CN108314071A - A method of preparing aluminium polychloride using gasification slag - Google Patents
A method of preparing aluminium polychloride using gasification slag Download PDFInfo
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- CN108314071A CN108314071A CN201810421978.3A CN201810421978A CN108314071A CN 108314071 A CN108314071 A CN 108314071A CN 201810421978 A CN201810421978 A CN 201810421978A CN 108314071 A CN108314071 A CN 108314071A
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- hydrochloric acid
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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
- C01F7/48—Halides, with or without other cations besides aluminium
- C01F7/56—Chlorides
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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
- C01P2006/10—Solid density
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Abstract
The present invention provides a kind of methods preparing aluminium polychloride using gasification slag, and described method includes following steps：(1) hydrochloric acid circulating leaching gasification slag is used, obtains containing molten aluminum and leached mud；(2) molten aluminum will be contained to post-process, and will obtain aluminium polychloride.The method is using the slag that gasifies as raw material, only it is the content that aluminium oxide in liquid phase can be improved by circulating leaching, without adding any silicon source, operating process is simple, and operating flexibility is big, solid phase impurity content is low after acidleach, non-secondary pollution object generates, and preparing industry for aluminium polychloride provides a kind of new technology and new raw material, alleviates the high-quality bauxite resource exhaustion in China, it is prepared for silica-base material and building materialsization is using a kind of quality raw materials are provided, realize economy and environmental benefit joint development.
Description
Technical field
The invention belongs to inorganic solid wastes recycling utilize technical field, be related to it is a kind of using gasification slag prepare aluminium polychloride
Method.
Background technology
Coal is mainly used for thermal power generation, and ratio is up to 60% or more, and organic resource is relatively low using added value, and causes
The problems such as serious air, soil and water pollution.Based on the above issues, Coal Gasification Technology has been closed extensively in recent years
Organic carbon in coal is synthesized organic products (ethyl alcohol, methane etc.) by the modification technology that gasifies, greatly improves organic resource by note
Utilization rate and added value, but waste residue ingredient/mineral phase structure that the process generates is complicated, it is big using difficulty.
For the physical characteristic of gasification slag, CN106336164A and CN106467376A individually disclose a kind of utilize and gasify
Slag prepares non-burning brick method, using the slag that gasifies as raw material, adds the substances tune such as cement, sweetened bean paste stone or gangue, slag thereto
Section composition ratio is mixed, and unburned brick product is obtained after overmolding-maintenance；CN104774023A and CN105130487A points
Do not disclose a kind of method preparing light ceramic and ceramic for filtration using the gentle slugging of flyash, by flyash, gasification slag and
After sodium/potassium feldspar mixes according to a certain percentage, adds a small amount of auxiliary agent and be molded-dry-processes such as firing, qualification can be obtained
Light ceramic and ceramic for filtration product.Based on its Characteristics of Chemical Constituents, CN103936134A discloses a kind of utilize and synthesizes ammonia
The method of gasification Slag treatment phenol wastewater is done after the slag that will gasify carries out hybrid reaction with diluted alkaline sodium hydroxide solution by washing-
Dry to obtain modified gas slugging, the absorption property of wherein particle surface and duct is substantially turned up, and the removal efficiency of Phenol for Waste Water is reachable
90% or so；CN106800416A discloses a kind of method preparing low-creep refractory brick using gasification slag, green with the slag that gasifies, violet
Stone, fused alumina zirconia, lime stone, flyash and feldspar etc. are raw material, the auxiliary agents such as boron carbide fibre and nanometer tungsten oxide are added, through meticulous
The workshop sections such as mill-microwave high-temperature sintering-washing-drying obtain the refractory material that mechanical performance is high, creep properties is low and anti-seismic performance is good.
Based on the high feature of gasification slag phosphorus content, CN102980195A discloses a kind of processing method of coal chemical industry gasification slag, will gasify
Slag adds clay wash after evenly mixing with coal slime, and being passed to fluidized-bed combustion boiler by conveyance conduit burns, and improves it
The utilization ratio of middle carbon.But slag mixed ratio is low, valuable resource is lost in the problems such as serious, Wu Fashi there are still gasification for the above method
Now gasify slag full dose and higher value application.
