CN106893865B - From the method for relating to extraction mercury in the sour mud of weight - Google Patents
From the method for relating to extraction mercury in the sour mud of weight Download PDFInfo
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- CN106893865B CN106893865B CN201710211864.1A CN201710211864A CN106893865B CN 106893865 B CN106893865 B CN 106893865B CN 201710211864 A CN201710211864 A CN 201710211864A CN 106893865 B CN106893865 B CN 106893865B
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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
- C22B7/007—Wet processes by acid leaching
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B19/00—Selenium; Tellurium; Compounds thereof
- C01B19/008—Salts of oxyacids of selenium or tellurium
-
- 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
- C22B43/00—Obtaining mercury
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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
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- Organic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Inorganic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Treatment Of Sludge (AREA)
Abstract
Present invention relates particularly to a kind of from the method for extracting mercury in the sour mud of weight is related to, and belongs to resource and environment technical field.This method comprises the following steps：Step 1：The sour mud of weight will be related to and hydrochloric acid is added to the water, heat up, potassium chlorate is added, is reacted under certain temperature, obtains the mixed liquor containing mercury chloride；Step 2：Alkali neutralization is added, controls pH, obtains containing mercury oxide precipitation and Na2SeO3Mixed solution, be separated by solid-liquid separation, by Se solution enter selenium piece-rate system recycle selenium；Step 3：The isolated mercury oxide of step 2 is precipitated into drying, rectifying is carried out using continuous vacuum rectification method, the condensed recycling of mercuryvapour of generation obtains hydrargyrum depuratum.This method is handled using wet processing, realizes efficiently separating for mercury and selenium, then produced high-purity mercury product by continuous vacuum rectifying, avoids the smoke pollution that sour mud roasting direct generates.
Description
Technical field
The invention belongs to resource and environment technical fields, and in particular to a method of extracting mercury from relating in the sour mud of weight.
Background technology
Sulfuric acid is important basic chemical industry raw material, is widely used in nonferrous smelting, petrochemical industry, textile printing and dyeing, inorganic salts
The industrial departments such as industry, rubber industry, paint industry and defence and military, pesticide medicine, process hides, coking.Produce the original of sulfuric acid
Material mainly has sulphur, troilite, non-ferrous metal metallurgy flue gas, gypsum, hydrogen sulfide and Waste Sulfuric Acid etc..Sulfuric acid industry essentially forms
The gesture that acid production with sulphur, pyrite-based sulfuric acid production and metallurgical off-gas acid-making are stood like the legs of a tripod, pyrite-based sulfuric acid production and metallurgical off-gas acid-making production
Amount reaches the 60% of sulfuric acid total output, and in rising trend year by year.Pyrite-based sulfuric acid production and flue gas acid preparing, which can all generate, largely to be related to
Weight acid mud.It relates to the sour mud of weight and mainly contains the ingredients such as Se, Hg, because raw material sources are different, Se content may be up to 2-50%, mercury content
Reachable 0.5%-5%, in addition, the heavy metal elements such as also a small amount of Pb, Zn, Cd, Cu, As, therefore the acid mud belongs to high value danger
Dangerous waste poisons environment very big if not being recycled.
The method for extracting mercury from sour mud both at home and abroad is rarely reported, and is detected in Wang Xiaowu etc.《Selenium is extracted from selenic acid mud
Experimental study》（Hydrometallurgy, 2013）Mercury method is steamed in the roasting used in one text（Pyrogenic process）, it is that will be roasted after sour mud desiccation
It burns, the condensed collection of mercuryvapour obtains.The method can recycle mercury from sour mud, but the mercury and selenium in sour mud are evaporated simultaneously, gas
State selenium dioxide can be by mercury oxidation at mercury oxide, and selenium dioxide is reduced into selenium, and the reaction of selenium mercury produces mercury selenide again, therefore not
It can realize that efficiently separating for selenium mercury, the mercury product purity of recycling are low；Flue gas is generated in technical process simultaneously to cause atmospheric environment
Pollution.
It is to store up or take out to small enterprise to be recycled, however stockpiling seriously threatens to relate to the main disposal options of the sour mud of weight at present
Ambient enviroment is taken out to small enterprise and carries out the problems such as recycling is primarily present illegal transfer dangerous waste, transport leakage, the rate of recovery is low, and
There are the uncontrollable discharge equivalent risks of waste water,waste gas and industrial residue in removal process.Therefore, research relates to valuable element in the sour mud of weight
Extractive technique, realization relates to the valuable elements recycling such as mercury in the sour mud of weight, final to realize the comprehensive utilization of resources for relating to the sour mud of weight, has pole
Big environment, social and economic benefit.
Invention content
The invention aims to solve the deficiencies in the prior art, provide a kind of from the method for relating to extraction mercury in the sour mud of weight.
This method is handled using wet processing, realizes efficiently separating for mercury and selenium, then is passed through continuous vacuum rectification method and carried out rectifying, production
The condensed recycling of raw mercuryvapour obtains hydrargyrum depuratum；The smoke pollution that sour mud roasting direct generates is avoided simultaneously.
