CN107285350A - A kind of method that hydrochloric acid leaching flyash extracts aluminum and coproducing white carbon - Google Patents
A kind of method that hydrochloric acid leaching flyash extracts aluminum and coproducing white carbon Download PDFInfo
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- CN107285350A CN107285350A CN201710718099.2A CN201710718099A CN107285350A CN 107285350 A CN107285350 A CN 107285350A CN 201710718099 A CN201710718099 A CN 201710718099A CN 107285350 A CN107285350 A CN 107285350A
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- white carbon
- hydrochloric acid
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- aluminum
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- 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
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/20—Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts
- C01F7/22—Preparation of aluminium oxide or hydroxide from aluminous ores using acids or salts with halides or halogen acids
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- 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
- 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
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- Life Sciences & Earth Sciences (AREA)
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Abstract
The invention discloses a kind of method that hydrochloric acid leaching flyash extracts aluminum and coproducing white carbon, white carbon black technique is prepared with flyash extraction carry out coproduction using the alumina technology in hydrochloric acid method extraction flyash, not only aluminium chloride crystal can be separated out with one-step method crystallization, remaining leaching liquid in aluminium chloride crystal preparation technology is recycled simultaneously, white carbon black product can be prepared by sol-gal process, not only greatly save the energy and realize waste reclamation, avoid white carbon preparation technology in the prior art complicated, need additionally to add dispersant and surfactant, the problems such as course of reaction can release sulfuric acid flue gas influence environment, remaining solution other impurities ion (sodium after white carbon is extracted simultaneously, potassium, magnesium, calcium etc.) defect that removes is not required to the complicated impurity removal process such as resin adsorption and can be achieved to reclaim or separate.
Description
Technical field
Join the invention belongs to flyash higher value application field, more particularly to a kind of HCl treatment coal ash for manufacturing for aluminum oxide
Produce the device of white carbon.
Background technology
In recent years, the drastically increasing of solid waste coal ash discharge capacity is brought while China's coal electricity industry is developed rapidly
Plus, the current more than one hundred million tons of China's flyash annual emissions, total volume of cargo in storage of China's flyash has more than ten00000000 tons.The row of a large amount of flyash
Put and not only occupy a large amount of soils, and severe contamination environment, constitute the dual destruction to ecological and environment.Therefore fine coal is carried out
The comprehensive utilization of ash has Great significance and long-range strategic importance.Equally, China is the not rich country of a bauxite resource,
According to the waste in growth rate and the bauxite exploitation of current aluminum oxide yield, utilization, even if in view of prospective reserves, China
The time limit of bauxite also be difficult to reach 50 years.So, solving the method for this crisis of resource has two kinds：One is reasonable utilize now
There is bauxite resource；Two be actively to look for and contain bauxite resource using other.And aluminum oxide is one of main component of flyash, its
Mass fraction is generally 15%~40%, reaches as high as 58%.So, in bauxite resource increasingly poor today, from fine coal
It is the effective way for making flyash turn waste into wealth, comprehensively utilizing that aluminum oxide is extracted in ash, with good social benefit and economy
Benefit.
At present, domestic and international treated coal ash is broadly divided into alkaline process and acid system.The research of aluminum oxide is extracted from flyash
Comparative maturity has limestone sintering process and soda lime sintering process, and both are commonly referred to as alkaline process for this.But oxygen in alkalinity extraction flyash
Change aluminium there is also some problems, the calcium silicate slag that mainly 1. sintering process is produced can only be used as cement raw material, often produce 1 ton of oxygen
The calcium silicate slag for being several times as much as flyash will be produced by changing aluminium, and cement has it to sell radius accordingly, if locality is without large-scale water
Bricklayer's's industry supports that secondary pollution will be caused；2. sintering process is only extracted the aluminum oxide in flyash, the utilization of its silica
Value is low.3. the equipment investment of sintering process treated coal ash is big, high energy consumption, and cost is high.
