CN107354301A - A kind of method for improving arsenic-containing material arsenic-removing rate - Google Patents
A kind of method for improving arsenic-containing material arsenic-removing rate Download PDFInfo
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- CN107354301A CN107354301A CN201710588260.9A CN201710588260A CN107354301A CN 107354301 A CN107354301 A CN 107354301A CN 201710588260 A CN201710588260 A CN 201710588260A CN 107354301 A CN107354301 A CN 107354301A
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D3/00—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances
- A62D3/30—Processes for making harmful chemical substances harmless or less harmful, by effecting a chemical change in the substances by reacting with chemical agents
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B30/00—Obtaining antimony, arsenic or bismuth
- C22B30/04—Obtaining arsenic
-
- A—HUMAN NECESSITIES
- A62—LIFE-SAVING; FIRE-FIGHTING
- A62D—CHEMICAL MEANS FOR EXTINGUISHING FIRES OR FOR COMBATING OR PROTECTING AGAINST HARMFUL CHEMICAL AGENTS; CHEMICAL MATERIALS FOR USE IN BREATHING APPARATUS
- A62D2101/00—Harmful chemical substances made harmless, or less harmful, by effecting chemical change
- A62D2101/40—Inorganic substances
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a kind of method for improving arsenic-containing material arsenic-removing rate.Using following steps:(1) arsenic-containing material is crushed to below 2.0mm;(2) arsenic-containing material after will be broken is put into the ball mill that liner is polytetrafluoroethylene (PTFE) after being mixed with compound Hydrodearsenic Catalyst I, non iron abrading-ball, carries out a ball milling, separation of solid and liquid is carried out after ball milling;(3) by the filter residue after separation of solid and liquid and compound Hydrodearsenic Catalyst II, continue to be put into above-mentioned ball mill after the mixing of non iron abrading-ball, progress secondary ball milling, separation of solid and liquid after ball milling.Filter residue caused by final can be used as raw materials recovery valuable metal;Filtrate caused by ball milling is after mixing twice, and sinking the steady arsenic of arsenic by calcium salt is handled, and carries out solidification landfill disposal.Compared with conventional leaching method, the present invention can increase substantially arsenic leaching rate;Compared with the arsenic removing methods such as high temperature hot pressing, this method can be carried out at normal temperatures and pressures, effectively reduce energy consumption.
Description
Technical field
It is more particularly to a kind of to pass through two benches wet ball grinding the present invention relates to a kind of method for improving arsenic-containing material arsenic-removing rate
Extract technology and leaching pharmaceutical agent combinations, can efficiently separate and be enriched with arsenic therein from arsenic-containing material, it is wet to belong to non-ferrous metal
Method field of metallurgy.
Background technology
The arsenic-containing materials such as the earth of positive pole, arsenic-containing smoke dust, arsenic filter cake are the important source materials for reclaiming gold and silver and various valuable metals;
But due to the presence of arsenic, whether pyrogenic process or wet recycling process, larger dirt can be brought to environment in processing procedure
Dye, flow is become complicated, the quality of other comprehensive utilization products is influenceed, along with the continuous improvement of current environmental requirement, smelting
Refining dearsenification is increasingly taken seriously.
On 08 15th, 2007 Chinese invention patent publication number CN101016582A, disclose the limited public affairs of Chenzhou City noble metal
Take charge of Cai's troop training, Yang Yue neoteric " Dearsenifying process for anode mud with high As and Pb content ".The invention is proposed anode mud with high As and Pb, adds alkali
Liquid, under conditions of air and heating is constantly blasted, leached through alkali;Lead anode slurry after dearsenification, utilize existing process synthesis
Reclaim gold and silver and other valuable metals;Natrium arsenicum in leachate sinks arsenic recovery arsenic concentrate through lime.The main pin of this patent of invention
To arsenic-containing materials such as the earth of positive pole, arsenic-containing material need to be crushed to defined granularity, if being applied to industrialized production, in operating process
In caused by dust can have a strong impact on air quality, workload is larger.On 08 15th, 2012 Chinese invention patent publication numbers
CN102634666A, disclose the " a kind of from fresh high concn. arsenic and lead sun of Huludao Zinc Industry Co., Ltd. poplar Shang Feng et al. inventions
The method of oxygen pressure-off arsenic in the mud of pole ".The invention is proposed lead anode slurry by pre-processing, and is then added alkali and is passed through oxygen,
Alkali leaching is carried out under oxygen pressure, heat is filtered after alkali leaching, formation filtrate and the dearsenification earth of positive pole, after dearsenification earth of positive pole separation metal, is entered
Enter silver and smelt workshop section's acquisition silver.Filtrate crystallisation by cooling, isolate natrium arsenicum crystallization and crystalline mother solution.This patent of invention is needed sun
Pole mud is calcined 0.5~2.0h after 80~90 DEG C of hot-water pretreatments at 280~220 DEG C, is crushed to granularity after cooling as 100
~200 mesh, earth of positive pole pretreatment process are complicated;Oxygen pressure alkali leaching stage oxygen demand it is big, need in autoclave control pressure
Operation;Whole operation process is complicated, and energy consumption is big, and cost is high, air can be polluted, there is certain potential safety hazard.