Aluminium polychloride has the characteristics that flocculation ability is strong, cleaning water is high and adaptive faculty is strong, is current water treatment field
The most commonly used is inorganic polymer flocculants, such as aluminium polychloride, polyaluminum ferric chloride etc., are widely used in industrial water
With the processing of sewage etc..The existing method for preparing aluminium polychloride generally with low-grade bauxite object, containing the lower mineral of aluminium and
Solid waste is as silicon source, and using technical hydrochloric acid as chlorine source, CN101531388A discloses a kind of production of aluminium polychloride and matches
Qualified aluminium polychloride water purification is prepared by reaction-polymerization adjusting and controlling using bauxite and technical hydrochloric acid as raw material in side and technique
Agent；CN101279755A discloses a kind of preparation method of calcium type polyaluminium chloride water purification agent, and kaolin is passed through activation process
The reactivity of wherein aluminium is improved afterwards, and addition salt peracid strengthening dissolves out aluminium oxide therein, is further prepared by polymerization adjusting and controlling
To aluminium polychloride product.CN107021765A, which is disclosed, a kind of preparing the coproducing polymerized aluminium chloride of mullite using aluminous fly-ash
Method, using acid activation liquid carry out circulating leaching promote liquid phase in aluminium ion be enriched with, further pass through addition crystallize aluminum feedstock
Polymerization adjusting and controlling, which is carried out, with substances such as calcium raw materials obtains aluminium polychloride product；CN104724744A discloses one kind
The method that raw material develops solid-state polymerization aluminum chloride flocculant, using the flyash of chemical calcination activation and technical hydrochloric acid as raw material,
Aluminium polychloride product is prepared by reaction-polymerization；CN102295305A and CN106892444A discloses one kind
Technical hydrochloric acid is first added into aluminium ash and is reacted, aluminic acid is then added into solution for the method that raw material prepares aluminium polychloride
Calcium carries out pH regulation and control and prepares polyaluminium chloride water purification agent.Above-mentioned technique generally existing alumina leaching process is difficult, silicon source addition
It measures the problems such as big, economy and environmental benefit are relatively low.
Invention content
In view of the deficiencies of the prior art, the present invention intends to provide it is a kind of using gasification slag prepare polyaluminium
The method of aluminium, the method reaction condition is mild, and aluminium content is high in pickle liquor, and addition is not necessarily to during preparing aluminium polychloride
Any silicon source, operating process is simple, and the solid phase impurity content after acidleach is low, is prepared for silica-base material and building materialsization utilize and provide one
Kind quality raw materials, non-secondary pollution generate, and realize economy and environmental benefit joint development.
For this purpose, the present invention uses following technical scheme：
One of the objects of the present invention is to provide a kind of method preparing aluminium polychloride using gasification slag, the method packets
Include following steps：
(1) hydrochloric acid circulating leaching gasification slag is used, obtains containing molten aluminum and leached mud；
(2) molten aluminum will be contained to post-process, and will obtain aluminium polychloride.
The present invention is only the content that aluminium oxide in liquid phase can be improved by circulating leaching, can will contain using the slag that gasifies as raw material
Aluminium ion concentration is improved to 50-60g/L in molten aluminum, and simultaneous oxidation aluminium content (mass percentage) is up to 7.5% or more, without adding
Add any silicon source, operating process is simple, and operating flexibility is big, and solid phase impurity content is low after acidleach, Fe2O3Content is reduced to by 9%
1% or so, CaO content is reduced to 1% or so, Na by 6%2O content is reduced to 0.5% or so by 3%, and the process is without secondary
Pollutant generates, and is prepared for silica-base material and building materialsization are using a kind of quality raw materials are provided, it is total with environmental benefit to realize economy
With development.
The method reaction condition provided by the invention that aluminium polychloride is prepared using gasification slag is mild, is polyaluminium aluminum
For a kind of new technology of industry offer and new raw material, it is exhausted to alleviate the high-quality bauxite resource in China.
Gasification slag is replaced with into other materials, is unable to reach using the method for circulating leaching and improves aluminium ion in leachate
Content purpose because can not use circulating leaching method prepare aluminium polychloride.
Step (1) described hydrochloric acid is industrial by-product hydrochloric acid and/or technical hydrochloric acid.It is provided by the invention to prepare aluminium polychloride
Method achieved the purpose that waste resource reuse, required raw material are only industrial by-product hydrochloric acid and/or technical hydrochloric acid and coal
The gasification slag that gasification generates.
Preferably, a concentration of 200-350g/L of step (1) described hydrochloric acid, such as 210g/L, 230g/L, 250g/L, 280g/
L, 300g/L, 320g/L or 340g/L etc..
Preferably, the liquid-solid ratio of step (1) hydrochloric acid and gasification slag is 3:1-6:1, such as 3.5:1、4.0:1、4.5:1、
4.8:1、5.2:1、5.5:1 or 5.8:1 etc..
