailings；
S4, the flotation tailings is calcined, obtains silica flour.
2. method of comprehensive utilization according to claim 1, it is characterised in that in the step S1, the chlorizated raw material
In also include additive；Wherein, the ratio between the quality of the additive and the flyash and quality sum of the carbon source do not surpass
Cross 10%.
3. method of comprehensive utilization according to claim 2, it is characterised in that the suppression breaks additive and is selected from carboxymethyl cellulose
At least one of plain sodium, water soluble starch, pre-gelatinized starch, potassium chloride, sodium chloride, diboron trioxide, borax.
4. according to any described method of comprehensive utilization of claim 1-3, it is characterised in that the flyash and the carbon source
Mass ratio is 10:4~10:1.
5. method of comprehensive utilization according to claim 4, it is characterised in that the carbon source is selected from coke, bituminous coal, smokeless
At least one of coal, charcoal, activated carbon, graphite, bamboo charcoal.
6. method of comprehensive utilization according to claim 4, it is characterised in that used during flotation in the step S3
Collecting agent is kerosene or diesel oil, and foaming agent is at least one of fusel, sec-octyl alcohol, No. two oil；Wherein, the use of the collecting agent
Measure as 500g/t~5000g/t, the consumption of the foaming agent is 20g/t~2000g/t.
7. method of comprehensive utilization according to claim 4, it is characterised in that in the step S4, roasting during roasting
Temperature is 1000 DEG C~1300 DEG C, and roasting time is 5min~60min.
8. according to any described method of comprehensive utilization of claim 1-3, it is characterised in that in the step S2, during chlorination
Chlorinating agent be chlorine.
9. method of comprehensive utilization according to claim 8, it is characterised in that in the step S2, chlorination during chlorination
Device is shaft furnace or rotary kiln.
10., will be described according to any described method of comprehensive utilization of claim 1-3, it is characterised in that in the step S2
Gaseous state chlorizate carry out condensation recovery specific method be：
The gaseous state chlorizate is condensed at 200 DEG C~260 DEG C, the chloride and the first condensing gaseous of the iron is obtained
Product；
The first condensing gaseous product is condensed at 60 DEG C~180 DEG C, chloride and the second condensation of the aluminium is obtained
Gaseous products；
The second condensing gaseous product is condensed below 55 DEG C, the chloride of the silicon is obtained.
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Cited By (2)
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| CN108906339A (en) * | 2018-09-10 | 2018-11-30 | 贵州大学 | A kind of Floatation of Removal Carbon method of flyash |
| CN114717417A (en) * | 2020-12-21 | 2022-07-08 | 青岛惠城环保科技股份有限公司 | Treatment method of heavy metal-containing silicon-aluminum-based waste residue, amorphous silicon-aluminum powder and application thereof |
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| CN114717417A (en) * | 2020-12-21 | 2022-07-08 | 青岛惠城环保科技股份有限公司 | Treatment method of heavy metal-containing silicon-aluminum-based waste residue, amorphous silicon-aluminum powder and application thereof |
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