It is not difficult to find out, to realize that the efficient selective of arsenic separates, prior art usually uses the processing modes such as HTHP,
It is high to required reaction condition and equipment Requirement.In fact, among the processing disposal of solid waste, in order to realize the broken of waste residue
Broken, mixing, refinement, it can largely introduce the strong mechanical forces such as ball milling, grinding;And mechanical force would generally make the work of heavy metal
Property increase, be advantageous to the leaching of arsenic.But because ball-milling medium mostly may using iron-based medium, mechanical milling processes such as stainless steels
Iron ion is discharged, arsenic has very strong compatibility with iron ion, can generate insoluble precipitate, influence the leaching of arsenic.But this hair
It is bright by using non-iron-based milling material, avoid the generation of the insoluble matters such as ferric arsenate;The present invention passes through different choice simultaneously
Hydrodearsenic Catalyst component formula, optimize two sections of ball-milling technologies (Ball-milling Time, ratio of grinding media to material, ball milling speed), avoid it is overground caused by its
The leaching of his metal, realize the separation of arsenic-selective.The technical operation is simple, and reaction efficiency is high;Reaction is at normal temperatures and pressures
Carry out, relatively low is required to raw aqueous rate, granularity etc..
The content of the invention
For high pollution existing for existing arsenic-containing material dearsenic technique, high energy consumption, high cost, potential safety hazard etc. be present and lack
Point, the present invention is intended to provide one kind is using more metal arsenic-containing materials as object, using combining Hydrodearsenic Catalyst, by two sections of wet ball grindings,
Realize efficiently separating and being enriched with for arsenic in more metal arsenic-containing materials.This method technique is simple, and energy consumption is low, high-efficiency cleaning, solves to contain
The technical problem of arsenic material dearsenification processing, meets industrial production application needs.
In order to realize above-mentioned technical purpose, it is achieved using following technical scheme:
A kind of method for improving arsenic-containing material arsenic-removing rate:
Arsenic-containing material, non iron abrading-ball, compound Hydrodearsenic Catalyst I are put into non iron ball grinder and carry out first by a certain percentage
Secondary wet ball grinding;After reaction terminates, separation of solid and liquid, filter residue adds compound Hydrodearsenic Catalyst II and carries out second of wet ball grinding, solid-liquid point
From;
Compound Hydrodearsenic Catalyst I is NaOH, Na2S and thiocarbamide mixture, compound Hydrodearsenic Catalyst II are NaOH and Na2S mixture.
The method of described raising arsenic-containing material arsenic-removing rate:Arsenic mass content is 1.0~35.0% more metal objects containing arsenic
Material, including:Containing the one or more in arsenic smoke dust, the earth of positive pole containing arsenic, arsenic filter cake and arsenic alkaline slag.
The method of described raising arsenic-containing material arsenic-removing rate:By arsenic-containing material low temperature drying before first time wet ball grinding, break
It is below 2.0mm to be broken to particle diameter.
The method of described raising arsenic-containing material arsenic-removing rate:
Compound Hydrodearsenic Catalyst I is NaOH, Na2S and thiocarbamide mixture, its mass ratio are (5~9):(0.5~4.5):
(0.5~1), compound Hydrodearsenic Catalyst II are NaOH and Na2S mixture, its mass ratio are (7~9):(1~3).
The method of described raising arsenic-containing material arsenic-removing rate:
In first time wet ball grinding, the arsenic-containing material of butt is converted into:Compound Hydrodearsenic Catalyst I:Water:Mill ball quality ratio is 1:
(0.1~0.3):(2~3):(2~3);
In second of wet ball grinding, the first time wet ball grinding filter residue I of butt is converted into:Compound Hydrodearsenic Catalyst II:Water:Abrading-ball
Mass ratio is 1:(0.2~0.3):(2~3):(1~1.5).