Preferably, in step (1) the gasification slag quality of alumina percentage composition be not less than 20%, such as 22%, 25%,
28%, 30%, 32%, 38% or 45% etc..
Step (1) the utilization hydrochloric acid refers to being gasified using salt Ore Leaching when leaching for the first time to gasification slag circulating leaching
Slag, leaching later leaches previous leached mud using previous leachate, until cycle terminates.
Part hydrochloric acid is added in the cyclic process of step (1) described circulating leaching.The part refers to that the hydrochloric acid added accounts for
The volume of total leaching agent is more than 0 and is less than 100%.
Preferably, it adds a concentration of of hydrochloric acid and is more than 300g/L, such as 310g/L, 320g/L, 350g/L, 380g/L, 390g/
L, it is best can to reach leaching effect at this time by 420g/L or 450g/L etc..
The temperature of step (1) described circulating leaching is 75-95 DEG C, such as 78 DEG C, 80 DEG C, 85 DEG C, 88 DEG C or 92 DEG C.
Preferably, the time leached every time during step (1) described circulating leaching is 60-180min, as 80min,
100min, 120min or 150min etc..
Preferably, step (1) described circulating leaching carries out in a water bath.
Preferably, step (1) circulating leaching 5 times or more, such as 5 times, 6 times, 7 times, 8 times, 9 times, 10 times or 15 are inferior, pass through
It can will contain aluminium ion concentration in molten aluminum after 5 times or more cycles to improve to 50-60g/L, (quality percentage contains simultaneous oxidation aluminium content
Amount) reach 7.5-9.5% or more.
Step (1) described leached mud is washed, and building materials are used to prepare after dry.
Step (2) it is described post-processing include：Molten aluminum will be contained and carry out polymerisation, curing with basic salt.By basic salt into
Aluminium polychloride product is prepared in row polymerization adjusting and controlling, meets national standard (GB15892-2009) requirement.
The basic salt in calcium aluminate, calcium oxide or calcium base solid waste any one or at least two combination.Allusion quotation
Type but unrestricted combination such as calcium aluminate and calcium oxide, calcium aluminate and calcium base solid waste, calcium aluminate, calcium oxide and calcium base solid waste.
Preferably, the calcium base solid waste is selected from Industry Waste phosphorus slag and/or high calcium fluidization bed fly ash.
Preferably, liquid-solid ratio containing molten aluminum and basic salt is 6-15mL/g, as 7mL/g, 8mL/g, 9mL/g, 10mL/g,
11mL/g, 12mL/g or 14mL/g etc..
Preferably, the 2-4 addition of alkaline salinity is containing in molten aluminum, and such as 3 is inferior.Add the polymerization that basic salt obtains by several times
Aluminium chloride it is best in quality.
Preferably, the addition partial alkaline salt in containing molten aluminum is added every 0.5-1.5h, such as 0.6h, 0.8h, 1.0h, 1.2h
Or 1.4h etc., the optimal quality of the aluminium polychloride obtained at this time.The adjacent time for adding basic salt twice is preferably 1h.If
Overlong time is added portionwise, the volatilization of system hydrochloric acid reduces acidity to reduce the dissolving of basic salt, causes basic salt to waste, product
Basicity reduces；If be added portionwise, the time is too short, and basic salt is unable to fully quickly dissolve, and will also basic salt be caused to waste.
The temperature of the polymerisation is 75-95 DEG C, such as 78 DEG C, 80 DEG C, 85 DEG C, 88 DEG C or 92 DEG C.
Preferably, the polymerization reactor control pH is in 3-5, such as 4.
Preferably, the time of the polymerisation be 60-210min, as 80min, 100min, 120min, 150min,
180min or 200min etc..
The temperature of the curing is 45-75 DEG C, such as 50 DEG C, 60 DEG C, 65 DEG C or 72 DEG C.
Preferably, the time of the curing is 18-36h, such as 20h, 22h, 25h, 28h, 30h or 34h.
