CN106277085A - A kind of method utilizing aluminium section bar plant sludge to prepare aluminium polychlorid - Google Patents
A kind of method utilizing aluminium section bar plant sludge to prepare aluminium polychlorid Download PDFInfo
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- CN106277085A CN106277085A CN201610645826.2A CN201610645826A CN106277085A CN 106277085 A CN106277085 A CN 106277085A CN 201610645826 A CN201610645826 A CN 201610645826A CN 106277085 A CN106277085 A CN 106277085A
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- aluminium
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- aluminium section
- plant sludge
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
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- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Treatment Of Water By Oxidation Or Reduction (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention discloses a kind of method utilizing aluminium section bar plant sludge to prepare aluminium polychlorid, comprise the following steps: 1) aluminium section bar plant sludge and mixed in hydrochloric acid reaction, and remove insoluble matter；2) removal of escaping gas；3) Fenton's reaction, removes dissolved organic matter；4) heavy metal ion agent for capturing removes heavy metal ion；5) generation of aluminium polychlorid.The present invention uses Fenton reagent to decompose the dissolved organic matter in aluminium section bar plant sludge, use heavy metal ion agent for capturing heavy metal ion to carry out precipitation to remove, and aluminium oxide is converted into aluminium polychlorid, decrease solids discharge, save landfill expense；The aluminium polychlorid quality of the present invention is good, can be directly used for sewage purification, does not produce secondary pollution in production process; achieve the comprehensive reutilization of resource; decrease the exploitation of bauxite resource, meet National Sustainable Development Strategies, environmental conservation is had positive meaning.
Description
Technical field
The present invention relates to a kind of method utilizing aluminium section bar plant sludge to prepare aluminium polychlorid.
Background technology
China is through the development of more than 20 years, it has also become the big producing country of world aluminum section bar, aluminium section bar yield continuous five
Year is sure to occupy the first in the world.Guangdong is the region that the whole nation or even global aluminum section bar enterprise concentrate most, and industry size is big, yearly productive capacity
More than 2,000,000 tons.Architectural aluminum section needs to carry out surface process, needs to use substantial amounts of water resource, annual production 100000 tons
Aluminium section bar enterprise, process, for aluminium material surface, the year water consumption that each operation cleans and be about 2,000,000 tons, the water after over cleaning is i.e.
For aluminium section bar plant industrial wastewater.Major pollutants in aluminum section industrial wastewater include fluorion, ammonia nitrogen, COD, Cr VI, have
Machine thing, sulfate radical, phosphate radical etc., waste water is processed by the method combining coagulating sedimentation in general employing alkali with regulation, can produce
Raw substantial amounts of mud.
Aluminium section bar produces the processing method of waste water and is broadly divided into following three kinds: 1) chemical method: neutralization precipitation method, sulfide are heavy
Shallow lake method, the ferrite sedimentation method, chemical reduction method, electrochemical reducing；2) Physical: coagulation, air supporting, absorption, membrance separation；3) raw
Thing method: bioflocculation, biochemical process, plant ecological reparation.At present, aluminium section bar produces the treatment technology comparative maturity of waste water,
Substantially can meet the requirement of qualified discharge, have even can also realize recycling of waste water.
In aluminium section bar plant sludge in addition to containing substantial amounts of aluminium compound and calcium compounds, possibly together with a small amount of Organic substance with
And the compound such as zinc, nickel, copper, composition is more complicated.Aluminium section bar plant sludge is broadly divided into chromium-bearing sludge and high aluminium-containing sludge, no
Generic mud needs classification to process, and could fully realize the recycling of resource.But, current most of factories are the most right
Mud is classified, but the mixing of several mud is stacked, then uses the mode of landfill to focus on, and not only can take
The land resource of limit, also can cause the wasting of resources, pollutes environment.
Aluminium polychlorid (PAC) is a kind of water-purifying material, is the inorganic polymer water that a kind of molecular weight is relatively big, electric charge is higher
Treatment agent, it is common that use the mineral aggregate (such as: light-burned bauxite, stammerer aluminum, aluminium hydroxide, calcium aluminate powder etc.) containing aluminum and hydrochloric acid
Prepared by reaction, the consumption to bauxite resource is the biggest.If able to by the alum recovery in aluminium section bar plant sludge, be used for preparing polymerization
Aluminum chloride, can reduce the consumption of bauxite resource, can bring extra output for enterprise again, also reduce the discharge of mud simultaneously
Amount, reduces Treatment of Sludge cost.
