CN106365173B - A kind of method that sial slag prepares White Carbon black and water treatment agent - Google Patents
A kind of method that sial slag prepares White Carbon black and water treatment agent Download PDFInfo
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- CN106365173B CN106365173B CN201610744433.7A CN201610744433A CN106365173B CN 106365173 B CN106365173 B CN 106365173B CN 201610744433 A CN201610744433 A CN 201610744433A CN 106365173 B CN106365173 B CN 106365173B
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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
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Inorganic Chemistry (AREA)
- Processing Of Solid Wastes (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Abstract
The invention discloses a kind of method that sial slag prepares White Carbon black and water treatment agent, this method uses sodium carbonate basic roasting sial slag, and through solution leaching separation, leachate is passed through CO after aluminium is separated by extraction2Gas is carbonized, and then separating, washing, drying obtains White Carbon black product；Extraction organic phase is stripped through hydrochloric acid solution, and strip liquor is through evaporating, being concentrated to give aluminium chloride water treatment agent.The method of the present invention technical process and equipment are simple, operation is easy, is safe, it is a kind of processing technology routine using utilization of resources of the trade waste production with chemical products with high added-value, can reach secondary resource comprehensive utilization, realize circular economy, energy-saving and emission-reduction purpose.
Description
Technical field
The invention belongs to solid waste in chemical industry to utilize field, specially be related in industrial water conditioning agent production process
The utilization method of the industrial residue of generation.
Background technology
Sial slag is water process manufacturing enterprise, and polyaluminum sulfate is produced through room temperature pressure leaching using low-grade bauxite
When the water treatment agents such as aluminium, aluminium chloride, the industrial residue of generation is detached, appearance is canescence, and the main component of the waste residue is SiO2
And aluminium, wherein SiO2Content 80~85%, Al2O3Content 15~18%, SiO2And Al2O3Account for 95% or more.Sial slag is as water process
The waste residue that manufacturing enterprise generates mainly is handled using air storage at present, due to containing the valuable elements such as a large amount of silicon, aluminium in slag
And some other harmful element, stacking processing not only waste of resource, but also meeting land occupation, pollution environment influence the ecological balance,
With great potential risk.
The purpose of the present invention is exactly to develop the processing method of a sial slag, is extracted by this method valuable in sial slag
Elemental silicon and aluminium prepare the precipitation SiO with high added value2Product and aluminium chloride water treatment agent are the utilization of sial slag
One effective approach is provided, harm of the sial slag to environment is reduced.
Invention content
The purpose of the present invention is to provide a kind of utilization method of sial slag, this method is utilized by handling industrial residue
The valuable element contained in slag produces the chemical products with high added value, can reach secondary resource recycling, realizes cycle
Economy, energy-saving and emission-reduction purpose.
The present invention is realized using the following steps：
A, in sial slag: the ratio that sodium carbonate mass ratio is 1: 1.0~1.2 weighs a certain amount of two kinds of materials, and mixing is equal
It is contained in pottery and is positioned in high temperature furnace after even, calcined 1~2 hour at a temperature of 600 DEG C~800 DEG C, it is then cold
But to room temperature and be ground to material all by 120 mesh sieve；
B, according to the sial slag amount of step A, in liquid phase: sial slag liquid consolidates the ratio that mass ratio is 3~4: 1, is reacting
Liquid phase that the water that corrresponding quality is added in device or the mixed liquor that is returned by step H are prepared with supplement water is simultaneously warming up to 70~90 DEG C,
Then the material after the grinding that step A is obtained is added under agitation, 2~3 are leached under the stirring condition of 400~500rpm
Hour, it is isolated to leachate and leached mud；
C, leachate isolated step B, by organic phase and water phase（Leachate）Volume ratio is 1:1 ratio is added
The carbon tetrachloride organic extractant phase aluminium of 120~150g/L and 3~5g/L diisobutyl carbinol (DIBC) containing 8~oxyquinoline, extraction temperature
Room temperature, mixing speed are 300~500rpm, and extraction time 20~40 minutes is isolated to and extracts organic phase and raffinate containing aluminium
Aqueous solution；
D, in the isolated raffinate aqueous solutions of step C, under the stirring condition of room temperature, normal pressure and 300~500rpm
It is passed through CO2Gas carries out carbonization treatment, and when pH value of solution reaches 8~10, stopping is passed through CO2Gas continues in 300~500rpm
Stirring condition under react 0.5 hour, then isolated filtrate and silicic acid hydrate precipitation；
E, step D is obtained silicic acid hydrate precipitation, washed 2 times with the water of step A sial slags amount 80%~100% and in
Then 120~150 DEG C of dryings 2.0~3.0 hours calcine 0.5~1.0 hour at a temperature of 600~800 DEG C and obtain white carbon
Black product；
F, filtrate isolated step D, through being concentrated by evaporation, crystallizing, isolated sodium carbonate and crystalline mother solution；It obtains
Sodium carbonate is used back to step A for dispensing；
What G, step C was obtained extracts organic phase containing aluminium, with the hydrochloric acid solution of 50~80g/L, by organic phase and water phase body（Salt
Acid solution）The ratio of 2 ︰ 1 of volume ratio is stripped 20~30 minutes at room temperature, after back extraction isolated liquor alumini chloridi and back extraction have
Machine phase；Organic phase return to step C is stripped to recycle；Liquor alumini chloridi is through evaporating, being concentrated to give aluminium chloride water treatment agent；
H, the crystalline mother solution mixing that cleaning solution isolated step E and step F are isolated, return to step B are used.