Compared with alkaline process, acid treatment flyash has obvious advantage.Hydrochloric acid method extracts the master of the aluminum oxide in flyash
It is exactly sour molten, slag-liquid separation, liquor alumini chloridi edulcoration purification, aluminum chloride crystals and calcining to want step.The acid system work of prior art
Skill level of residue is small, while aluminum oxide is effectively extracted, can obtain silicon product, further can be made into white carbon after processing and goes out
Sell.White carbon is a kind of especially excellent functional material, and it has and its extensive purposes.It is in synthetic rubber as excellent
Reinforcing agent, served as in promising coating industry and opacifier and help precipitating reagent, in industries such as fire-fighting, pharmacy and ink
In can serve as dispersant and carrier etc., with China industry grow continuously and fast, the demand of the various raw materials of industry is increasingly high
Rise, the production requirement of white carbon is also growing day by day, and with the emergence of new energy industry, white carbon is also obtained in association area
Universal attention and favor.As patent CN200610012780.7 is disclosed in the technique of existing flyash leaching production white carbon
White carbon preparation technology be that the flyash after activation and ammonium sulfate mix occur to add hydrogen in solid phase reaction, filter residue
Sodium hydroxide solution obtains high-modulus sodium silicate liquid, dispersant and surfactant is then added in waterglass, and add sulphur
Acid adjustment pH value, obtains precipitation of silica (white carbon).But the preparation technology of this patent white carbon is complicated, it is necessary to which extra add
Dispersant and surfactant, and course of reaction can release sulfuric acid flue gas, influence environment.
The content of the invention
In order to overcome above-mentioned deficiency, aluminum and coproducing is extracted it is an object of the invention to provide a kind of hydrochloric acid leaching flyash white
The method of carbon black,
To achieve these goals, the present invention is adopted the following technical scheme that：
A kind of method that hydrochloric acid leaching flyash extracts aluminum and coproducing white carbon, comprises the following steps：
(1) aluminum oxide in dissolution ash is reacted under high alumina active fly ash and mixed in hydrochloric acid, certain temperature.
(2) step (1) reaction obtains slurries and forms leaching liquid and high silicon leach residue after sedimentation, washing and filtering,
Leaching liquid is used to extract crystal aluminum chloride, and leach residue is used to prepare white carbon.
(3) leach residue for obtaining step (2) carries out causticizing reaction with aqua calcis and obtains the calcium silicates aqueous solution.
(4) dry hydrogen chloride gas is passed through in the leaching liquid for obtaining step (2), makes the aluminum chloride crystals in leaching liquid
Form Aluminum Chloride Hexahydrate crystal and separate out, thick aluminium chloride and Liquid Residue are obtained through separation of solid and liquid；
(5) the calcium silicates aqueous solution obtained to step (3) adds polyethylene glycol (PEG), heating stirring；Reach assigned temperature
Afterwards, fast drop step (4) Liquid Residue, the pH value of regulation system is less than 1, and quantitative concentrated ammonia liquor is added dropwise, and regulation pH value is increased to 6
~7；A certain amount of step (4) Liquid Residue is rapidly added again, regulation pH value is less than 1, filtered, then clean neutral to pH with distilled water,
Obtain white carbon black product.
The alumina technology that the present invention is extracted in flyash using hydrochloric acid method prepares white carbon black technique with flyash extraction and entered
Row coproduction, not only can separate out aluminium chloride crystal, while by remaining leaching in aluminium chloride crystal preparation technology with one-step method crystallization
Liquid is recycled, and white carbon black product can be prepared by sol-gal process, is not only greatlyd save the energy and is realized waste
Recycle, while it is complicated, it is necessary to additionally add dispersant and surface-active to avoid white carbon preparation technology in the prior art
Agent, the problems such as course of reaction can release sulfuric acid flue gas influence environment, remaining solution other impurities ion after white carbon is extracted
The defect that (sodium, potassium, magnesium, calcium etc.) is removed is not required to the complicated impurity removal process such as resin adsorption and can be achieved to reclaim or separate.
It is preferred that, causticizing reaction temperature is 110-130 DEG C in step (3), preferably 120 DEG C.
It is preferred that, calcium silicates concentration of aqueous solution is 25-30wt% in step (3).
It is preferred that, the concentration of hydrochloric acid is 10-40wt%, preferably 35wt% in Liquid Residue in step (4).
It is preferred that, reaction temperature is 80 DEG C in step (4), and the content of Surfactant PEG is 8-12%.
It is preferred that, fast drop Liquid Residue in step (4), the pH value of regulation system is less than 1, reaction time 2h-5h.
