CN111690830A - Method for recovering waste mercury nitrate reagent - Google Patents

Method for recovering waste mercury nitrate reagent Download PDF

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Publication number
CN111690830A
CN111690830A CN202010379940.1A CN202010379940A CN111690830A CN 111690830 A CN111690830 A CN 111690830A CN 202010379940 A CN202010379940 A CN 202010379940A CN 111690830 A CN111690830 A CN 111690830A
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China
Prior art keywords
mercury
waste
recovering
nitrate reagent
precipitate
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CN202010379940.1A
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Chinese (zh)
Inventor
李宝磊
祁国恕
侯海盟
赵岩
孔德勇
曾乐
闫向阳
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Shenyang Academy Environmental Sciences
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Shenyang Academy Environmental Sciences
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Priority to CN202010379940.1A priority Critical patent/CN111690830A/en
Publication of CN111690830A publication Critical patent/CN111690830A/en
Pending legal-status Critical Current

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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B43/00Obtaining mercury
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B5/00General methods of reducing to metals
    • C22B5/02Dry methods smelting of sulfides or formation of mattes
    • C22B5/16Dry methods smelting of sulfides or formation of mattes with volatilisation or condensation of the metal being produced
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working 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
    • C22B7/001Dry processes
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B7/00Working 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
    • C22B7/006Wet processes

Abstract

The invention discloses a method for recovering a waste mercuric nitrate reagent in the mercury-containing waste recovery industry. Meanwhile, the produced mercury-containing waste gas is condensed and adsorbed to achieve the emission standard and the waste water is precipitated to achieve the emission standard. The method has the advantages of simple operation, low treatment cost, mercury recovery rate of more than 97% on average, simple process, low cost, good economy and the like compared with a solidification landfill method.

Description

Method for recovering waste mercury nitrate reagent
Technical Field
The invention belongs to the technical field of mercury wet regeneration, and particularly relates to a method for recovering a waste mercury nitrate reagent.
Background
In recent years, the national emphasis on the prevention and control of heavy metal pollution is increasing, and people pay more and more attention to the prevention and control of mercury pollution due to the effective notice of 'water guarantee about mercury' issued by the country in 8 months in 2017, and the pressure on the prevention and control of mercury pollution in the mercury-related industry is increasing. Particularly, the mercury smelting industry is strictly regulated by related national departments, and the industry faces huge environmental protection pressure.
At present, the waste mercury-containing reagent is treated by adopting a curing and burying technology in China, and the technology mainly has the problems of large consumption of a curing stabilizer, no resource recovery and the like.
In recent years, most of the domestic and foreign treatment and disposal of mercury-containing reagents are solidification landfill technologies, such as "a mercury-containing reagent waste stabilization and solidification disposal process" (application publication No. CN 108687114 a). The technology has a certain curing and stabilizing effect on the treatment of the waste mercury-containing reagent, is suitable for the treatment and disposal of various waste mercury-containing reagents, but has the problems of complex process, high treatment cost, certain landfill cost needing to be paid and the like, and is difficult to meet the actual requirements of waste production units.
The method has good application value in recovering metallic mercury from waste mercury nitrate reagent by wet extraction technology, generates basic salt precipitate after being dissolved by a large amount of water, generates mercury oxide by uniform and slow heating decomposition, recovers elemental mercury by pyrogenic process of the mercury oxide, and has the mercury recovery rate of more than 97%.
Disclosure of Invention
The invention mainly solves the technical problem of providing a method for recovering a waste mercury nitrate reagent, and solves the problems of difficult disposal and high cost of the current waste mercury-containing reagent.
In order to achieve the purpose, the technical scheme provided by the invention is as follows: a method for recovering a waste mercury nitrate reagent is technically characterized by comprising the following steps: the method comprises the following steps:
step (I): adding the waste mercuric nitrate reagent into a reaction kettle, adding excessive distilled water, fully stirring and dissolving to generate basic nitrate Hg (NO)3)2The precipitate is formed by the precipitation of the mixture,
step (II): hg (NO) to be generated3)2Uniformly and slowly heating the precipitate to gradually decompose the precipitate and generate HgO;
step (three): and carrying out pyrogenic distillation and condensation on the generated HgO to obtain crude mercury, and purifying to obtain a simple substance mercury product.
The adding amount of the distilled water in the invention is 1-3L/kg Hg (NO)3)2The optimum range is 2-3L/kg Hg (NO)3)2
The reaction temperature in the invention is 50-100 ℃, and the optimal range is 70-100 ℃.
The reaction time is 2-5 h, and the optimal range is more than 4 h.
The invention has the advantages and beneficial effects that: the method has the advantages of simple operation, low treatment cost, average mercury recovery rate of more than 97 percent, simple process, low cost, good economy and the like compared with a solidification landfill method.
Drawings
FIG. 1 is a process flow diagram of the present invention.
Detailed Description
As shown in figure 1, the invention relates to a method for recovering a waste mercury nitrate reagent, which comprises the steps of adding the waste mercury nitrate reagent into a reaction kettle, adding excessive distilled water, fully stirring and dissolving to generate basic nitrate Hg (NO)3)2Precipitating, uniformly and slowly heating the mercury to gradually decompose the mercury and generate HgO, then carrying out pyrogenic distillation and condensation on the HgO to obtain crude mercury, and purifying to obtain a simple substance mercury product. Meanwhile, the produced mercury-containing waste gas is condensed and adsorbed to achieve the emission standard and the waste water is precipitated to achieve the emission standard. The chemical reaction formula of the method is as follows:
Figure DEST_PATH_IMAGE001
the process flow is as follows: the waste mercury nitrate is added with excessive distilled water to be stirred and dissolved to generate Hg (NO)3)2Precipitating and filtering to obtain Hg (NO)3)2The filtered waste water entersPerforming precipitation treatment and then discharging after reaching the standard; for Hg (NO)3)2And uniformly and slowly heating to generate HgO, carrying out pyrogenic distillation and condensation to obtain elemental mercury, and treating the condensed waste gas by an adsorption device to reach the standard and discharge.
The present invention is further illustrated by the following examples, which are not intended to limit the scope of the invention.
The first embodiment is as follows:
adding 1 kg of waste mercuric nitrate reagent into 1L of deionized water (room temperature), stirring for dissolving, standing for 10min, filtering, transferring the precipitate into a 1L reaction kettle, controlling the reaction time to be 3 h, gradually increasing the reaction temperature from 50 ℃ to 80 ℃, and uniformly, uniformly and slowly heating.
Cooling to room temperature to generate HgO, then carrying out pyrogenic distillation and condensation on the HgO to obtain crude mercury, and purifying to obtain a simple substance mercury product, wherein the purity of the mercury is 97.01% through testing.
Example two:
adding 1 kg of waste mercuric nitrate reagent into 2L of deionized water (room temperature), stirring for dissolving, standing for 10min, filtering, transferring the precipitate into a 1L reaction kettle, controlling the reaction time to be 4 h, gradually increasing the reaction temperature from 60 ℃ to 90 ℃, and uniformly, uniformly and slowly heating.
Cooling to room temperature to generate HgO, then carrying out pyrogenic distillation and condensation on the HgO to obtain crude mercury, and purifying to obtain a simple substance mercury product, wherein the purity of the mercury is 97.58% through testing.
Example three:
adding 1 kg of waste mercuric nitrate reagent into 3L of deionized water (room temperature), stirring for dissolving, standing for 10min, filtering, transferring the precipitate into a 1L reaction kettle, controlling the reaction time to be 5h, gradually increasing the reaction temperature from 70 ℃ to 100 ℃, and uniformly, uniformly and slowly heating.
Cooling to room temperature to generate HgO, then carrying out pyrogenic distillation and condensation on the HgO to obtain crude mercury, and purifying to obtain a simple substance mercury product, wherein the purity of mercury is 99.21% by testing.
The above-mentioned embodiments are only preferred embodiments of the present invention, and do not limit the scope of the present invention. Any modification and replacement within the principle of the present invention should be included in the protection scope of the present invention.