The sial slag is, by sulfuric acid room temperature pressure leaching, when producing water treatment agent, to be detached using low-grade bauxite
Obtained industrial residue, key component are：SiO2Content 80~85%, Al2O3Content 15~18%, the crystallization water 45~50%.
The present invention has following advantages and effect：
（1）The Si and Al in sial slag can be effectively extracted, an approach efficiently used is provided for sial slag；
（2）The features such as present invention has technical process and equipment simple, and operation is easy, is safe.
Specific implementation mode
Below by embodiment, invention is further described in detail, but the scope of the present invention is not limited in described
Hold.
Embodiment 1：
A, 400 grams of sial slag, 400 grams of sodium carbonate are weighed, two kinds of materials are mounted in pottery and are put after mixing
It is placed in high temperature furnace, is calcined 1 hour at a temperature of 800 DEG C, then cool to room temperature and be ground to material all by 120 mesh
Sieve；
B, 1600 grams of water is added in the reactor and is warming up to 70 DEG C, is then added what step A was obtained under agitation
Material after grinding leaches 2 hours under the stirring condition of 500rpm, is isolated to leachate and leached mud；
C, leachate isolated step B, by organic phase and water phase volume ratio 1:1, it is added and contains 8~oxyquinoline
The carbon tetrachloride organic extractant phase aluminium of 150g/L and 3g/L diisobutyl carbinol (DIBC)s, extraction temperature room temperature, mixing speed 300rpm,
Extraction time 40 minutes is isolated to and extracts organic phase and raffinate aqueous solution containing aluminium；
D, it in the isolated raffinate aqueous solutions of step C, is passed through under the stirring condition of room temperature, normal pressure and 500rpm
CO2Gas carries out carbonization treatment, and when pH value of solution reaches 10, stopping is passed through CO2Gas continues under the stirring condition of 300rpm
Reaction 0.5 hour, then isolated filtrate and silicic acid hydrate precipitate；
E, step D is obtained silicic acid hydrate precipitation, it is with 400 grams of water washings 2 times and 2.0 hours dry in 150 DEG C, then
It is calcined at a temperature of 600 DEG C 1.0 hours and obtains White Carbon black product；
F, filtrate isolated step D, through being concentrated by evaporation, crystallizing, isolated sodium carbonate and crystalline mother solution；
What G, step C was obtained extracts organic phase containing aluminium, with the hydrochloric acid solution of 50g/L, by organic phase and water phase body volume ratio
2 ︰ 1 are stripped 30 minutes at room temperature, after back extraction isolated liquor alumini chloridi and back extraction organic phase, liquor alumini chloridi through evaporation,
It is concentrated to give aluminium chloride water treatment agent；
H, the crystalline mother solution mixing that cleaning solution isolated step E and step F are isolated.