It is preferred that, calcination after white carbon is fully dried in step (5), calcination temperature is 800-900 DEG C, reaction time
2.5-3h。
It is preferred that, the hydrogen chloride and water vapour that thick aluminium chloride calcining is produced can be passed directly into Liquid Residue and be made for step (5)
Standby white carbon.
White carbon prepared by the above method is also the protection domain of this patent.
The present invention compared with prior art, has the following advantages that：
(1) present invention prepares white carbon black technique using the alumina technology in hydrochloric acid method extraction flyash with flyash extraction
Coproduction is carried out, not only aluminium chloride crystal can be separated out with one-step method crystallization, while by remaining leaching in aluminium chloride crystal preparation technology
Take liquid to be recycled, white carbon black product can be prepared by sol-gal process, not only greatly save energy realization useless
Thing is recycled.
(2) white carbon preparation technology of the present invention avoid white carbon preparation technology in the prior art it is complicated, it is necessary to it is extra plus
Enter dispersant and surfactant, the problems such as course of reaction can release sulfuric acid flue gas influence environment.
(3) the white carbon defect that remaining solution other impurities ion (sodium, potassium, magnesium, calcium etc.) removes after extracting is not required to tree
The complicated impurity removal process such as fat absorption are that can be achieved to reclaim or separate.
(4) alumina technology that hydrochloric acid method of the invention is extracted in flyash prepares white carbon black technique with flyash extraction and entered
Row coproduction, the hydrogen chloride gas that aluminum oxide calcining is produced can be reclaimed directly for white carbon preparation technology, substantial amounts of saving hard charcoal
The cost of black preparation technology and the consumption of hydrochloric acid solution.
Brief description of the drawings
The Figure of description for constituting the part of the application is used for providing further understanding of the present application, and the application's shows
Meaning property embodiment and its illustrate be used for explain the application, do not constitute the improper restriction to the application.
The hydrochloric acid leaching flyash of Fig. 1 present invention extracts the production technology journey figure of aluminum and coproducing white carbon.
Embodiment
It is noted that described further below is all exemplary, it is intended to provide further instruction to the application.Unless another
Indicate, all technologies used herein and scientific terminology are with usual with the application person of an ordinary skill in the technical field
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe embodiment, and be not intended to restricted root
According to the illustrative embodiments of the application.As used herein, unless the context clearly indicates otherwise, otherwise singulative
It is also intended to include plural form, additionally, it should be understood that, when in this manual using term "comprising" and/or " bag
Include " when, it indicates existing characteristics, step, operation, device, component and/or combinations thereof.
The present invention is further described with reference to the accompanying drawings and examples, in order to the understanding of technical staff of the same trade：
Flyash composition used of the invention is as shown in table 1：
| SiO2 | Al2O3 | Fe2O3 | TiO2 | K2O | Na2O | CaO | MgO | FeO | LOI |
| 33.62 | 49.35 | 1.90 | 2.48 | 0.28 | 0.03 | 2.10 | 0.22 | 0.14 | 3.62 |
Table 1
Embodiment 1：
A kind of method that hydrochloric acid leaching flyash extracts aluminum and coproducing white carbon, comprises the following steps：
(1) aluminum oxide in dissolution ash is reacted under high alumina active fly ash and mixed in hydrochloric acid, certain temperature；
(2) step (1) reaction obtains slurries and forms leaching liquid and high silicon leach residue after sedimentation, washing and filtering,
Leaching liquid is used to extract crystal aluminum chloride, and leach residue is used to prepare white carbon.
