CN108164071B - Method for recovering bromine salt from flue gas absorption liquid - Google Patents

Method for recovering bromine salt from flue gas absorption liquid Download PDF

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Publication number
CN108164071B
CN108164071B CN201810022963.XA CN201810022963A CN108164071B CN 108164071 B CN108164071 B CN 108164071B CN 201810022963 A CN201810022963 A CN 201810022963A CN 108164071 B CN108164071 B CN 108164071B
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defluorination
pac
pam
double
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CN108164071A (en
Inventor
曹自喜
张兴勇
刘红芳
段振兴
叶小勇
黄亚飞
刘俊
陈煜�
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China ruim engineering technology Limited by Share Ltd
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China Nerin Engineering Co Ltd
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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
    • C02F9/00—Multistage treatment of water, waste water, or sewage
    • 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
    • C02F1/001—Processes for the treatment of water whereby the filtration technique is of importance
    • 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
    • C02F1/02—Treatment of water, waste water, or sewage by heating
    • C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • C02F1/16—Treatment of water, waste water, or sewage by heating by distillation or evaporation using waste heat from other processes
    • 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
    • C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
    • C02F1/583—Treatment of water, waste water, or sewage by removing specified dissolved compounds by removing fluoride or fluorine compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/12—Halogens or halogen-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00—Nature of the contaminant
    • C02F2101/10—Inorganic compounds
    • C02F2101/12—Halogens or halogen-containing compounds
    • C02F2101/14—Fluorine or fluorine-containing compounds
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/18—Nature of the water, waste water, sewage or sludge to be treated from the purification of gaseous effluents
    • C—CHEMISTRY; METALLURGY
    • C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2301/00—General aspects of water treatment
    • C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions

Abstract

A method for recovering bromine salt from flue gas absorption liquid is characterized in that a waste circuit board is used as a main raw material, valuable metals are extracted by adopting a pyrogenic process smelting process, generated flue gas enters a tubular washing tower after pretreatment, washing is carried out by using 30% liquid alkali, and generated washing liquid contains bromine of which the content is as high as 4000 mg/L. The invention adopts a two-stage fluorine removal process, wherein the first stage fluorine removal uses Ca (OH)2‑CaCl2-combined PAM-PAC defluorination; and the second-stage fluorine removal uses a polyferric sulfate-PAM-PAC combined method to remove fluorine. Compared with the conventional wastewater fluorine removal method of removing fluorine and then removing calcium, the method has higher fluorine removal efficiency, controls the fluorine content in the recovered bromine salt to be 0.1 percent or even lower, and effectively improves the quality of the bromine salt.