The invention discloses a kind of method utilizing aluminium section bar plant sludge to prepare aluminium polychlorid, with aluminium section bar plant sludge,
Calcium oxide and hydrochloric acid etc. produce aluminium polychlorid for primary raw material, are possible not only to realize recycling of resource, greatly reduce
The consumption of bauxite resource, it is also possible to reduce the pollution to environment.
Summary of the invention
It is an object of the invention to provide a kind of method utilizing aluminium section bar plant sludge to prepare aluminium polychlorid.
The technical solution used in the present invention is:
A kind of method utilizing aluminium section bar plant sludge to prepare aluminium polychlorid, comprises the following steps:
1) aluminium section bar plant sludge, hydrochloric acid are added in the hermetic container with device for recovering tail gas, fully reaction is stirred at room temperature, quiet
Put, remove insoluble matter；
2) in the solution of step 1), steam it is passed through, 55～60 DEG C of stirring fully reactions；
3) to step 2) solution in be passed through steam, add Fenton reagent, 55～60 DEG C of stirring fully reactions, stand, remove not
Molten thing；
4) in the solution of step 3), add heavy metal ion agent for capturing, fully reaction is stirred at room temperature, stands, remove insoluble matter；
5) in the solution of step 4), calcium oxide is added, the basicity of regulation product, it is passed through steam simultaneously, 94～98 DEG C of stirrings are filled
Divide reaction, filter, remove filtering residue, obtain aluminium polychlorid.
Described in step 1), aluminium section bar plant sludge, the mass ratio of hydrochloric acid are 1:(0.8～2.5).
In aluminium section bar plant sludge described in step 1), the mass fraction of aluminium oxide is 10%～35%.
The mass fraction of hydrochloric acid described in step 1) is 30%～33%.
In step 1) aluminium section bar plant sludge and hydrochloric acid reaction fully after, the mass fraction of HCl free in feed liquid be 2%～
3%。
After step 3) adds Fenton reagent, H in solution2O2Concentration be 50～200mg/L, Fe in solution2+、H2O2Rub
That ratio is 1:(5～10).
In step 4), the addition of heavy metal ion agent for capturing is the 0.005%～0.02% of solution gross mass.
Heavy metal ion agent for capturing described in step 4) be xanthic acid esters, dithiocarbamate salt derivative, 1,3,
5-triazine-2, at least one in 4,6-tri-mercaptan trisodium salts.
The addition of calcium oxide described in step 5) is the 10%～48.9% of aluminium section bar plant sludge quality.
The basicity of aluminium polychlorid described in step 5) is 75%～90%.
The invention has the beneficial effects as follows:
1) present invention uses Fenton reagent to decompose the dissolved organic matter in aluminium section bar plant sludge, uses heavy metal ion
Agent for capturing heavy metal ion carries out precipitation and removes, and aluminium oxide is converted into aluminium polychlorid, decreases solids discharge, joint
About landfill expense；
2) the aluminium polychlorid quality of the present invention is good, can be directly used for sewage purification, does not produce secondary pollution in production process, real
Show the comprehensive reutilization of resource, decreased the exploitation of bauxite resource, meet National Sustainable Development Strategies, environmental conservation has been had
There is positive meaning.
Detailed description of the invention
A kind of method utilizing aluminium section bar plant sludge to prepare aluminium polychlorid, comprises the following steps:
1) aluminium section bar plant sludge, hydrochloric acid are added in the hermetic container with device for recovering tail gas, fully reaction is stirred at room temperature, quiet
Put, remove insoluble matter；
2) in the solution of step 1), steam it is passed through, 55～60 DEG C of stirring fully reactions；
3) to step 2) solution in be passed through steam, add Fenton reagent, 55～60 DEG C of stirring fully reactions, stand, remove not
Molten thing；
4) in the solution of step 3), add heavy metal ion agent for capturing, fully reaction is stirred at room temperature, stands, remove insoluble matter；
5) in the solution of step 4), calcium oxide is added, the basicity of regulation product, it is passed through steam simultaneously, 94～98 DEG C of stirrings are filled
Divide reaction, filter, remove filtering residue, obtain aluminium polychlorid.
