CN109110981A - A method of removing thallium in high acid water containing halogen - Google Patents

A method of removing thallium in high acid water containing halogen Download PDF

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Publication number
CN109110981A
CN109110981A CN201811307802.1A CN201811307802A CN109110981A CN 109110981 A CN109110981 A CN 109110981A CN 201811307802 A CN201811307802 A CN 201811307802A CN 109110981 A CN109110981 A CN 109110981A
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China
Prior art keywords
oxidation
thallium
acid water
water containing
containing halogen
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CN201811307802.1A
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CN109110981B (en
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付高明
付绸琳
陈国兰
白成庆
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HUNAN SHUIKOUSHAN NONFERROUS METALS GROUP CO Ltd
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HUNAN SHUIKOUSHAN NONFERROUS METALS GROUP CO Ltd
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    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00Multistage treatment of water, waste water, or sewage
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/001Processes for the treatment of water whereby the filtration technique is of importance
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F1/5236Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/66Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/72Treatment of water, waste water, or sewage by oxidation
    • C02F1/722Oxidation by peroxides
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/10Inorganic compounds
    • C02F2101/20Heavy metals or heavy metal compounds
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/16Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2301/00General aspects of water treatment
    • C02F2301/08Multistage treatments, e.g. repetition of the same process step under different conditions

Abstract

A method of removing thallium in high acid water containing halogen, comprising the following steps: (1) carry out defluorinate processing;(2) oxidation processes;(3) vulcanizing treatment;Present invention process process is simple, processing cost is low, suitable for large-scale industry containing high halogen acid water except thallium processing, and the removal rate of thallium is up to 99.9% or more, one section of waste residue that treatment process generates is free of heavy metal ion, it can be used as general fixed-end forces, thallium stable content is up to standard in treated waste water.