The method of described raising arsenic-containing material arsenic-removing rate:
In first time ball milling, ball milling stabilizes to normal temperature, and rotating speed is 300~500r/min, and Ball-milling Time is 2~4h.
In second of ball milling, ball milling stabilizes to normal temperature, and rotating speed is 200~300r/min, and Ball-milling Time is 0.5~2h.
The method of described raising arsenic-containing material arsenic-removing rate:
Ball radius is 5~20mm.
The method of described raising arsenic-containing material arsenic-removing rate:
The ball grinder of polytetrafluoroethylene (PTFE) is used in ball milling, abrading-ball uses zirconium oxide material.
The method of described raising arsenic-containing material arsenic-removing rate:
Arsenic pregnant solution is obtained after filtrate mixing caused by ball milling twice, carries out heavy arsenic processing, the filter of second of wet ball grinding
Slag is as raw materials recovery valuable metal.
The method of described raising arsenic-containing material arsenic-removing rate:
The filtrate obtained after ball milling twice is mixed, after standing, lime is added in above-mentioned solution, separated
To solid arsenic slag and supernatant, Gu arsenic slag main component is calcium arsenate;Supernatant obtains alkali after treatment, is recycled back into for the first time
The wet ball grinding stage.
Wide adaptation range of the present invention, the earth of positive pole can be directed to, a variety of arsenic-containing materials containing arsenic smoke dust etc. are handled, dearsenification effect
More preferably, can be greatly improved using the wet ball grinding dearsenification process arsenic-removing rate of the present invention, the filtrate after heavy arsenic can circulate profit
With, both avoid the waste of resource or secondary pollution will not have been caused to environment, and be advantageous to environmental protection, suitable industrialized production.
Brief description of the drawings
Fig. 1 is the process chart of the present invention;
Embodiment
Following examples or embodiment are intended to further illustrate the present invention, rather than limitation of the invention.
Embodiment 1
The mechanical force and chemical dearsenification of the earth of positive pole of certain copper smelting plant
Step 1:The earth of positive pole of certain copper smelting plant is dried to constant weight at 65 DEG C, it is below 2.0mm to be crushed to particle diameter,
By arsenic-containing material:Compound Hydrodearsenic Catalyst I:Water:Abrading-ball is using quality as 1:(0.1~0.3):(2~3):The ratio of (2~3) is placed at
In the ball grinder of polytetrafluoroethylene (PTFE), it is 300r/min, 400r/min, 500r/min to set rotational speed of ball-mill respectively, and Ball-milling Time is
3h, after reaction stops, slurry is subjected to separation of solid and liquid with suction method, and cleaned slag 2-3 times with deionized water, obtain filter residue I
With filtrate I.
Step 2:By the filter residue I of above-mentioned gained with filter residue I:Compound Hydrodearsenic Catalyst II:Water:Abrading-ball is using quality as 1:(0.2~
0.3):(2~3):The ratio of (1~1.5), ball mill is opened, it is 200r/min, 300r/min to set rotational speed of ball-mill respectively, ball
Consume time as 1.5h, after reaction stops, slurry be subjected to separation of solid and liquid with suction method, and cleaned slag 2-3 times with deionized water,
Obtain filter residue II and filtrate II.
Step 3:Filtrate I and filtrate II are collected it is well mixed, after diluting certain multiple, with ICP determine filtrate
The concentration of middle arsenic.
The Main chemical component and content of certain the copper smelting plant earth of positive pole of table 1
Arsenic, antimony, the leaching rate of bismuth after the two sections of ball millings of certain copper smelting plant earth of positive pole of table 2
Embodiment 2:
The mechanical force and chemical dearsenification of the earth of positive pole of certain copper smelting plant
Step 1:The earth of positive pole of certain copper smelting plant is dried to constant weight at 65 DEG C, it is below 2.0mm to be crushed to particle diameter,
By arsenic-containing material:Compound Hydrodearsenic Catalyst I:Water:Abrading-ball is using quality as 1:(0.1~0.3):(2~3):The ratio of (2~3) is placed at
In the ball grinder of polytetrafluoroethylene (PTFE), rotational speed of ball-mill 400r/min, it is 1.5h, 2h, 3h, 3h to set Ball-milling Time respectively, is reacted
After stopping, slurry is subjected to separation of solid and liquid with suction method, and cleaned slag 2-3 times with deionized water, obtains filter residue I and filtrate I.