Through analysis, White Carbon black product SiO2Content is 96.47%, and appearance is white, specific surface area 90m3/g。
Embodiment 2：
A, 400 grams of sial slag, 480 grams of sodium carbonate are weighed, two kinds of materials are mounted in pottery and are put after mixing
It is placed in high temperature furnace, is calcined 2 hours at a temperature of 600 DEG C, then cool to room temperature and be ground to material all by 120 mesh
Sieve；
B, 1200 grams of water is added in the reactor and is warming up to 90 DEG C, is then added what step A obtained under agitation
Material after grinding leaches 3 hours under the stirring condition of 400rpm, is isolated to leachate and leached mud；
C, leachate isolated step B, by organic phase and water phase volume ratio 1:1, it is added and contains 8~oxyquinoline
The carbon tetrachloride organic extractant phase aluminium of 120g/L and 5g/L diisobutyl carbinol (DIBC)s, extraction temperature room temperature, mixing speed 500rpm,
Extraction time 20 minutes is isolated to and extracts organic phase and raffinate aqueous solution containing aluminium；
D, it in the isolated raffinate aqueous solutions of step C, is passed through under the stirring condition of room temperature, normal pressure and 300rpm
CO2Gas carries out carbonization treatment, and when pH value of solution reaches 8, stopping is passed through CO2Gas continues anti-under the stirring condition of 500rpm
It answers 0.5 hour, then isolated filtrate and silicic acid hydrate precipitate；
E, step D is obtained silicic acid hydrate precipitation, it is with 320 grams of water washings 2 times and 3.0 hours dry in 120 DEG C, then
It is calcined at a temperature of 800 DEG C 0.5 hour and obtains White Carbon black product；
F, filtrate isolated step D, through being concentrated by evaporation, crystallizing, isolated sodium carbonate and crystalline mother solution；
What G, step C was obtained extracts organic phase containing aluminium, with the hydrochloric acid solution of 80g/L, by organic phase and water phase body volume ratio
2 ︰ 1 are stripped 20 minutes at room temperature, after back extraction isolated liquor alumini chloridi and back extraction organic phase, liquor alumini chloridi through evaporation,
It is concentrated to give aluminium chloride water treatment agent；
H, the crystalline mother solution mixing that cleaning solution isolated step E and step F are isolated.
Through analysis, White Carbon black product SiO2Content is 95.83%, and appearance is white, and specific surface area is 92 m3/g。
Embodiment 3：
A, 400 grams of sial slag is weighed, the obtained sodium carbonate of 1 step F of embodiment and 2 step F of embodiment is mixed and takes 440
Gram, two kinds of materials are mounted in pottery after mixing and are positioned in high temperature furnace, 1.5 are calcined at a temperature of 700 DEG C
Hour, it then cools to room temperature and is ground to material and all sieved by 120 mesh；
B, 1 step H of embodiment and 2 step H of embodiment are obtained mixed liquor to remix and take 1500 grams, is added to reactor
In and be warming up to 80 DEG C, the material after the obtained grinding of step A is then added under agitation, in the stirring condition of 450rpm
Lower leaching 2.5 hours, is isolated to leachate and leached mud；
C, leachate isolated step B, by organic phase and water phase volume ratio 1:1, it is added and contains 8~oxyquinoline
The carbon tetrachloride organic extractant phase aluminium of 140g/L and 4g/L diisobutyl carbinol (DIBC)s, extraction temperature room temperature, mixing speed 400rpm,
Extraction time 30 minutes is isolated to and extracts organic phase and raffinate aqueous solution containing aluminium；
D, it in the isolated raffinate aqueous solutions of step C, is passed through under the stirring condition of room temperature, normal pressure and 400rpm
CO2Gas carries out carbonization treatment, and when pH value of solution reaches 9, stopping is passed through CO2Gas continues anti-under the stirring condition of 400rpm
It answers 0.5 hour, then isolated filtrate and silicic acid hydrate precipitate；
E, step D is obtained silicic acid hydrate precipitation, it is with 360 grams of water washings 2 times and 2.5 hours dry in 135 DEG C, then
It is calcined at a temperature of 700 DEG C 0.75 hour and obtains White Carbon black product；
F, filtrate isolated step D, through being concentrated by evaporation, crystallizing, isolated sodium carbonate and crystalline mother solution；
What G, step C was obtained extracts organic phase containing aluminium, with the hydrochloric acid solution of 65g/L, by organic phase and water phase body volume ratio
2 ︰ 1 are stripped 30 minutes at room temperature, after back extraction isolated liquor alumini chloridi and back extraction organic phase, liquor alumini chloridi through evaporation,
It is concentrated to give aluminium chloride water treatment agent；
H, the crystalline mother solution mixing that cleaning solution isolated step E and step F are isolated.