The method for preparing aluminium polychloride using gasification slag includes the following steps as a preferred technical solution,：
(1) it is 3 by liquid-solid ratio with the hydrochloric acid of a concentration of 200-350g/L:1-6:1 circulating leaching gasification slag, recycles 6 times, follows
Ring leach temperature be 75-95 DEG C, the time leached every time be 60-180min, added in cyclic process moiety concentrations be more than
300g/L hydrochloric acid, circulating leaching carry out under water bath condition, obtain containing molten aluminum and leached mud；
(2) molten aluminum will be contained and carry out polymerisation 60- under conditions of temperature is 75-95 DEG C and pH is 3-5 with basic salt
210min, the liquid-solid ratio containing molten aluminum and basic salt are 6-15mL/g, wherein the addition portion in containing molten aluminum is added every 0.5-1.5h
Basic salt, the 2-4 addition of alkaline salinity is divided to cure 18-36h under conditions of 45-75 DEG C later containing in molten aluminum, obtain polymerization chlorine
Change aluminium.
The aluminium polychloride product aluminium oxide that the method provided by the invention for preparing aluminium polychloride using gasification slag obtains
Content (mass percentage) reaches 7.8% or more, and basicity 54%-82%, density reaches 1.15g/cm3More than.
Numberical range of the present invention includes not only enumerated point value, further includes the above-mentioned numerical value not included
Arbitrary point value between range, as space is limited and for concise consideration, range includes described in the present invention no longer exclusive list
Specific point value.
Compared with prior art, beneficial effects of the present invention are：
The method provided by the invention for preparing aluminium polychloride using gasification slag can be improved in liquid phase by circulating leaching
The content of aluminium oxide can will contain aluminium ion concentration in molten aluminum and improve to 50-60g/L, simultaneous oxidation aluminium content up to 7.9-9.5% with
On, without adding any silicon source, reaction condition is mild, and process is simple, easy to operate, and operating flexibility is big, obtained polyaluminium
Aluminium product alumina content (mass percentage) reaches 7.8% or more, and basicity 54%-82%, density reaches 1.15g/
cm3More than, comply with the national standard requirements (GB15892-2009), and production cost is low, realizes gasification slag minimizing and recycling
It efficiently utilizes, preparing gentle slugging scale consumption for aluminium polychloride provides new technology, and preparing industry for aluminium polychloride carries
For a kind of new technology and new raw material, the high-quality bauxite resource exhaustion in China, economy and obvious environment benefit are alleviated.
Solid phase impurity content is low after the method acidleach provided by the invention for preparing aluminium polychloride using gasification slag, Fe2O3Contain
Amount is reduced to 1% or so by 9%, and CaO content is reduced to 1% or so, Na by 6%2O content is reduced to 0.5% or so by 3%,
And the process non-secondary pollution object generate, for silica-base material prepare and building materialsization utilization a kind of quality raw materials are provided, realize through
Ji and environmental benefit joint development.
Description of the drawings
Fig. 1 is the process flow chart that aluminium polychloride is prepared using gasification slag that one embodiment of the present invention provides.
Specific implementation mode
Technical solution to further illustrate the present invention below with reference to the accompanying drawings and specific embodiments.
The technique that aluminium polychloride is prepared using gasification slag that one embodiment of the present invention provides, as shown in Figure 1, described
Technique includes the following steps：
(1) waste hydrochloric acid circulating leaching gasification slag is used, obtains containing molten aluminum and leached mud, leached mud is used to prepare building materials；
(2) molten aluminum and basic salt will be contained and carry out polymerisation, post curing, obtain aluminium polychloride.
Embodiment 1
A method of aluminium polychloride being prepared using gasification slag, is included the following steps：
Process in leaching：Using gasification slag with industrial by-product hydrochloric acid according to liquid-solid ratio 4:1 carries out hybrid reaction, and wherein hydrochloric acid is dense
Degree is 200g/L, and reaction temperature is 95 DEG C, reaction time 120min, rotating speed 350r/min；After reaction, by solid-liquid
Isolated filtrate；
Cyclic process：It is added into above-mentioned filtrate needed for fresh process by-product hydrochloric acid (mass percentage 30%) preparation
Volume (reaches liquid-solid ratio 4 when leaching:1) acidleach process as above, is carried out, process as above is repeated, after recycling 6 times, richness is obtained by filtration
Aluminum solutions, wherein alumina content (mass percentage) are up to 8.3%；
Polymerization adjusting and controlling：High calcium fluidization bed fly ash (the mass percentage of CaO is added into the richness aluminum solutions>10%),
It is added three times, addition interval time is 1h, carries out polymerization adjusting and controlling, and control pH is in 3-5, liquid-solid ratio 12mL/g, polymerization temperature