Preferably, a kind of method utilizing aluminium section bar plant sludge to prepare aluminium polychlorid, comprise the following steps:
1) aluminium section bar plant sludge, hydrochloric acid are added in the hermetic container with device for recovering tail gas, reaction 1～2 is stirred at room temperature little
Time, stand, remove insoluble matter；
2) being passed through steam in the solution of step 1), 55～60 DEG C of stirrings are reacted 2～3 hours；
3) to step 2) solution in be passed through steam, add Fenton reagent, 55～60 DEG C of stirring reactions 0.5～1 hour, stand,
Remove insoluble matter；
4) in the solution of step 3), add heavy metal ion agent for capturing, reaction 0.5～1 hour is stirred at room temperature, stands, remove not
Molten thing；
5) in the solution of step 4), calcium oxide is added, the basicity of regulation product, it is passed through steam simultaneously, 94～98 DEG C of stirrings are anti-
Answer 3～4 hours, filter, remove filtering residue, obtain aluminium polychlorid.
Preferably, described in step 1), aluminium section bar plant sludge, the mass ratio of hydrochloric acid are 1:(0.8～2.5).
Preferably, in aluminium section bar plant sludge described in step 1), the mass fraction of aluminium oxide is 10%～35%.
Preferably, the mass fraction of hydrochloric acid described in step 1) is 30%～33%.
Preferably, in step 1) aluminium section bar plant sludge and hydrochloric acid reaction fully after, the mass fraction of HCl free in feed liquid
It is 2%～3%.
Preferably, after step 3) adds Fenton reagent, H in solution2O2Concentration be 50～200mg/L, Fe in solution2+、
H2O2Mol ratio be 1:(5～10).
Preferably, in step 4), the addition of heavy metal ion agent for capturing is the 0.005%～0.02% of solution gross mass.
Preferably, heavy metal ion agent for capturing described in step 4) be xanthic acid esters, dithiocarbamate salt derive
Thing, 1,3,5-triazines-2, at least one in 4,6-tri-mercaptan trisodium salts.
It is further preferred that heavy metal ion agent for capturing described in step 4) is 1,3,5-triazines-2,4,6-tri-mercaptan trisodiums
Salt.
Preferably, the addition of calcium oxide described in step 5) is the 10%～48.9% of aluminium section bar plant sludge quality.
Preferably, the basicity of aluminium polychlorid described in step 5) is 75%～90%.
Preferably, being stirred the rotating speed of blender during reaction is 60～80r/min.
Below in conjunction with specific embodiment, the present invention is made further explanation and description.
Embodiment 1:
A kind of method utilizing aluminium section bar plant sludge to prepare aluminium polychlorid, comprises the following steps:
1), under room temperature, the hermetic container with device for recovering tail gas adds 1000g aluminium section bar plant sludge (alumina content
35wt%) with 2500g hydrochloric acid (33wt%), stirring reaction 1 hour, after reaction completely, stand 4 hours, the precipitation in removing solution；
2) starting device for recovering tail gas, be passed through steam in the solution of step 1), controlling solution temperature is 58 ± 2 DEG C, controls to stir
Mixing speed is 60r/min, reacts 2 hours, makes the HF in solution evaporate, qualified discharge after saturated limewater absorbs；
3) to step 2) solution in be passed through steam, controlling solution temperature is 58 ± 2 DEG C, and controls mixing speed is 60r/min, throwing
Add 1.75g hydrogen peroxide (H2O2Mass fraction is 27.5%) and 0.44g ferrous sulfate heptahydrate (Fe2+Mass fraction is 18%), reaction
0.5 hour, stand 4 hours, remove the precipitation separated out in solution；
4) in the solution of step 3), 1.47g 1,3,5-triazines-2 are added, 4,6-tri-mercaptan trisodium salts, react 0.5 hour, quiet
Put 4 hours, remove the precipitation in solution；
5) being passed through steam in the solution of step 4), controlling solution temperature is 96 ± 2 DEG C, and control mixing speed is 60r/min, throws
Adding 489g calcium oxide, the basicity of regulation product, react 4 hours, plate-and-frame filtration removes filtering residue, obtains aluminium polychlorid.