Description

A method of removing thallium in high acid water containing halogen
Technical field
The present invention relates to thalliums in acid water processing technology field more particularly to a kind of high acid water containing halogen of removal Method.
Background technique
Metal smelt produces, and includes a large amount of SO in flue gas during smelting in the industries such as electrolytic etching of metal and flue gas acid preparing2And Some harmful metal components, most smelteries all have double conversion double absorption acid making system, realize fume recovery and SO2Sulphuric acid, but It is the strongly acid wastewater that can be generated in the process largely containing heavy metal, abbreviation waste acid.
Wherein, it is always a hang-up that lead, which smelts the processing of acid water, mainly more because containing in its acid water Halide ion, such as fluorine, chlorine, and there are Tl in acid water for thallium+And Tl3+Two kinds of forms, wherein Tl3+There is very strong match Capability can form stable complex with halide ion, so while the presence of high-fluorine chlorine ion, thallium removes difficulty and increases.This Outside, Tl+Hydroxide TlOH be dissolved in water, generally use the more difficult removal of lime sedimentation.
The process for removing thallium for being able to achieve a large amount of wastewater treatments in lead smelting industry at present is seldom, Chinese patent CN201410685634.5, a kind of lead-zinc smelting flue gas washing acid water process for removing thallium are equal using first acid water is carried out Change pond sedimentation, tentatively removes a large amount of flue dust and other solids, then add the sulfide removal of mercury, the acid water after demercuration is passed through Acid-base accommodation pH value sequentially adds sulfide, flocculant, removes most of thallium and heavy metal ion by filters pressing to 9;To level-one Supernatant purified water and level-one the pressure clear liquid of processing, to 11, sequentially add sulfide, flocculant, by oblique by acid-base accommodation pH value Plate settles depth and removes thallium therein and heavy metal ion.But this method be suitble to remove low content thallium, and be not suitable for high fluorine, The acid water processing of chlorine, thallium content.
Chinese patent CN201611071686.9, a kind of pair high thallium content waste water carry out the method that segmentation removes thallium, this method Using two stages of Wastewater Pretreatment and advanced treating, wherein Wastewater Pretreatment segment mainly uses electrochemistry balancing reservoir to handle Waste water after the pretreatment for being 9 ~ 10 to thallium-containing quantity≤0.2mg/L, pH;Advanced treating stage waste water after it will pre-process is pumped to one Section removes thallium reaction tank, a series of processing such as flows through after electrochemical reaction system, aeration tank, flocculation tank.This method technique mistake In complexity, the processing waste water period is long, electrochemical treatments are at high cost, is not suitable for the processing of large-scale industry acid water.
Summary of the invention
The technical problem to be solved by the present invention is it is simple to overcome the deficiencies of the prior art and provide a kind of process flow, processing At low cost, the method for thallium suitable for the high acid water containing halogen of the removal of large-scale industry acid water processing.
The technical solution adopted by the present invention to solve the technical problems is: thallium in a kind of high acid water containing halogen of removal Method, comprising the following steps: (1) carry out defluorinate processing;(2) oxidation processes;(3) vulcanizing treatment;
Further, the oxidation processes include two-stage oxidation.
Further, defluorinate processing includes: that (1) calcium carbonate is added into acid water, at the same control pH in waste water= 1.4~1.8;(2) it is stirred to react 30min or more;(3) it filters: carrying out one section of filters pressing.
Further, stair oxidation includes: that ferrous iron is added into the clear liquid after one section of filters pressing of progress in (1) in the two-stage oxidation The solid-to-liquid ratio of salt and hydrogen peroxide, ferrous salt and hydrogen peroxide is 1:1 ~ 4, while controlling oxidation-reduction potential 500mv or more in waste water; (2) it is stirred to react 10min or more;(3) lime is added and adjusts wastewater pH=11.5 or more, the reaction was continued 30min or more;(3) mistake Filter: two sections of filters pressings are carried out.
Further, secondary oxidation includes: that (1) diluted acid adjusting is added into the clear liquid after two sections of filters pressings in the two-stage oxidation Wastewater pH=1.5 ~ 3;(2) ferrous salt and hydrogen peroxide are added, the solid-to-liquid ratio of ferrous salt and hydrogen peroxide is 1:1 ~ 4, while controlling oxygen Change reduction potential 600mv or more;(3) react 30min or more, add lime and adjust wastewater pH=6 ~ 8, the reaction was continued 10min with On;(4) three sections of filters pressings filters pressing: are carried out;
Further, the vulcanizing treatment includes: that (1) diluted acid adjusting wastewater pH=11 or more are added into the clear liquid after three sections of filters pressings; (2) vulcanized sodium and auxiliary are added except thallium agent, while controlling oxidation-reduction potential -300mv or less;(3) 30min or more is reacted; (4) it filters: carrying out four sections of filters pressings.
Further, the solid-to-liquid ratio of ferrous salt and hydrogen peroxide is 1:2 in the stair oxidation.
Further, the filtering carries out filters pressing using diaphragm filter press.
Further, oxidation-reduction potential is 500mv ~ 600mv in the stair oxidation.
Further, oxidation-reduction potential is 600mv ~ 700mv in the secondary oxidation.
A kind of principle that technical solution of the present invention is based primarily upon: side for removing thallium in high acid water containing halogen of the present invention Method removes the thallium in high acid water containing halogen using neutralization precipitation and sulfide precipitation integrated processes, and thallium is in acid water There are Tl+And Tl3+Two kinds of forms, wherein Tl3+There is very strong coordination ability, stable complex can be formed with halide ion, so Due to the presence of halogen high in waste acid, thallium removes difficulty and increases, and therefore, the present invention first carries out defluorinate processing containing halogen to height, subtracts Interference of few halide ion to thallium is removed, then two-stage oxidation is used, the numerical value of oxidation-reduction potential is controlled, converts thallium largely For Tl (OH)3Precipitating removes, and remaining thallium is removed using vulcanization, removes thallium agent by addition vulcanized sodium and auxiliary, can make to locate Thallium stable content is up to standard in waste water after reason.
Compared with the prior art, the advantages of the present invention are as follows: process flow is simple, and processing cost is low, is suitable for big rule Die worker's industry is containing high halogen acid water except thallium is handled, and the removal rate of thallium is up to 99.9% or more, one section of waste residue for the treatment of process generation Without heavy metal ion, it can be used as general fixed-end forces, thallium stable content is up to standard in treated waste water.
Detailed description of the invention
Fig. 1-is a kind of method and process flow chart for removing thallium in high acid water containing halogen of the present invention.
Specific embodiment