Claims (4)

1. A method for recovering a waste mercury nitrate reagent is characterized by comprising the following steps: the method comprises the following steps:
step (I): adding the waste mercuric nitrate reagent into a reaction kettle, adding excessive distilled water, fully stirring and dissolving to generate basic nitrate Hg (NO)3)2The precipitate is formed by the precipitation of the mixture,
step (II): hg (NO) to be generated3)2Uniformly and slowly heating the precipitate to gradually decompose the precipitate and generate HgO;
step (three): and carrying out pyrogenic distillation and condensation on the generated HgO to obtain crude mercury, and purifying to obtain a simple substance mercury product.
2. The method for recovering the waste mercury nitrate reagent according to claim 1, characterized in that: the addition amount of the distilled water is 1-3L/kg Hg (NO)3)2The optimum range is 2-3L/kg Hg (NO)3)2
3. The method for recovering the waste mercury nitrate reagent according to claim 1, characterized in that: the heating temperature is 50-100 ℃, and the optimal range is 70-100 ℃.
4. The method for recovering the waste mercury nitrate reagent according to claim 1, characterized in that: the reaction time is 3-5 h, and the optimal range is more than 4 h.
CN202010379940.1A 2020-05-08 2020-05-08 Method for recovering waste mercury nitrate reagent Pending CN111690830A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113604674A (en) * 2021-08-23 2021-11-05 云南金鼎锌业有限公司 Synergistic waste mercury regeneration technology and soaking precipitation pool thereof

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108687114A (en) * 2018-05-16 2018-10-23 扬州杰嘉工业固废处置有限公司 A kind of Organomercurial waste is stable and cures disposing technique

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108687114A (en) * 2018-05-16 2018-10-23 扬州杰嘉工业固废处置有限公司 A kind of Organomercurial waste is stable and cures disposing technique

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
姜晓明,陈扬,刘俐媛主编: "《含汞废物处置与环境风险管理》", 31 July 2018, 上海:上海科学技术出版社 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113604674A (en) * 2021-08-23 2021-11-05 云南金鼎锌业有限公司 Synergistic waste mercury regeneration technology and soaking precipitation pool thereof

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