Embodiment 2:
A kind of method utilizing aluminium section bar plant sludge to prepare aluminium polychlorid, comprises the following steps:
1), under room temperature, the hermetic container with device for recovering tail gas adds 1000g aluminium section bar plant sludge (alumina content
20wt%) with 1500g hydrochloric acid (33wt%), stirring reaction 1 hour, after reaction completely, stand 4 hours, the precipitation in removing solution；
2) starting device for recovering tail gas, be passed through steam in the solution of step 1), controlling solution temperature is 58 ± 2 DEG C, controls to stir
Mixing speed is 60r/min, reacts 2 hours, makes the HF in solution evaporate, qualified discharge after saturated limewater absorbs；
3) to step 2) solution in be passed through steam, controlling solution temperature is 58 ± 2 DEG C, and controls mixing speed is 60r/min, throwing
Add 0.875g hydrogen peroxide (H2O2Mass fraction is 27.5%) and 0.306g ferrous sulfate heptahydrate (Fe2+Mass fraction is 18%), instead
Answer 0.5 hour, stand 4 hours, remove the precipitation separated out in solution；
4) in the solution of step 3), 0.2g 1,3,5-triazines-2 are added, 4,6-tri-mercaptan trisodium salts, react 0.5 hour, stand
4 hours, remove the precipitation in solution；
5) being passed through steam in the solution of step 4), controlling solution temperature is 96 ± 2 DEG C, and control mixing speed is 60r/min, throws
Adding the basicity of 303g calcium oxide regulation product, react 3.5 hours, plate-and-frame filtration removes filtering residue, obtains aluminium polychlorid.
Embodiment 3:
A kind of method utilizing aluminium section bar plant sludge to prepare aluminium polychlorid, comprises the following steps:
1), under room temperature, the hermetic container with device for recovering tail gas adds 1000kg aluminium section bar plant sludge (alumina content
10wt%) with 800kg hydrochloric acid (32wt%), stirring reaction 1 hour, after reaction completely, stand 4 hours, the precipitation in removing solution；
2) starting device for recovering tail gas, be passed through steam in the solution of step 1), controlling solution temperature is 58 ± 2 DEG C, controls to stir
Mixing speed is 60r/min, reacts 2 hours, makes the HF in solution evaporate, qualified discharge after saturated limewater absorbs；
3) to step 2) solution in be passed through steam, controlling solution temperature is 58 ± 2 DEG C, and controls mixing speed is 60r/min, throwing
Add 0.4875kg hydrogen peroxide (H2O2Mass fraction is 27.5%) and 0.245kg ferrous sulfate heptahydrate (Fe2+Mass fraction is 18%),
React 0.5 hour, stand 4 hours, remove the precipitation separated out in solution；
4) in the solution of step 3), 0.117kg 1,3,5-triazines-2 are added, 4,6-tri-mercaptan trisodium salts, react 0.5 hour,
Stand 4 hours, remove the precipitation in solution；
5) being passed through steam in the solution of step 4), controlling solution temperature is 96 ± 2 DEG C, and control mixing speed is 60r/min, throws
Adding 173kg calcium oxide, the basicity of regulation product, react 3 hours, plate-and-frame filtration removes filtering residue, obtains aluminium polychlorid.
After testing, the basicity of the aluminium polychlorid product of embodiment 1～3 preparation is 75～90%, and the content of aluminium oxide is
5～9%, pH value (aqueous solution of product 1wt%) is 4.0～5.0, water insoluble matter content≤0.05mg/L, content of beary metal summation
≤0.00002mg/L。
Above-described embodiment is the present invention preferably embodiment, but embodiments of the present invention are not by above-described embodiment
Limit, the change made under other any spirit without departing from the present invention and principle, modify, substitute, combine, simplify,
All should be the substitute mode of equivalence, within being included in protection scope of the present invention.