Description

Method for recovering bromine salt from flue gas absorption liquid
Technical Field
The invention relates to a method for recovering bromine salt from a flue gas absorption liquid, which mainly takes waste circuit boards and low-grade impure copper as main raw materials, adopts flue gas treated by a pyrogenic process smelting process, and comprehensively removes fluorine from washing liquid generated by liquid alkali absorption, and particularly belongs to the technical field of wastewater treatment.
Background
The method is characterized in that a waste circuit board and low-grade impure copper are mixed as main raw materials, flue gas treated by a pyrometallurgical smelting process is adopted, washing liquid generated by liquid alkali absorption contains sulfur, bromide, fluoride and other components, wherein the concentration of fluorine and bromine is high, the concentration of fluorine is about 300-600 mg/L, the bromine content is 4000mg/L, the recovered bromine in the washing liquid has high economic value, usually, a double-effect evaporation process is adopted to recover bromine salt in the washing liquid, but the washing liquid contains high fluorine ions, so that the bromine salt cannot be directly fed into double-effect evaporation equipment for treatment, otherwise, the equipment is greatly corroded, and the recovered bromine salt quality is influenced by high fluorine content.
The conventional lime defluorination and calcium removal process is influenced by the pH value, when the pH value is more than 10, the defluorination efficiency is obviously reduced, and the lime defluorination is repeatedly carried out after the PH value is adjusted back. The invention is realized by a section of Ca (OH)2-CaCl2The fluorine removal by the PAM-PAC combined method solves the problem, and the further fluorine removal by the polyferric sulfate-PAM-PAC combined method at the second stage solves the problem that the PH value is adjusted back to F and is continuously increased.
Disclosure of Invention
The invention aims to remove high-content fluorine from the recovered washing liquid and ensure the quality of bromine salt. The fluorine content in the washing liquid is reduced by improving the pretreatment process of the washing liquid, and the treated washing liquid enters a double-effect evaporation system, so that double-effect evaporation equipment can be protected, and the quality of bromine salt can be effectively improved. Compared with the conventional calcium removal process after lime fluorine removal, the process is better, and the fluorine content of the bromine salt can be reduced to be below 0.1 percent.
A process for recovering bromine salt from the washed liquid of fume includes such steps as absorbing the waste gas containing bromide, fluoride and chloride with 30% liquid alkali to generate an absorption liquid containing bromide, chloride and fluoride, delivering the washed liquid to the pre-treating system of washed liquid, delivering the supernatant to dual-effect evaporating regulating pool, filtering by plate-frame liquid press, and pumping it to dual-effect evaporating system. The pretreatment is mainly to remove fluoride in the washing liquid, and the steam used by the double-effect evaporation system comes from a waste heat boiler.
The method comprises the following steps:
the flue gas is generated by using waste circuit boards and low-grade impure copper as main raw materials and limestone, quartz stone and coke as auxiliary materials through pyrogenic process treatment.
The absorption liquid is subjected to defluorination pretreatment, a two-stage defluorination method is adopted, and a first-stage defluorination process comprises the following steps: using Ca (OH)2-CaCl2Removing fluorine by using a PAM polyacrylamide-PAC polyaluminium chloride combination method; two-stage defluorination process: fluorine removal is carried out by using a polymeric ferric sulfate-PAM-PAC combined method.
A first-stage defluorination process: using Ca (OH)2-CaCl2PAM-PAC combinations using Ca (OH)2-CaCl2And (4) removing by a PAM-PAC combined method, conveying the washed liquid to a first-stage defluorination reaction tank, adding lime emulsion, and controlling the pH value to be 10.0.
Adding CaCl2The amount of the solution added is the Ca content of the coagulated solution2+The content is 45-50 mg/L. PAC and PAM medicaments are added simultaneously, wherein the adding amount of the PAC coagulant is 100mg/L, and the adding amount of the PAM flocculating agent is 5.0 mg/L. Controlling the solution to coagulate and react for 25-30 min, and then putting the solution into a first-stage defluorination sedimentation tank for natural sedimentation.
And after the natural settling time of the solution in the first-stage defluorination settling tank is more than or equal to 5.0 hours, performing second-stage defluorination.
Two-stage defluorination process: the fluorine is removed by using a polymeric ferric sulfate-PAM-PAC combined method, and the two-stage fluorine removal process also adopts an intermittent treatment mode.
The possible reactions of polymeric ferric sulphate with fluoride ions are as follows:
Fe3++6F-＝FeF6 3-Fe3++5F-＝FeF5 2-