Step 2:By the filter residue I of above-mentioned gained with filter residue I:Compound Hydrodearsenic Catalyst II:Water:Abrading-ball is using quality as 1:(0.2~
0.3):(2~3):The ratio of (1~1.5), open ball mill, rotational speed of ball-mill 300r/min, respectively set Ball-milling Time be
0.5h, 1h, 1.5h, 2h, after reaction stops, slurry is subjected to separation of solid and liquid with suction method, and slag is cleaned into 2-3 with deionized water
It is secondary, obtain filter residue II and filtrate II.
Step 3:Filtrate I and filtrate II are collected it is well mixed, after diluting certain multiple, with ICP determine filtrate
The concentration of middle arsenic.
Arsenic, antimony, the leaching rate of bismuth after the two sections of ball millings of certain copper smelting plant earth of positive pole of table 3
1,2 result in conjunction with the embodiments, optimal experiment condition is selected through comparing, follow-up case is in first paragraph
Rotational speed of ball-mill is 400r/min, and Ball-milling Time 3h, second segment rotational speed of ball-mill are 300r/min, and Ball-milling Time is 1.5h condition
Lower progress.
Embodiment 3:
The mechanical force and chemical dearsenification of the earth of positive pole of certain copper smelting plant
Step 1:The earth of positive pole of certain copper smelting plant is dried to constant weight at 65 DEG C, it is below 2.0mm to be crushed to particle diameter,
By arsenic-containing material:Compound Hydrodearsenic Catalyst I:Water:Abrading-ball is using quality as 1:(0.1~0.3):(2~3):The ratio of (2~3) is placed at
In the ball grinder of polytetrafluoroethylene (PTFE), ball mill, rotating speed 400r/min, Ball-milling Time 3h, after reaction stops, with suction filtration are opened
Slurry is carried out separation of solid and liquid by method, and is cleaned slag 2-3 times with deionized water, obtains filter residue I and filtrate I.
Step 2:By the filter residue I of above-mentioned gained with filter residue I:Compound Hydrodearsenic Catalyst II:Water:Abrading-ball is using quality as 1:(0.2~
0.3):(2~3):The ratio of (1~1.5), opens ball mill, rotating speed 300r/min, Ball-milling Time 1.5h, and reaction stops
Afterwards, slurry is subjected to separation of solid and liquid with suction method, and cleaned slag 2-3 times with deionized water, obtain filter residue II and filtrate II.
Step 3:Filtrate I and filtrate II are collected it is well mixed, after diluting certain multiple, with ICP determine filtrate
The concentration of middle arsenic.
Present case is provided with a blank control test, is not added with abrading-ball under the same test conditions, other steps and
It is above-mentioned identical.
The Main chemical component and content of the earth of positive pole of certain copper smelting plant of table 4
Arsenic, lead, antimony, the leaching rate of bismuth after 5 two sections of ball millings of table
After the processing of this method, the leaching rate of arsenic significantly improves, and the leaching rate of other valuable metals substantially reduces,
The efficient leaching of arsenic and the purpose of the solid arsenic of the heavy arsenic of follow-up lime are realized, in turn ensure that the possibility of the recovery of valuable metal.
Embodiment 4:
The mechanical force and chemical dearsenification that the melting electricity of certain copper smelting plant gathers dust
Step 1:The melting electricity of certain copper smelting plant is gathered dust and is dried to constant weight at 65 DEG C, be crushed to particle diameter for 2.0mm with
Under, by arsenic-containing material:Compound Hydrodearsenic Catalyst I:Water:Abrading-ball is using quality as 1:(0.1~0.3):(2~3):The ratio of (2~3) is placed in
In the ball grinder of polytetrafluoroethylene (PTFE), ball mill, rotating speed 400r/min, Ball-milling Time 3h, after reaction stops, with taking out are opened
Slurry is carried out separation of solid and liquid by filter method, and is cleaned slag 2-3 times with deionized water, obtains filter residue I and filtrate I.
Step 2:By the filter residue I of above-mentioned gained with filter residue I:Compound Hydrodearsenic Catalyst II:Water:Abrading-ball is using quality as 1:(0.2~
0.3):(2~3):The ratio of (1~1.5), opens ball mill, rotating speed 300r/min, Ball-milling Time 1.5h, and reaction stops
Afterwards, slurry is subjected to separation of solid and liquid with suction method, and cleaned slag 2-3 times with deionized water, obtain filter residue II and filtrate II.