Claims (10)
1. one kind utilizes the method that aluminium section bar plant sludge prepares aluminium polychlorid, it is characterised in that: comprise the following steps:
1) aluminium section bar plant sludge, hydrochloric acid are added in the hermetic container with device for recovering tail gas, fully reaction is stirred at room temperature, quiet
Put, remove insoluble matter；
2) in the solution of step 1), steam it is passed through, 55～60 DEG C of stirring fully reactions；
3) to step 2) solution in be passed through steam, add Fenton reagent, 55～60 DEG C of stirring fully reactions, stand, remove not
Molten thing；
4) in the solution of step 3), add heavy metal ion agent for capturing, fully reaction is stirred at room temperature, stands, remove insoluble matter；
5) in the solution of step 4), calcium oxide is added, the basicity of regulation product, it is passed through steam simultaneously, 94～98 DEG C of stirrings are filled
Divide reaction, filter, remove filtering residue, obtain aluminium polychlorid.
Method the most according to claim 1, it is characterised in that: the mass ratio of aluminium section bar plant sludge, hydrochloric acid described in step 1)
For 1:(0.8～2.5).
Method the most according to claim 1, it is characterised in that: the quality of aluminium oxide in aluminium section bar plant sludge described in step 1)
Mark is 10%～35%.
Method the most according to claim 1, it is characterised in that: the mass fraction of hydrochloric acid described in step 1) is 30%～33%.
Method the most according to claim 1, it is characterised in that: in step 1), aluminium section bar plant sludge and hydrochloric acid reaction are abundant
After, the mass fraction of HCl free in feed liquid is 2%～3%.
Method the most according to claim 1, it is characterised in that: after step 3) adds Fenton reagent, H in solution2O2Concentration
It is 50～200mg/L, Fe in solution2+、H2O2Mol ratio be 1:(5～10).
Method the most according to claim 1, it is characterised in that: in step 4), the addition of heavy metal ion agent for capturing is molten
The 0.005%～0.02% of liquid gross mass.
8. according to the method described in claim 1 or 7, it is characterised in that: heavy metal ion agent for capturing described in step 4) is xanthan
Esters of gallic acid, dithiocarbamate salt derivative, 1,3,5-triazines-2, at least one in 4,6-tri-mercaptan trisodium salts.
Method the most according to claim 1, it is characterised in that: the addition of calcium oxide described in step 5) is that aluminium section bar plant is dirty
The 10%～48.9% of shale amount.
Method the most according to claim 1, it is characterised in that: the basicity of aluminium polychlorid described in step 5) be 75%～
90%。
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| CN108455642A (en) * | 2017-12-28 | 2018-08-28 | 江苏永葆环保科技有限公司 | A method of it is prepared without slag PAC using efficiently emulsification shear agitation technology |
| CN110042242A (en) * | 2019-03-11 | 2019-07-23 | 广东环境保护工程职业学院 | A method of aluminium chromium nickel in separation aluminium shape surface processing sludge |
| CN110282802A (en) * | 2019-06-26 | 2019-09-27 | 绍兴绿嘉环保科技有限公司 | The technique that recycling prepares aluminium polychloride in a kind of waste water |
| CN111925099A (en) * | 2020-09-25 | 2020-11-13 | 北京环球中科水务科技有限公司 | Inorganic polymer sludge conditioner and preparation method and application thereof |
| CN112897658A (en) * | 2021-01-18 | 2021-06-04 | 广州博芳环保科技股份有限公司 | Method for preparing polyaluminum chloride composite flocculant by using sludge from aluminum profile plant |
| CN113135789A (en) * | 2021-05-24 | 2021-07-20 | 鄂尔多斯应用技术学院 | Method for processing total-nutrient compound fertilizer based on coal-based solid waste |
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| CN112897658A (en) * | 2021-01-18 | 2021-06-04 | 广州博芳环保科技股份有限公司 | Method for preparing polyaluminum chloride composite flocculant by using sludge from aluminum profile plant |
| CN113135789A (en) * | 2021-05-24 | 2021-07-20 | 鄂尔多斯应用技术学院 | Method for processing total-nutrient compound fertilizer based on coal-based solid waste |
| CN113135789B (en) * | 2021-05-24 | 2022-07-08 | 鄂尔多斯应用技术学院 | Method for processing total-nutrient compound fertilizer based on coal-based solid waste |
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Application publication date: 20170104 |