The present invention adopts the following technical scheme that：
From the method for extracting mercury in the sour mud of weight is related to, include the following steps：
Step 1：The sour mud of weight will be related to and hydrochloric acid is added to the water, heat up, potassium chlorate is added, is reacted under certain temperature,
The mixed liquor containing mercury chloride is obtained, in the step, the mercury in sour mud is with HgCl2Form enter leachate, leaching process
Chemical reaction is as follows：
HgSe + HCl + KClO3→ H2SeO3 + KCl + HgCl2；
Step 2：Alkali neutralization is added, controls pH, obtains containing mercury oxide precipitation and Na2SeO3Mixed solution, solid-liquid point
From Se solution is entered selenium piece-rate system and recycles selenium by the separation of realization mercury and selenium, and the main chemical reactions being related to are as follows：
HCl + NaOH→ H2O + NaCl
HgCl2 + NaOH→ H2O + NaCl + HgO↓
H2SeO3 + NaOH→ Na2SeO3+ NaCl；
Step 3：The isolated mercury oxide of step 2 is precipitated into drying, rectifying, production are carried out using continuous vacuum rectification method
The condensed recycling of raw mercuryvapour obtains hydrargyrum depuratum.
Further, a concentration of 1.47 ~ 6mol/L of hydrochloric acid described in step 1.
Further, related to described in step 1 weight acid mud, hydrochloric acid, water, potassium chlorate mass ratio be 100:16~118:
100:70~80。
Further, heating described in step 1 is specially to be warming up to 50-80 DEG C.
Further, it is reacted at 50-120 DEG C in step 1, reaction time 2-7h.
Further, pH described in step 2 is 13-14.
Further, rectification temperature described in step 3 is 500 ~ 600 DEG C.
Further, the purity of hydrargyrum depuratum described in step 3 is 99.999%.
Compared with prior art, beneficial effects of the present invention：
The present invention is handled using wet processing, realizes efficiently separating for mercury and selenium under mild conditions, then pass through company
Continuous rectification under vacuum technique, obtains high-purity mercury product；The smoke pollution that sour mud roasting direct generates is avoided simultaneously.
Specific implementation mode
With reference to embodiment, the present invention is described in further detail.
It will be understood to those of skill in the art that the following example is merely to illustrate the present invention, and it should not be regarded as limiting this hair
Bright range.
The present invention's is as follows from the method for relating to extraction mercury in the sour mud of weight：
Step 1：Relate to the leaching of the sour mud of weight
Embodiment 1：1L beakers are taken to add water 100mL, stirring while opens electric furnace heating, and is gradually added into 100g and relates to weight acid
Mud（Mercurous 25.67%）And hydrochloric acid.When temperature L to 50 DEG C, it is gradually added into potassium chlorate 80g.50-70 DEG C of temperature is controlled, hydrochloric acid is dense
Spend 6mol/L, reaction time 7h, the leaching rate of mercury is up to 99.79%.
Embodiment 2：1L beakers are taken to add water 100mL, stirring while opens electric furnace heating, and is gradually added into 100g and relates to weight acid
Mud（Mercurous 25.67%）And hydrochloric acid.When temperature L to 50 DEG C, it is gradually added into potassium chlorate 70g.50-80 DEG C of temperature is controlled, hydrochloric acid is dense
Spend 4mol/L, reaction time 2h, the leaching rate of mercury is up to 98.68%.
Embodiment 3：1L beakers are taken to add water 100mL, stirring while opens electric furnace heating, and is gradually added into 100g and relates to weight acid
Mud（Mercurous 25.67%）And hydrochloric acid.When temperature L to 80 DEG C, it is gradually added into potassium chlorate 70g.Control 80-120 DEG C of temperature, hydrochloric acid
Concentration 1.47mol/L, reaction time 2h, the leaching rate of mercury is up to 99.18%.
Embodiment 4：1L beakers are taken to add water 100mL, stirring while opens electric furnace heating, and is gradually added into 100g and relates to weight acid
Mud（Mercurous 25.67%）And hydrochloric acid.When temperature L to 80 DEG C, it is gradually added into potassium chlorate 80g.Control 80-106 DEG C of temperature, hydrochloric acid
Concentration 2.16mol/L, reaction time 3h, the leaching rate of mercury is up to 99.99%.
As it can be seen that concentration of hydrochloric acid it is higher i.e. be more than 4 mol/L, can be leached under 70 DEG C of lower temperatures below, obtain 95% with
On mercury leaching rate；When controlling 80 DEG C of temperature or more, concentration of hydrochloric acid can be reduced to 3 mol/L hereinafter, also can get higher mercury
Leaching rate.
Step 2：The heavy mercury of alkalinity
Embodiment 1：The leachate 420mL generated after the sour mud acid leaching of weight is related to, sodium hydroxide is added to neutralize, control ph 13-14,
The mercury oxide slag of generation is 35.2g, mercurous 60.5% in slag, contains selenium 0.49%.