Fe3++4F-＝FeF4 -Fe3++3F-＝FeF3
conveying the supernatant of the first-stage defluorination sedimentation tank to a second-stage defluorination reaction tank, and adding acid (HCl or H) after the tank is full2SO4) Adjusting the pH value to 6.0-7.5, and stirring for 3-5 min.
And after the reaction is finished, adding a polymeric ferric sulfate solution, wherein the adding amount is 450-500 mg/L. PAC and PAM medicaments are added simultaneously, wherein the adding amount of the PAC coagulant is 100mg/L, and the adding amount of the PAM flocculating agent is 5.0 mg/L. And controlling the coagulation and reaction time for 25-30 min, and then placing the mixture into a two-stage defluorination sedimentation tank for natural sedimentation.
And after the natural settling time of the solution in the second-stage defluorination settling tank is more than or equal to 5.0 hours, conveying the supernatant of the settling tank to a double-effect evaporation regulating tank, filtering by a plate-frame type hydraulic press, and then feeding into a double-effect evaporation system by a feeding pump.
The steam required by the double-effect evaporation system is generated by a waste heat boiler and is conveyed through a pipeline to evaporate the heat required by salt.
The invention has the beneficial effects that:
the invention recovers the bromine salt through double-effect evaporation after the two-stage defluorination pretreatment of the washed liquid, obviously reduces the corrosive damage of the washed liquid to double-effect evaporation equipment, ensures that the fluorine content in the recovered bromine salt is lower than 0.1 percent, effectively improves the quality of the bromine salt, reduces the discharge of waste water while realizing the reutilization of effective components in the waste water, and is beneficial to the environmental protection.
Drawings
FIG. 1 is a schematic view of the process of the present invention.
Detailed Description
Example 1
The method comprises the steps of carrying out pyrogenic smelting by using waste circuit boards and low-grade impure copper as main raw materials and limestone, quartz stone and coke as auxiliary materials, passing smelted flue gas through a high-efficiency pipeline type reaction desulfurizing tower, and obtaining acidic Substances (SO) in the flue gas2HBr, HCl, HF, etc.) is dissolved in the lye sprayed from the top of the desulfurization tower. The alkali liquor with dissolved acid substances circulates in the desulfurizing tower, and the washing liquid is obtained when the concentration of the concentrated solution reaches the discharge set value.
The washing liquid contains 300-600 mg/L of fluorine, the fluorine content in the wastewater passing through the first-stage fluorine removal reaction tank is 40-50 mg/L, the fluorine removal efficiency is up to 90%, and the effect is very obvious.
And (3) through a two-stage defluorination process, further reducing the fluorine content in the washed liquid to 25-40 mg/L, conveying the treated supernatant to a double-effect evaporation regulating pool, filtering by a plate-frame type hydraulic press, and then feeding into a double-effect evaporation system by a feeding pump. The steam used by the double-effect evaporation system is sourced from a waste heat boiler. The fluorine content in the recovered bromine salt is lower than 0.1 percent, and all heavy metals are far less than the 'hazardous waste identification Standard leaching toxicity identification' (GB)
5085-.
The first stage defluorination process comprises the following steps: delivering the washed solution to a first-stage defluorination reaction tank, adding lime emulsion to control the pH to be 10.0, and then adding CaCl2The amount of the added solution is the Ca in the coagulated solution2+The content is 50 mg/L; PAC and PAM medicaments are added simultaneously, wherein the adding amount of the PAC coagulant is 100mg/L, and the adding amount of the PAM flocculating agent is 5.0 mg/L; controlling the solution to coagulate and react for 25-30 min, and then placing the coagulated reaction mixture into a first-stage defluorination sedimentation tank for natural sedimentation for more than 5.0 h;
and a second-stage defluorination process: conveying the supernatant of the first-stage defluorination sedimentation tank to a second-stage defluorination reaction tank, adding acid hydrochloric acid or sulfuric acid to adjust the pH value to 6.0-7.5, and stirring for 3-5 min; then adding 5 wt% of polymeric ferric sulfate solution, wherein the adding amount is 500 mg/L; PAC and PAM medicaments are added simultaneously, wherein the adding amount of the PAC coagulant is 100mg/L, and the adding amount of the PAM flocculating agent is 5.0 mg/L; controlling the coagulation and reaction time to be 25-30 min, and then placing the coagulation reaction mixture into a second-stage defluorination sedimentation tank for natural sedimentation for more than 5.0 h; and then, conveying the supernatant in the second sedimentation tank to a double-effect evaporation regulating tank, filtering by a plate-frame type liquid pressing machine, pumping into a double-effect evaporation system, and recovering bromine salt.