85 DEG C, polymerization time 180min, curing temperature is at 55 DEG C, curing time 18h.
Aluminium polychloride product alumina content (mass percentage) 8.7%, basicity 73% are obtained, density is
1.22g/cm3。
Embodiment 2
A method of aluminium polychloride being prepared using gasification slag, is included the following steps：
Process in leaching：Using gasification slag with industrial by-product hydrochloric acid according to liquid-solid ratio 6:1 carries out hybrid reaction, and wherein hydrochloric acid is dense
Degree is 220g/L, and reaction temperature is 85 DEG C, reaction time 180min, rotating speed 350r/min；After reaction, by solid-liquid
Isolated filtrate；
Cyclic process：It is added into above-mentioned filtrate needed for fresh process by-product hydrochloric acid (mass percentage 30%) preparation
Volume (reaches liquid-solid ratio 6 when leaching:1) acidleach process as above, is carried out, process as above is repeated, after recycling 7 times, richness is obtained by filtration
Aluminum solutions, wherein alumina content (mass percentage) are up to 7.8%；
Polymerization adjusting and controlling：Industry Waste phosphorus slag (the mass percentage of CaO is added into the richness aluminum solutions>30%), divide 2 times to add
Entering, addition interval time is 1.5h, carries out polymerization adjusting and controlling, and control pH is 85 DEG C in 3-5, liquid-solid ratio 10mL/g, polymerization temperature,
Polymerization time is 180min, and curing temperature is at 60 DEG C, curing time 30h.
Aluminium polychloride product alumina content (mass percentage) 8.2%, basicity 61% are obtained, density is
1.17g/cm3。
Embodiment 3
A method of aluminium polychloride being prepared using gasification slag, is included the following steps：
Process in leaching：Using gasification slag with industrial by-product hydrochloric acid according to liquid-solid ratio 6:1 carries out hybrid reaction, and wherein hydrochloric acid is dense
Degree is 200g/L, and reaction temperature is 95 DEG C, reaction time 180min, rotating speed 350r/min；After reaction, by solid-liquid
Isolated filtrate；
Cyclic process：It is added into above-mentioned filtrate needed for fresh process by-product hydrochloric acid (mass percentage 30%) preparation
Volume (reaches liquid-solid ratio 6 when leaching:1) acidleach process as above, is carried out, process as above is repeated, after recycling 9 times, richness is obtained by filtration
Aluminum solutions, wherein alumina content (mass percentage) are up to 8.2%；
Polymerization adjusting and controlling：Industry Waste phosphorus slag (the mass percentage of CaO is added into the richness aluminum solutions>30%), divide 4 times to add
Entering, addition interval time is 0.5h, carries out polymerization adjusting and controlling, and control pH is 95 DEG C in 3-5, liquid-solid ratio 8mL/g, polymerization temperature,
Polymerization time is 210min, and curing temperature is at 65 DEG C, curing time 36h.
Aluminium polychloride product alumina content (mass percentage) 8.4%, basicity 54% are obtained, density is
1.15g/cm3。
Embodiment 4
A method of aluminium polychloride being prepared using gasification slag, is included the following steps：
Process in leaching：Using gasification slag with industrial by-product hydrochloric acid according to liquid-solid ratio 3:1 carries out hybrid reaction, and wherein hydrochloric acid is dense
Degree is 350g/L, and reaction temperature is 75 DEG C, reaction time 180min, rotating speed 350r/min；After reaction, by solid-liquid
Isolated filtrate；
Cyclic process：It is added into above-mentioned filtrate needed for fresh process by-product hydrochloric acid (mass percentage 30%) preparation
Volume (reaches liquid-solid ratio 3 when leaching:1) acidleach process as above, is carried out, process as above is repeated, after recycling 5 times, richness is obtained by filtration
Aluminum solutions, wherein alumina content (mass percentage) are up to 7.7%；
Polymerization adjusting and controlling：Calcium aluminate is added into the richness aluminum solutions, carries out polymerization adjusting and controlling, pH is in 3-5 for control, and liquid-solid ratio is
15mL/g, polymerization temperature are 75 DEG C, polymerization time 180min, and curing temperature is at 45 DEG C, curing time 36h.