To facilitate the understanding of the present invention, below in conjunction with illustrate attached drawing and preferred embodiment to the present invention make more comprehensively, Careful description, but protection scope of the present invention is not limited to following specific embodiments.
Unless otherwise defined, all technical terms used hereinafter and the normally understood meaning of those skilled in the art It is identical.Technical term used herein is intended merely to the purpose of description specific embodiment, it is no intended to limit of the invention Protection scope.
Unless otherwise specified, a variety of materials, reagent, the instrument and equipment etc. used in the present invention can pass through market It is commercially available or can be prepared by existing method.
Embodiment 1:
A kind of method for removing thallium in high acid water containing halogen of the present invention, comprising the following steps: Certain District, Hunan lead smelts waste acid Waste water, main component Tl 17.36mg/L, F 2.87g/L, Cl 5.32g/L, H in acid water2SO435.6g/L, using such as A kind of method for removing thallium in high acid water containing halogen of the present invention shown in FIG. 1 handles it, (1) defluorinate processing: to It is slowly added to calcium carbonate in acid water and detects pH, the pH value 1.83 when controlling terminal in waste water, after being stirred to react 30min, One section of filters pressing is carried out using diaphragm filter press, obtains one section of slag of one section of filters pressing clear liquid and moisture content 26.7%;(2) stair oxidation: to Ferrous sulfate heptahydrate and hydrogen peroxide are added in one section of filters pressing clear liquid, wherein the solid-to-liquid ratio of ferrous sulfate heptahydrate and hydrogen peroxide difference Matched for ferrous sulfate heptahydrate in 0:1,1:1,1:2(such as table 1 and hydrogen peroxide), control oxidation-reduction potential 580mv, reaction It after 10min, adds lime and adjusts wastewater pH=11.58, after reacting 30min, two sections of filters pressings are carried out using diaphragm filter press, are obtained Two sections of filters pressing filterings and two sections of slags;(3) secondary oxidation: two sections of filters pressing clear liquid pH=2.38 first are adjusted with diluted acid, add seven water sulphur The solid-to-liquid ratio of sour ferrous and hydrogen peroxide, ferrous sulfate heptahydrate and hydrogen peroxide is 1:2, controls oxidation-reduction potential 650mv, fills thallium Point be oxidized to trivalent thallium, after reacting 30min, add lime and adjust pH=7.32, after reacting 10min, using diaphragm filter press into Three sections of filters pressings of row, obtain three sections of filters pressing filterings and three sections of slags;(4) vulcanizing treatment first with lime adjust three sections of filters pressing clear liquid pH= 11.89, vulcanized sodium and auxiliary is being added except thallium agent portland cement, is controlling oxidation-reduction potential -300mv, keeps remaining thallium raw It is precipitated at thallium sulfide, after reacting 30min, four sections of filters pressings is carried out using diaphragm filter press, obtain four sections of filters pressing clear liquids and four sections of slags. It takes two sections of filters pressing filterings to measure its thallium-containing quantity, calculates the removal efficiency of thallium.Experimental result is as shown in table 1.
Ferrous sulfate heptahydrate and hydrogen peroxide proportion dosage comparison in 1 stair oxidation of table
As it can be seen from table 1 being not added ferrous sulfate heptahydrate in stair oxidation processing or ferrous sulfate heptahydrate has been added all to removing Thallium is unfavorable, and when ferrous sulfate heptahydrate is 1:2 with hydrogen peroxide solid-to-liquid ratio, the removal effect of thallium is best in two sections of filters pressing clear liquids, takes off Except rate is 98.72%.
Further, it takes ferrous sulfate heptahydrate and hydrogen peroxide solid-to-liquid ratio is the four sections of filters pressing clear liquids obtained under 1:2 experiment condition, Measure its thallium-containing quantity be 1.565 μ g/L, calculate thallium removal efficiency be 99.99%.
Embodiment 2:
A kind of method for removing thallium in high acid water containing halogen of the present invention, comprising the following steps: Certain District, Hunan lead smelts waste acid Waste water, main component Tl 5.81mg/L, F 3.22g/L, Cl 4.85g/L, H in acid water2SO443.8g/L, using such as figure A kind of method for removing thallium in high acid water containing halogen of the present invention shown in 1 handles it, (1) defluorinate processing: to dirt It is slowly added to calcium carbonate in sour waste water and detects pH, the pH value 1.38 when controlling terminal in waste water after being stirred to react 30min, is adopted One section of filters pressing is carried out with diaphragm filter press, obtains one section of slag of one section of filters pressing filtering and moisture content 24.3%;(2) stair oxidation: Xiang Yi Ferrous sulfate heptahydrate and hydrogen peroxide is added in section filters pressing clear liquid, wherein the solid-to-liquid ratio of ferrous sulfate heptahydrate and hydrogen peroxide is 1:2, Oxidation-reduction potential 592mv is controlled, after reacting 10min, lime is added and adjusts wastewater pH=11.83, after reacting 30min, use Diaphragm filter press carries out two sections of filters pressings, obtains two sections of filters pressing filterings and two sections of slags;(3) two sections of pressures first secondary oxidation: are adjusted with diluted acid Cleaner liquid pH=2.38, add ferrous sulfate heptahydrate and hydrogen peroxide, and the solid-to-liquid ratio of ferrous sulfate heptahydrate and hydrogen peroxide is 1:2, control Oxygenerating reduction potential 665mv, keeping thallium fully oxidized is trivalent thallium, after reacting 30min, adds lime and adjusts pH=6.7, instead After answering 10min, three sections of filters pressings are carried out using diaphragm filter press, obtain three sections of filters pressing filterings and three sections of slags;(4) vulcanizing treatment first uses stone Ash adjusts three sections of filters pressing clear liquid pH=11.82, and vulcanized sodium is being added and is assisting removing thallium agent, is controlling oxidation-reduction potential -345v, makes Remaining thallium generates thallium sulfide precipitating, after reacting 30min, carries out four sections of filters pressings using diaphragm filter press, it is clear to obtain four sections of filters pressings Liquid and four sections of slags.Four sections of filters pressing clear liquids are taken, measuring its thallium-containing quantity is 2.767 μ g/L, and the removal efficiency for calculating thallium is 99.95%.
Other chemical reagent are used to adjust pH it should be noted that those skilled in the art also can choose, as follows chlorine Sour calcium, sodium hydroxide etc., and other ferrous salts, such as frerrous chloride are selected as needed;Ferrous carbonate etc., in addition, auxiliary Except thallium agent may be containing the common of one or more of tricalcium silicate, dicalcium silicate, tricalcium aluminate or tetra calcium aluminoferrite Portland cement.
The present invention is not intended to limit to the description of the specific embodiment of the invention above, those skilled in the art can be according to this The technical principle and principle of invention are compared to various adjustment and change to the composition of each component, and without departing from skill of the invention Art principle and principle belong to appended claims range of the present invention.