Claims (2)

1. A method for recovering bromine salt from a flue gas absorption liquid is characterized in that: the method comprises the steps of mixing a waste circuit board and low-grade impure copper as raw materials, taking limestone, quartz stone and coke as auxiliary materials, absorbing flue gas generated by a pyrogenic process by 30wt% of caustic soda, treating obtained washing liquid by a defluorination pretreatment system, conveying supernate to a double-effect evaporation regulating tank, filtering by a plate-frame type liquid pressing machine, then entering a double-effect evaporation system for evaporation and concentration, and recovering to obtain bromine salt; the defluorination pretreatment system adopts a two-stage defluorination process: the first stage uses Ca (OH)2- CaCl2-combined PAM-PAC defluorination; in the second stage, fluorine is removed by using a polymeric ferric sulfate-PAM-PAC combined method;
the method comprises the following specific steps:
step 1: first stage defluorination
Delivering the washed solution to a first-stage defluorination reaction tank, adding lime emulsion to control the pH to be 10.0, and then adding CaCl2The amount of the added solution is the Ca in the coagulated solution2+The content is 50 mg/L; PAC and PAM medicaments are added simultaneously, wherein the adding amount of the PAC coagulant is 100mg/L, and the adding amount of the PAM flocculating agent is 5.0 mg/L; controlling the solution to coagulate and react for 25-30 min, and then placing the coagulated reaction mixture into a first-stage defluorination sedimentation tank for natural sedimentation for more than 5.0 h;
step 2: second stage defluorination
Conveying the supernatant in the first-stage defluorination sedimentation tank to a second-stage defluorination reaction tank, adding hydrochloric acid or sulfuric acid to adjust the pH value to 6.0-7.5, and stirring for 3-5 min; then adding 5 wt% of polymeric ferric sulfate solution, wherein the adding amount is 500 mg/L; PAC and PAM medicaments are added simultaneously, wherein the adding amount of the PAC coagulant is 100mg/L, and the adding amount of the PAM flocculating agent is 5.0 mg/L; controlling the coagulation and reaction time to be 25-30 min, and then placing the coagulation reaction mixture into a second-stage defluorination sedimentation tank for natural sedimentation for more than 5.0 h;
and step 3: double effect evaporation concentration
And then, conveying the supernatant in the second sedimentation tank to a double-effect evaporation regulating tank, filtering by a plate-frame type liquid pressing machine, pumping into a double-effect evaporation system for concentration, and recovering to obtain the bromine salt.
2. The method for recovering bromine salt from flue gas absorption liquid according to claim 1, wherein: the steam used by the double-effect evaporation system is sourced from a waste heat boiler.
CN201810022963.XA 2018-01-10 2018-01-10 Method for recovering bromine salt from flue gas absorption liquid Active CN108164071B (en)

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CN111036038A (en) * 2019-12-31 2020-04-21 洛阳丰瑞氟业有限公司 Equipment and process method for removing fluorine in flue gas generated in sulfuric acid preparation from pyrite

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CN1765516A (en) * 2005-09-13 2006-05-03 北京化工大学 Laminated material for reclaiming bromine and bromine-containing water treatment method
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CN104496063A (en) * 2014-11-17 2015-04-08 中国石油集团东北炼化工程有限公司吉林设计院 Method for removing fluorine in wastewater
CN105217869A (en) * 2015-10-16 2016-01-06 北京欧泰克能源环保工程技术股份有限公司 The method of resource of the spent acid produced in a kind of flue gas during smelting Sulphuric acid
CN105366839A (en) * 2015-08-19 2016-03-02 华电电力科学研究院 Treatment device and method for simultaneously removing high-concentration SS, fluoride, sulfate, arsenate and COD in desulfurization waste water
CN105481179A (en) * 2015-12-28 2016-04-13 中国石油集团东北炼化工程有限公司吉林设计院 Concentrated salt sewage zero-discharge treatment method
CN105502782A (en) * 2015-12-07 2016-04-20 湖南湘牛环保实业有限公司 Technology for recovering water resources and salt from coking wastewater in coal chemical industry

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US6776972B2 (en) * 2001-10-29 2004-08-17 Council Of Scientific And Industrial Research Recovery of common salt and marine chemicals from brine

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH10263558A (en) * 1997-03-26 1998-10-06 Japan Organo Co Ltd Treatment of fluorine-containing desulfurized waste water
CN1765516A (en) * 2005-09-13 2006-05-03 北京化工大学 Laminated material for reclaiming bromine and bromine-containing water treatment method
CN101746874A (en) * 2010-02-04 2010-06-23 武汉中新化工有限公司 Processing method of wastewater desulfurized by fume wet method
CN104496063A (en) * 2014-11-17 2015-04-08 中国石油集团东北炼化工程有限公司吉林设计院 Method for removing fluorine in wastewater
CN105366839A (en) * 2015-08-19 2016-03-02 华电电力科学研究院 Treatment device and method for simultaneously removing high-concentration SS, fluoride, sulfate, arsenate and COD in desulfurization waste water
CN105217869A (en) * 2015-10-16 2016-01-06 北京欧泰克能源环保工程技术股份有限公司 The method of resource of the spent acid produced in a kind of flue gas during smelting Sulphuric acid
CN105502782A (en) * 2015-12-07 2016-04-20 湖南湘牛环保实业有限公司 Technology for recovering water resources and salt from coking wastewater in coal chemical industry
CN105481179A (en) * 2015-12-28 2016-04-13 中国石油集团东北炼化工程有限公司吉林设计院 Concentrated salt sewage zero-discharge treatment method

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