Aluminium polychloride product alumina content (mass percentage) 8.5%, basicity 82% are obtained, density is
1.25g/cm3。
Embodiment 5
A method of aluminium polychloride being prepared using gasification slag, is included the following steps：
Process in leaching：Using gasification slag with industrial by-product hydrochloric acid according to liquid-solid ratio 5:1 carries out hybrid reaction, and wherein hydrochloric acid is dense
Degree is 250g/L, and reaction temperature is 95 DEG C, reaction time 120min, rotating speed 350r/min；After reaction, by solid-liquid
Isolated filtrate；
Cyclic process：It is added into above-mentioned filtrate needed for fresh process by-product hydrochloric acid (mass percentage 30%) preparation
Volume (reaches liquid-solid ratio 5 when leaching:1) acidleach process as above, is carried out, process as above is repeated, after recycling 6 times, richness is obtained by filtration
Aluminum solutions, wherein alumina content (mass percentage) are up to 7.5%；
Polymerization adjusting and controlling：High-calcium fly ass (the mass percentage of CaO is added into the richness aluminum solutions>10%), divide 3 times to add
Entering, addition interval time is 0.5h, carries out polymerization adjusting and controlling, and control pH is 85 DEG C in 3-5, liquid-solid ratio 12mL/g, polymerization temperature,
Polymerization time is 120min, and curing temperature is at 55 DEG C, and the curing time is for 24 hours.
Aluminium polychloride product alumina content (mass percentage) 7.8%, basicity 68% are obtained, density is
1.21g/cm3。
Embodiment 6
A method of aluminium polychloride being prepared using gasification slag, is included the following steps：
Process in leaching：Using gasification slag with industrial by-product hydrochloric acid according to liquid-solid ratio 4:1 carries out hybrid reaction, and wherein hydrochloric acid is dense
Degree is 300g/L, and reaction temperature is 85 DEG C, reaction time 120min, rotating speed 350r/min；After reaction, by solid-liquid
Isolated filtrate；
Cyclic process：It is added into above-mentioned filtrate needed for fresh process by-product hydrochloric acid (mass percentage 30%) preparation
Volume (reaches liquid-solid ratio 4 when leaching:1) acidleach process as above, is carried out, process as above is repeated, after recycling 7 times, richness is obtained by filtration
Aluminum solutions, wherein alumina content (mass percentage) are up to 8.1%；
Polymerization adjusting and controlling：Industry Waste phosphorus slag (the mass percentage of CaO is added into the richness aluminum solutions>30%), divide 2 times to add
Enter, addition interval time is 1h, carries out polymerization adjusting and controlling, and control pH is 95 DEG C in 3-5, liquid-solid ratio 10mL/g, polymerization temperature, is gathered
The conjunction time is 120min, and curing temperature is at 60 DEG C, curing time 30h.
Aluminium polychloride product alumina content (mass percentage) 8.5%, basicity 63% are obtained, density is
1.26g/cm3。
Embodiment 7
A method of aluminium polychloride being prepared using gasification slag, is included the following steps：
Process in leaching：Using gasification slag with industrial by-product hydrochloric acid according to liquid-solid ratio 5:1 carries out hybrid reaction, and wherein hydrochloric acid is dense
Degree is 300g/L, and reaction temperature is 95 DEG C, reaction time 180min, rotating speed 350r/min；After reaction, by solid-liquid
Isolated filtrate；
Cyclic process：It is added into above-mentioned filtrate needed for fresh process by-product hydrochloric acid (mass percentage 30%) preparation
Volume (reaches liquid-solid ratio 5 when leaching:1) acidleach process as above, is carried out, process as above is repeated, after recycling 6 times, richness is obtained by filtration
Aluminum solutions, wherein alumina content (mass percentage) are up to 9.3%；
Polymerization adjusting and controlling：Industry Waste phosphorus slag (the mass percentage of CaO is added into the richness aluminum solutions>30%), divide 3 times to add
Entering, addition interval time is 0.5h, carries out polymerization adjusting and controlling, and control pH is 95 DEG C in 3-5, liquid-solid ratio 12mL/g, polymerization temperature,
Polymerization time is 180min, and curing temperature is at 65 DEG C, curing time 36h.
Aluminium polychloride product alumina content (mass percentage) 9.8%, basicity 68% are obtained, density is
1.24g/cm3。
Embodiment 8
A method of aluminium polychloride being prepared using gasification slag, is included the following steps：
Process in leaching：Using gasification slag of the alumina content not less than 20% with industrial by-product hydrochloric acid according to liquid-solid ratio 3:1
Hybrid reaction is carried out, wherein concentration of hydrochloric acid is 300g/L, and reaction temperature is 95 DEG C, reaction time 150min, rotating speed 350r/
min；After reaction, filtrate is obtained by separation of solid and liquid；
Cyclic process：It is added into above-mentioned filtrate needed for fresh process by-product hydrochloric acid (mass percentage 30%) preparation
Volume (reaches liquid-solid ratio 3 when leaching:1) acidleach process as above, is carried out, process as above is repeated, after recycling 5 times, richness is obtained by filtration
Aluminum solutions, wherein alumina content (mass percentage) are up to 9.1%；
Polymerization adjusting and controlling：High-calcium fly ass (CaO mass percentages are added into the richness aluminum solutions>10%), divide 4 times to add
Entering, addition interval time is 0.5h, carries out polymerization adjusting and controlling, and control pH is 90 DEG C in 3-5, liquid-solid ratio 10mL/g, polymerization temperature,
Polymerization time is 120min, and curing temperature is at 55 DEG C, curing time 36h.