(3) leach residue for obtaining step (2) carries out causticizing reaction at 110 DEG C with aqua calcis and obtains calcium silicates
The aqueous solution, calcium silicates concentration of aqueous solution is 25wt%；
(4) dry hydrogen chloride gas is passed through in the leaching liquid for obtaining step (2), makes the aluminum chloride crystals in leaching liquid
Form Aluminum Chloride Hexahydrate crystal and separate out, thick aluminium chloride and Liquid Residue are obtained through separation of solid and liquid；The concentration of Liquid Residue hydrochloric acid is
25wt%；
(5) the calcium silicates aqueous solution obtained to step (3) adds polyethylene glycol (PEG), and the content of Surfactant PEG is
8%, heating stirring is to 80 DEG C；Reach after assigned temperature, fast drop step (4) Liquid Residue, the chlorine that thick aluminium chloride calcining is produced
Liquid Residue can be passed directly into by changing hydrogen and water vapour, and the pH value of regulation system is less than 1, reaction time 2h, quantitative concentrated ammonia liquor is added dropwise,
Regulation pH value is increased to 6~7；It is rapidly added a certain amount of step (4) Liquid Residue again, regulation pH value is less than 1, filtering, then with distilling
Water cleans neutral to pH, obtains white carbon black product；Calcination after white carbon is fully dried, calcination temperature is 800 DEG C, reaction time
2.5h。
Embodiment 2
A kind of method that hydrochloric acid leaching flyash extracts aluminum and coproducing white carbon, comprises the following steps：
(1) aluminum oxide in dissolution ash is reacted under high alumina active fly ash and mixed in hydrochloric acid, certain temperature；
(2) step (1) reaction obtains slurries and forms leaching liquid and high silicon leach residue after sedimentation, washing and filtering,
Leaching liquid is used to extract crystal aluminum chloride, and leach residue is used to prepare white carbon.
(3) leach residue for obtaining step (2) carries out causticizing reaction at 120 DEG C with aqua calcis and obtains calcium silicates
The aqueous solution, calcium silicates concentration of aqueous solution is 30wt%；
(4) dry hydrogen chloride gas is passed through in the leaching liquid for obtaining step (2), makes the aluminum chloride crystals in leaching liquid
Form Aluminum Chloride Hexahydrate crystal and separate out, thick aluminium chloride and Liquid Residue are obtained through separation of solid and liquid；The concentration of Liquid Residue hydrochloric acid is
25wt%；
(5) the calcium silicates aqueous solution obtained to step (3) adds polyethylene glycol (PEG), and the content of Surfactant PEG is
10%, heating stirring is to 80 DEG C；Reach after assigned temperature, fast drop step (4) Liquid Residue, the chlorine that thick aluminium chloride calcining is produced
Liquid Residue can be passed directly into by changing hydrogen and water vapour, and the pH value of regulation system is less than 1, reaction time 3.5h, quantitative dense ammonia is added dropwise
Water, regulation pH value is increased to 6~7；It is rapidly added a certain amount of step (4) Liquid Residue again, regulation pH value is less than 1, filtering, then with steaming
Distilled water cleans neutral to pH, obtains white carbon black product；Calcination after white carbon is fully dried, calcination temperature is 850 DEG C, reaction time
3h。
Embodiment 3
A kind of method that hydrochloric acid leaching flyash extracts aluminum and coproducing white carbon, comprises the following steps：
(1) aluminum oxide in dissolution ash is reacted under high alumina active fly ash and mixed in hydrochloric acid, certain temperature.
(2) step (1) reaction obtains slurries and forms leaching liquid and high silicon leach residue after sedimentation, washing and filtering,
Leaching liquid is used to extract crystal aluminum chloride, and leach residue is used to prepare white carbon.
(3) leach residue for obtaining step (2) carries out causticizing reaction at 130 DEG C with aqua calcis and obtains calcium silicates
The aqueous solution, calcium silicates concentration of aqueous solution is 30wt%；
(4) dry hydrogen chloride gas is passed through in the leaching liquid for obtaining step (2), makes the aluminum chloride crystals in leaching liquid
Form Aluminum Chloride Hexahydrate crystal and separate out, thick aluminium chloride and Liquid Residue are obtained through separation of solid and liquid；The concentration of Liquid Residue hydrochloric acid is
40wt%；
(5) the calcium silicates aqueous solution obtained to step (3) adds polyethylene glycol (PEG), and the content of Surfactant PEG is
12%, heating stirring is to 80 DEG C；Reach after assigned temperature, fast drop step (4) Liquid Residue, the chlorine that thick aluminium chloride calcining is produced
Liquid Residue can be passed directly into by changing hydrogen and water vapour, and the pH value of regulation system is less than 1, reaction time 5h, quantitative concentrated ammonia liquor is added dropwise,
Regulation pH value is increased to 6~7；It is rapidly added a certain amount of step (4) Liquid Residue again, regulation pH value is less than 1, filtering, then with distilling
Water cleans neutral to pH, obtains white carbon black product；Calcination after white carbon is fully dried, calcination temperature is 900 DEG C, reaction time
3h。
The preferred embodiment of the application is the foregoing is only, the application is not limited to, for the skill of this area
For art personnel, the application can have various modifications and variations.It is all within spirit herein and principle, made any repair
Change, equivalent substitution, improvement etc., should be included within the protection domain of the application.