Embodiment 2：The leachate 300mL generated after the sour mud acid leaching of weight is related to, sodium hydroxide is added to neutralize, control ph 13-14,
The mercury oxide slag of generation is 31.1g, mercurous 61.15% in slag, contains selenium 0.10%.
As it can be seen that neutralizing, the mercury slag generated is mainly mercurous, and Se content is 1% hereinafter, having achieved the purpose that selenium mercury detaches.
Step 3：The continuous vacuum rectifying of mercury oxide
Continuous charging enters vacuum fine furnace after the mercury oxide that step 2 obtains is dried, and is steamed at 500 ~ 600 DEG C
It evaporates, the mercuryvapour of generation condenses to obtain hydrargyrum depuratum product, and mercury purity is up to 99.999%.
It should be understood by those skilled in the art that the present invention is not limited to the above embodiments, above-described embodiment and explanation
Merely illustrating the principles of the invention described in book, without departing from the spirit and scope of the present invention, the present invention also has
Various changes and modifications, these changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention
It is defined by the appending claims and its equivalent thereof.
Claims (6)
1. from the method for extracting mercury in the sour mud of weight is related to, which is characterized in that include the following steps：
Step 1：The sour mud of weight will be related to and hydrochloric acid is added to the water, heat up, potassium chlorate is added, is reacted, is obtained under certain temperature
Mixed liquor containing mercury chloride；
Step 2：Alkali neutralization is added, controls pH, obtains containing mercury oxide precipitation and Na2SeO3Mixed solution, be separated by solid-liquid separation, will
Se solution enters selenium piece-rate system recycling selenium；
Step 3：The isolated mercury oxide of step 2 is precipitated into drying, rectifying is carried out using continuous vacuum rectification method, generation
The condensed recycling of mercuryvapour obtains hydrargyrum depuratum；
Related to described in step 1 weight acid mud, hydrochloric acid, water, potassium chlorate mass ratio be 100:16~118:100:70~80；
Heating described in step 1 is specially to be warming up to 50-80 DEG C；
Rectification temperature described in step 3 is 500~600 DEG C.
2. according to claim 1 from the method for relating to extraction mercury in the sour mud of weight, which is characterized in that hydrochloric acid described in step 1
A concentration of 4~6mol/L.
3. according to claim 1 from the method for relating to extraction mercury in the sour mud of weight, which is characterized in that in 50-120 in step 1
It is reacted at DEG C, reaction time 2-7h.
4. according to claim 1 from relating to the method for extracting mercury in the sour mud of weight, which is characterized in that pH described in step 2 is
13-14。
5. according to claim 1 from relating to the method for extracting mercury in the sour mud of weight, which is characterized in that alkali described in step 2 is
Sodium hydroxide.
6. according to claim 1 from the method for relating to extraction mercury in the sour mud of weight, which is characterized in that refined described in step 3
The purity of mercury is 99.999%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710211864.1A CN106893865B (en) | 2017-04-01 | 2017-04-01 | From the method for relating to extraction mercury in the sour mud of weight |
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| CN201710211864.1A CN106893865B (en) | 2017-04-01 | 2017-04-01 | From the method for relating to extraction mercury in the sour mud of weight |
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| CN106893865A CN106893865A (en) | 2017-06-27 |
| CN106893865B true CN106893865B (en) | 2018-10-30 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113528836B (en) * | 2021-07-23 | 2022-07-29 | 昆明理工大学 | Method for separating and recovering selenium and mercury in acid mud by one-step method |
| CN116443821A (en) * | 2023-03-21 | 2023-07-18 | 葫芦岛锌业股份有限公司 | Method for producing selenium-rich fertilizer additive by using selenate mud |
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| CN104498722A (en) * | 2014-12-16 | 2015-04-08 | 贵州重力科技环保有限公司 | Method for comprehensively recovering mercury and selenium from metallurgical slag |
| CN104561558B (en) * | 2015-01-19 | 2017-08-04 | 北京矿冶研究总院 | Method for treating selenium-containing mercury acid mud |
| CN104828788B (en) * | 2015-04-24 | 2016-08-17 | 湘潭大学 | A kind of method extracting selenium from hydrargyrum selenic acid mud waste material |
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Inventor after: Fu Guangyi Inventor after: Zhong Yu Inventor after: Cheng Chaoyang Inventor after: Cheng Yingxiang Inventor after: Zhao Zhiqiang Inventor after: Huang Shanyun Inventor after: Xu Youze Inventor after: Xiang Renjun Inventor after: Kang Daping Inventor after: Yang Yongqiang Inventor after: Zhao Yuanyuan Inventor before: Cheng Yingxiang Inventor before: Zhong Yu Inventor before: Cheng Chaoyang Inventor before: Zhao Zhiqiang Inventor before: Huang Shanyun Inventor before: Xu Youze Inventor before: Fu Guangyi Inventor before: Xiang Renjun Inventor before: Kang Daping Inventor before: Yang Yongqiang Inventor before: Zhao Yuanyuan |
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