Aluminium polychloride product alumina content (mass percentage) 9.5%, basicity 74% are obtained, density is
1.27g/cm3。
Embodiment 9
A method of aluminium polychloride being prepared using gasification slag, is included the following steps：
Process in leaching：Using gasification slag with industrial by-product hydrochloric acid according to liquid-solid ratio 3:1 carries out hybrid reaction, and wherein hydrochloric acid is dense
Degree is 320g/L, and reaction temperature is 90 DEG C, reaction time 150min, rotating speed 350r/min；After reaction, by solid-liquid
Isolated filtrate；
Cyclic process：It is added into above-mentioned filtrate needed for fresh process by-product hydrochloric acid (mass percentage 30%) preparation
Volume (reaches liquid-solid ratio 3 when leaching:1) acidleach process as above, is carried out, process as above is repeated, after recycling 9 times, richness is obtained by filtration
Aluminum solutions, wherein alumina content (mass percentage) are up to 9.5%；
Polymerization adjusting and controlling：Calcium oxide is added into the richness aluminum solutions, point 4 additions, addition interval time is 0.5h, is gathered
Regulation and control are closed, control pH is 92 DEG C in 3-5, liquid-solid ratio 6mL/g, polymerization temperature, and polymerization time 150min, curing temperature is 70
DEG C, curing time 18h.
Aluminium polychloride product alumina content (mass percentage) 9.8%, basicity 70% are obtained, density is
1.28g/cm3。
Comparative example 1
Except by the gasification slag in embodiment 1 replace in bauxite, kaolin or aluminous fly-ash any one or extremely
Outside few two kinds of combination, remaining is same as Example 1.
After circulating leaching, the alumina content in leachate is 2.3%-6.4%, obtains the oxidation of aluminium polychloride product
Aluminium content 2.5%-6.7%, basicity are higher than 60%, density 1.15-1.21g/cm3。
Comparative example 2
Bauxite in CN101531388A embodiments is replaced with into gasification slag.
After leaching, the alumina content in leachate is 5.7%, obtains aluminium polychloride product alumina content 6.2%,
Basicity is 47%, density 1.18g/cm3。
Applicant states, the foregoing is merely the specific implementation mode of the present invention, but protection scope of the present invention not office
It is limited to this, person of ordinary skill in the field is it will be clearly understood that any belong to those skilled in the art and taken off in the present invention
In the technical scope of dew, the change or replacement that can be readily occurred in are all fallen within protection scope of the present invention and the open scope.
Claims (10)
1. a kind of method preparing aluminium polychloride using gasification slag, which is characterized in that described method includes following steps：
(1) hydrochloric acid circulating leaching gasification slag is used, obtains containing molten aluminum and leached mud；
(2) molten aluminum will be contained to post-process, and will obtain aluminium polychloride.
2. according to the method described in claim 1, it is characterized in that, step (1) described hydrochloric acid is industrial by-product hydrochloric acid and/or work
Industry hydrochloric acid；
Preferably, a concentration of 200-350g/L of step (1) described hydrochloric acid；
Preferably, the liquid-solid ratio of step (1) hydrochloric acid and gasification slag is 3:1-6:1；
Preferably, quality of alumina percentage composition is not less than 20% in step (1) the gasification slag.
3. method according to claim 1 or 2, which is characterized in that the temperature of step (1) described circulating leaching is 75-95
℃；
Preferably, the time leached every time during step (1) described circulating leaching is 60-180min；
Preferably, step (1) described circulating leaching carries out in a water bath；
Preferably, step (1) circulating leaching 5 times or more.
4. according to the method described in one of claim 1-3, which is characterized in that the cyclic process of step (1) described circulating leaching
In add part hydrochloric acid；
Preferably, it adds a concentration of of hydrochloric acid and is more than 300g/L.
5. according to the method described in one of claim 1-4, which is characterized in that step (1) described leached mud is washed, after dry
It is used to prepare building materials.