Claims (10)
1. a kind of method that hydrochloric acid leaching flyash extracts aluminum and coproducing white carbon, it is characterised in that comprise the following steps：
(1) aluminum oxide in dissolution ash is reacted under high alumina active fly ash and mixed in hydrochloric acid, certain temperature；
(2) step (1) reaction obtains slurries and leaching liquid and high silicon leach residue, leaching is formed after sedimentation, washing and filtering
Liquid is used to extract crystal aluminum chloride, and leach residue is used to prepare white carbon；
(3) leach residue for obtaining step (2) carries out causticizing reaction with aqua calcis and obtains the calcium silicates aqueous solution；
(4) dry hydrogen chloride gas is passed through in the leaching liquid for obtaining step (2), forms the aluminum chloride crystals in leaching liquid
Aluminum Chloride Hexahydrate crystal is simultaneously separated out, and thick aluminium chloride and Liquid Residue are obtained through separation of solid and liquid；
(5) the calcium silicates aqueous solution obtained to step (3) adds polyethylene glycol (PEG), heating stirring；Reach after assigned temperature,
Fast drop step (4) Liquid Residue, the pH value of regulation system is less than 1, is added dropwise quantitative concentrated ammonia liquor, and regulation pH value is increased to 6~
7；A certain amount of step (4) Liquid Residue is rapidly added again, regulation pH value is less than 1, filtered, then cleans neutral to pH with distilled water, obtain
White carbon black product.
2. the method that hydrochloric acid leaching flyash as claimed in claim 1 extracts aluminum and coproducing white carbon, it is characterised in that institute
It is 110-130 DEG C to state causticizing reaction temperature in step (3).
3. the method that hydrochloric acid leaching flyash as claimed in claim 2 extracts aluminum and coproducing white carbon, it is characterised in that institute
State preferably 120 DEG C.
4. the method that hydrochloric acid leaching flyash as claimed in claim 1 extracts aluminum and coproducing white carbon, it is characterised in that institute
It is 25-30wt% to state calcium silicates concentration of aqueous solution in step (3).
5. the method that hydrochloric acid leaching flyash as claimed in claim 1 extracts aluminum and coproducing white carbon, it is characterised in that institute
The concentration for stating hydrochloric acid in Liquid Residue in step (4) is 10-40wt%, preferably 35wt%.
6. the method that hydrochloric acid leaching flyash as claimed in claim 1 extracts aluminum and coproducing white carbon, it is characterised in that institute
It is 80 DEG C to state reaction temperature in step (4), and the content of Surfactant PEG is 8-12%.
7. the method that hydrochloric acid leaching flyash as claimed in claim 1 extracts aluminum and coproducing white carbon, it is characterised in that institute
Fast drop Liquid Residue in step (4) is stated, the pH value of regulation system is less than 1, reaction time 2h-5h.
8. the method that hydrochloric acid leaching flyash as claimed in claim 1 extracts aluminum and coproducing white carbon, it is characterised in that institute
Calcination after white carbon is fully dried in step (5) is stated, calcination temperature is 800-900 DEG C, reaction time 2.5-3h.
9. the method that hydrochloric acid leaching flyash as claimed in claim 1 extracts aluminum and coproducing white carbon, it is characterised in that institute
Liquid Residue can be passed directly into and prepare white carbon for step (5) by stating the hydrogen chloride and water vapour of thick aluminium chloride calcining generation.
10. the white carbon prepared such as claim 1-9 methods describeds.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113484209A (en) * | 2021-05-24 | 2021-10-08 | 浦林成山（山东）轮胎有限公司 | Method for identifying white carbon black in vulcanized rubber and application thereof |
| CN114314621A (en) * | 2020-09-30 | 2022-04-12 | 中国科学院过程工程研究所 | Method for producing metallurgical-grade aluminum oxide and white carbon black by roasting-free and reinforced acid leaching coal gangue |
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Application publication date: 20171024 |