Step 3:Filtrate I and filtrate II are collected it is well mixed, after diluting certain multiple, with ICP determine filtrate
The concentration of middle arsenic.
Present case is provided with a blank control test, is not added with abrading-ball under the same test conditions, other steps and
It is above-mentioned identical.
The Main chemical component and content that the melting electricity of certain copper smelting plant of table 6 gathers dust
Arsenic, lead, antimony, the leaching rate of bismuth after the ball milling of table 7
After the processing of this method, the leaching rate of arsenic significantly improves, and the leaching rate of other valuable metals substantially reduces,
The efficient leaching of arsenic and the purpose of the solid arsenic of the heavy arsenic of follow-up lime are realized, in turn ensure that the possibility of the recovery of valuable metal.
Claims (10)
- A kind of 1. method for improving arsenic-containing material arsenic-removing rate, it is characterised in that:It is wet for the first time that arsenic-containing material, non iron abrading-ball, compound Hydrodearsenic Catalyst I are put into progress in non iron ball grinder by a certain percentage Method ball milling;After reaction terminates, separation of solid and liquid, filter residue adds compound Hydrodearsenic Catalyst II and carries out second of wet ball grinding, separation of solid and liquid;Compound Hydrodearsenic Catalyst I is NaOH, Na2S and thiocarbamide mixture, compound Hydrodearsenic Catalyst II are NaOH and Na2S mixture.
- 2. the method according to claim 1 for improving arsenic-containing material arsenic-removing rate, it is characterised in that:Arsenic mass content is 1.0~35.0% more metalliferous materials containing arsenic, including:Containing arsenic smoke dust, the earth of positive pole containing arsenic, arsenic filter cake and One or more in arsenic alkaline slag.
- 3. the method according to claim 1 or 2 for improving arsenic-containing material arsenic-removing rate, it is characterised in that:By arsenic-containing material low temperature drying before first time wet ball grinding, it is below 2.0mm to be crushed to particle diameter.
- 4. the method according to claim 1 for improving arsenic-containing material arsenic-removing rate, it is characterised in that:Compound Hydrodearsenic Catalyst I is NaOH, Na2S and thiocarbamide mixture, its mass ratio are (5~9):(0.5~4.5):(0.5~ 1), compound Hydrodearsenic Catalyst II is NaOH and Na2S mixture, its mass ratio are (7~9):(1~3).
- 5. according to the method for claim 1, it is characterised in that:In first time wet ball grinding, the arsenic-containing material of butt is converted into:Compound Hydrodearsenic Catalyst I:Water:Mill ball quality ratio is 1:(0.1~ 0.3):(2~3):(2~3);In second of wet ball grinding, the first time wet ball grinding filter residue I of butt is converted into:Compound Hydrodearsenic Catalyst II:Water:Mill ball quality Than for 1:(0.2~0.3):(2~3):(1~1.5).
- 6. the method according to claim 1 for improving arsenic-containing material arsenic-removing rate, it is characterised in that:In first time ball milling, ball milling stabilizes to normal temperature, and rotating speed is 300~500r/min, and Ball-milling Time is 2~4h.In second of ball milling, ball milling stabilizes to normal temperature, and rotating speed is 200~300r/min, and Ball-milling Time is 0.5~2h.
- 7. the method according to claim 1 for improving arsenic-containing material arsenic-removing rate, it is characterised in that:Ball radius is 5~20mm.
- 8. the method according to claim 1 for improving arsenic-containing material arsenic-removing rate, it is characterised in that:The ball grinder of polytetrafluoroethylene (PTFE) is used in ball milling, abrading-ball uses zirconium oxide material.
- 9. the method for the raising arsenic-containing material arsenic-removing rate described in as requested 1, it is characterised in that:Arsenic pregnant solution is obtained after filtrate mixing caused by ball milling twice, carries out heavy arsenic processing, the filter residue of second of wet ball grinding is made For raw materials recovery valuable metal.
- 10. the method for the raising arsenic-containing material arsenic-removing rate according to claim 1 or 9, it is characterised in that:The filtrate obtained after ball milling twice is mixed, after standing, lime is added in above-mentioned solution, it is isolated solid Arsenic slag and supernatant, Gu arsenic slag main component is calcium arsenate;Supernatant obtains alkali after treatment, is recycled back into first time wet method The ball milling stage.
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