6. according to the method described in one of claim 1-5, which is characterized in that step (2) it is described post-processing include：Molten aluminum will be contained
Polymerisation, curing are carried out with basic salt.
7. according to the method described in one of claim 1-6, which is characterized in that the basic salt be selected from calcium aluminate, calcium oxide or
In calcium base solid waste any one or at least two combination；
Preferably, the calcium base solid waste is selected from Industry Waste phosphorus slag and/or high calcium fluidization bed fly ash；
Preferably, the liquid-solid ratio containing molten aluminum and basic salt is 6-15mL/g；
Preferably, the 2-4 addition of alkaline salinity is containing in molten aluminum；
Preferably, addition partial alkaline salt, preferably 1h in containing molten aluminum is added every 0.5-1.5h.
8. according to the method described in one of claim 1-7, which is characterized in that the temperature of the polymerisation is 75-95 DEG C；
Preferably, the time of the polymerisation is 60-210min；
Preferably, the polymerization reactor control pH is in 3-5.
9. according to the method described in one of claim 1-8, which is characterized in that the temperature of the curing is 45-75 DEG C；
Preferably, the time of the curing is 18-36h.
10. according to the method described in one of claim 1-9, which is characterized in that described method includes following steps：
(1) it is 3 by liquid-solid ratio with the hydrochloric acid of a concentration of 200-350g/L:1-6:1 circulating leaching gasification slag, recycle 5 times or more, it follows
Ring leach temperature be 75-95 DEG C, the time leached every time be 60-180min, added in cyclic process moiety concentrations be more than
300g/L hydrochloric acid, circulating leaching carry out under water bath condition, obtain containing molten aluminum and leached mud；
(2) molten aluminum will be contained and carry out polymerisation 60-210min under conditions of temperature is 75-95 DEG C and pH is 3-5 with basic salt,
Liquid-solid ratio containing molten aluminum and basic salt is 6-15mL/g, wherein partial alkaline salt, alkali are added in containing molten aluminum every 0.5-1.5h
Property salinity 2-4 times be added containing in molten aluminum, 18-36h is cured under conditions of 45-75 DEG C later, obtains aluminium polychloride.
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| CN110903104A (en) * | 2018-09-17 | 2020-03-24 | 中国科学院过程工程研究所 | Method for preparing foamed ceramic and co-producing calcium chloride and polyaluminium chloride by fluidized bed fly ash |
| CN110902704A (en) * | 2018-09-17 | 2020-03-24 | 中国科学院过程工程研究所 | Method for preparing polyaluminum chloride by using fluidized bed fly ash |
| CN111943336A (en) * | 2020-07-16 | 2020-11-17 | 国家能源集团宁夏煤业有限责任公司 | Method for preparing polysilicate aluminum ferric flocculant, polysilicate aluminum ferric flocculant and application thereof |
| CN114940507A (en) * | 2022-06-22 | 2022-08-26 | 神华准能资源综合开发有限公司 | Method for extracting alumina from fly ash |
| CN114985435A (en) * | 2022-08-05 | 2022-09-02 | 中国科学院过程工程研究所 | Method for comprehensively utilizing waste salt and various solid wastes |
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| CN117069232A (en) * | 2023-10-17 | 2023-11-17 | 中国科学院过程工程研究所 | Resource utilization method of chromium-containing gasification slag impurity removal acid liquor |
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| CN110903104A (en) * | 2018-09-17 | 2020-03-24 | 中国科学院过程工程研究所 | Method for preparing foamed ceramic and co-producing calcium chloride and polyaluminium chloride by fluidized bed fly ash |
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| CN111943336A (en) * | 2020-07-16 | 2020-11-17 | 国家能源集团宁夏煤业有限责任公司 | Method for preparing polysilicate aluminum ferric flocculant, polysilicate aluminum ferric flocculant and application thereof |
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| CN114985435A (en) * | 2022-08-05 | 2022-09-02 | 中国科学院过程工程研究所 | Method for comprehensively utilizing waste salt and various solid wastes |
| CN115304090A (en) * | 2022-09-19 | 2022-11-08 | 西安科技大学 | Comprehensive utilization method of coal gasification fine slag |
| CN117069232A (en) * | 2023-10-17 | 2023-11-17 | 中国科学院过程工程研究所 | Resource utilization method of chromium-containing gasification slag impurity removal acid liquor |
| CN117069232B (en) * | 2023-10-17 | 2024-02-20 | 中国科学院过程工程研究所 | Resource utilization method of chromium-containing gasification slag impurity removal acid liquor |
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