Claims (10)

1. a kind of method for removing thallium in high acid water containing halogen, which comprises the following steps:
(1) defluorinate processing is carried out;(2) oxidation processes;(3) vulcanizing treatment.
2. a kind of method for removing thallium in high acid water containing halogen according to claim 1, it is characterised in that: the oxidation Processing includes two-stage oxidation.
3. a kind of method for removing thallium in high acid water containing halogen according to claim 1, it is characterised in that: the defluorinate Processing includes: that (1) calcium carbonate is added into acid water, while controlling pH=1.4 ~ 1.8 in waste water;(2) it is stirred to react 30min More than;(3) it filters: carrying out one section of filters pressing.
4. a kind of method for removing thallium in high acid water containing halogen according to claim 2, it is characterised in that: the two-stage Stair oxidation includes: (1) to carrying out that ferrous salt and hydrogen peroxide are added in the clear liquid after one section of filters pressing in oxidation, the ferrous salt and The solid-to-liquid ratio of hydrogen peroxide is 1:1 ~ 4, while controlling oxidation-reduction potential 500mv or more in waste water;(2) be stirred to react 10min with On;(3) lime is added and adjusts wastewater pH=11.5 or more, the reaction was continued 30min or more;(3) it filters: carrying out two sections of filters pressings.
5. a kind of method for removing thallium in high acid water containing halogen according to claim 2, it is characterised in that: the two-stage Secondary oxidation includes: that (1) diluted acid adjusting wastewater pH=1.5 ~ 3 are added into the clear liquid after two sections of filters pressings in oxidation;(2) it adds The solid-to-liquid ratio of ferrous salt and hydrogen peroxide, ferrous salt and hydrogen peroxide is 1:1 ~ 4, while controlling oxidation-reduction potential 600mv or more; (3) 30min or more is reacted, lime is added and adjusts wastewater pH=6 ~ 8, the reaction was continued 10min or more;(4) three sections filters pressing: are carried out Filters pressing.
6. a kind of method for removing thallium in high acid water containing halogen according to claim 1, it is characterised in that: the vulcanization Processing includes: that (1) diluted acid adjusting wastewater pH=11 or more are added into the clear liquid after three sections of filters pressings;(2) vulcanized sodium and auxiliary is added It helps except thallium agent, while controlling oxidation-reduction potential -300mv or less;(3) 30min or more is reacted;(4) it filters: carrying out four sections of pressures Filter.
7. a kind of method for removing thallium in high acid water containing halogen according to claim 4, it is characterised in that: the level-one The solid-to-liquid ratio of ferrous salt and hydrogen peroxide is 1:2 in oxidation.
8. a kind of method for removing thallium in high acid water containing halogen according to claim 4, it is characterised in that: the level-one Oxidation-reduction potential is 500mv ~ 600mv in oxidation.
9. a kind of method for removing thallium in high acid water containing halogen according to claim 5, it is characterised in that: the second level Oxidation-reduction potential is 600mv ~ 700mv in oxidation.
10. according to a kind of any one of claim 3 ~ 9 method for removing thallium in high acid water containing halogen, feature exists In: the filtering carries out filters pressing using diaphragm filter press.
CN201811307802.1A 2018-11-05 2018-11-05 Method for removing thallium from waste water containing high-halogen waste acid Active CN109110981B (en)

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