Through analysis, White Carbon black product SiO2Content is 96.32%, and appearance is white, and specific surface area is 87 m3/g。
Claims (1)
1. a kind of method that sial slag prepares White Carbon black and water treatment agent, it is characterised in that pass through the following steps：
A, in sial slag: the ratio that sodium carbonate mass ratio is 1: 1.0~1.2 weighs two kinds of materials, is contained in ceramics after mixing
It in vessel and is positioned in high temperature furnace, is calcined 1~2 hour at a temperature of 600 DEG C~800 DEG C, then cool to room temperature and grind
Material is milled to all to sieve by 120 mesh；
B, according to the sial slag amount of step A, in liquid phase: sial slag liquid consolidates the ratio that mass ratio is 3~4: 1, in the reactor
The liquid phase that water or the mixed liquor returned by step H are prepared with supplement water is added and is warming up to 70~90 DEG C, then in stirring condition
Material after the grinding that lower addition step A is obtained, leaches 2~3 hours under the stirring condition of 400~500rpm, through detaching
To leachate and leached mud；
C, leachate isolated step B is 1 by organic phase and leachate volume ratio:1 ratio, be added containing 120~
The carbon tetrachloride organic extractant phase aluminium of 8~oxyquinolines of 150g/L and 3~5g/L diisobutyl carbinol (DIBC)s, extraction temperature room temperature are stirred
It is 300~500rpm to mix speed, and extraction time 20~40 minutes is isolated to and extracts organic phase and raffinate aqueous solution containing aluminium；
D, it in the isolated raffinate aqueous solutions of step C, is passed through under the stirring condition of room temperature, normal pressure and 300~500rpm
CO2Gas carries out carbonization treatment, and when pH value of solution reaches 8~10, stopping is passed through CO2Gas continues stirring in 300~500rpm
It is reacted under the conditions of mixing 0.5 hour, then isolated filtrate and silicic acid hydrate precipitate；
E, the silicic acid hydrate precipitation that step D is obtained, 2 times are washed and in 120 with the water of step A sial slags amount 80%~100%
Then~150 DEG C of dryings 2.0~3.0 hours calcine 0.5~1.0 hour at a temperature of 600~800 DEG C and obtain White Carbon black
Product；
F, filtrate isolated step D, through being concentrated by evaporation, crystallizing, isolated sodium carbonate and crystalline mother solution；Obtained carbonic acid
Sodium is used back to step A for dispensing；
What G, step C was obtained extracts organic phase containing aluminium, with the hydrochloric acid solution of 50~80g/L, by organic phase and water phase body volume ratio
The ratio of 2 ︰ 1 is stripped 20~30 minutes at room temperature, isolated liquor alumini chloridi and back extraction organic phase after back extraction；It is stripped organic
Phase return to step C is recycled；Liquor alumini chloridi is through evaporating, being concentrated to give aluminium chloride water treatment agent；
H, the crystalline mother solution mixing that cleaning solution isolated step E and step F are isolated, return to step B are used.
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Citations (7)
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| CN101759210A (en) * | 2010-01-18 | 2010-06-30 | 马昱昭 | Method for extracting high purity alumina and silica gel from coal ash |
| CN101870489A (en) * | 2010-04-27 | 2010-10-27 | 中国神华能源股份有限公司 | Method for producing superfine aluminium hydroxide and aluminium oxide by using flyash |
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| CN103833042A (en) * | 2013-12-13 | 2014-06-04 | 中国神华能源股份有限公司 | Method for preparing silicone oxide micro powder by using residues after extracting aluminum from fly ash, and silicone oxide micro powder |
| CN103964482A (en) * | 2014-05-16 | 2014-08-06 | 山西大学 | Method for synergistically utilizing silicon, aluminium and carbon in gangue |
| CN104291349A (en) * | 2014-09-26 | 2015-01-21 | 东北石油大学 | Method for preparing P type molecular sieve by using coal ash as raw material |
| CN104445307A (en) * | 2013-09-16 | 2015-03-25 | 贵阳铝镁设计研究院有限公司 | Method for processing fly ash |
-
2016
- 2016-08-29 CN CN201610744433.7A patent/CN106365173B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101759210A (en) * | 2010-01-18 | 2010-06-30 | 马昱昭 | Method for extracting high purity alumina and silica gel from coal ash |
| CN101870489A (en) * | 2010-04-27 | 2010-10-27 | 中国神华能源股份有限公司 | Method for producing superfine aluminium hydroxide and aluminium oxide by using flyash |
| CN102241410A (en) * | 2010-05-14 | 2011-11-16 | 东北大学 | Ecological synthetic utilization method of fly ash |
| CN104445307A (en) * | 2013-09-16 | 2015-03-25 | 贵阳铝镁设计研究院有限公司 | Method for processing fly ash |
| CN103833042A (en) * | 2013-12-13 | 2014-06-04 | 中国神华能源股份有限公司 | Method for preparing silicone oxide micro powder by using residues after extracting aluminum from fly ash, and silicone oxide micro powder |
| CN103964482A (en) * | 2014-05-16 | 2014-08-06 | 山西大学 | Method for synergistically utilizing silicon, aluminium and carbon in gangue |
| CN104291349A (en) * | 2014-09-26 | 2015-01-21 | 东北石油大学 | Method for preparing P type molecular sieve by using coal ash as raw material |
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