CN108147437B - Method for producing high-purity magnesium oxide by taking magnesium arsenate as raw material - Google Patents
Method for producing high-purity magnesium oxide by taking magnesium arsenate as raw material Download PDFInfo
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- CN108147437B CN108147437B CN201810158637.1A CN201810158637A CN108147437B CN 108147437 B CN108147437 B CN 108147437B CN 201810158637 A CN201810158637 A CN 201810158637A CN 108147437 B CN108147437 B CN 108147437B
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- magnesium
- arsenate
- magnesium arsenate
- arsenic
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F5/00—Compounds of magnesium
- C01F5/02—Magnesia
- C01F5/06—Magnesia by thermal decomposition of magnesium compounds
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Abstract
The invention discloses a method for producing high-purity magnesium oxide by using magnesium arsenate as a raw material, which is characterized in that the magnesium arsenate produced in the process of treating arsenic-containing waste liquid is used as the raw material, the magnesium arsenate is purified through the processes of acid dissolution, alkaline precipitation, washing, drying and the like, and the purified magnesium arsenate is calcined to produce high-purity magnesium oxide and a simple substance arsenic product. The method has the advantages that a large amount of magnesium arsenate produced in the arsenic-containing waste liquid treatment process is deeply processed, high-purity magnesium oxide and simple substance arsenic products are produced and directly sold, the inventory of the magnesium arsenate is reduced, the economic benefit of arsenic-containing waste water treatment business is improved, and the comprehensive popularization and operation of arsenic-containing waste water treatment and comprehensive utilization technology can be effectively promoted.
Description
Technical Field
The invention belongs to the field of fine chemical engineering, relates to a method for producing magnesium oxide, and particularly relates to a method for preparing high-purity magnesium oxide by using magnesium arsenate obtained in the process of treating arsenic-containing waste liquid in the non-ferrous metal smelting industry as a raw material.
Background
Magnesium arsenate is mainly used as an insecticide or a wood preservative. The invention of the invention granted to china with patent number 2016109398598 uses arsenic-containing waste liquid formed in the production process of non-ferrous metal smelting enterprises as raw material, adds proper amount of magnesium oxide, removes elements such as iron, zinc, copper and the like step by controlling the reaction process, oxidizes trivalent arsenic ions in the liquid into divalent arsenic ions by hydrogen peroxide and fully combines with magnesium ions to produce a crude product containing magnesium arsenate components. Purifying the crude product to remove magnesium hydroxide, drying and crushing to obtain magnesium arsenate product with higher purity.
The Chinese patent application with the patent application number of 2011103156291 and the invention name of 'a comprehensive utilization method of arsenic-containing wastewater generated in the copper smelting process' discloses a method for producing magnesium oxide by using magnesium arsenate, but has the following problems: one is that magnesium arsenate has low purity, resulting in the inability to produce magnesium oxide. Specifically, since the magnesium arsenate in the above patent is a mixture of magnesium arsenate and magnesium hydroxide as the main component, the content of the purified magnesium arsenate is still less than 50%. During roasting, the excessive magnesium hydroxide and magnesium arsenate are decomposed to generate arsenic, and the arsenic is combined with the magnesium oxide generated by roasting to generate magnesium arsenide, so that the production of magnesium oxide cannot be realized. Secondly, the roasting temperature is too low, and the magnesium oxide cannot be generated.
In the absence of a reducing atmosphere, the decomposition temperature of the magnesium arsenate substance is higher than 1350 ℃, the decomposition temperature in the above patent is 900-1200 ℃, and the magnesium arsenate cannot be decomposed and magnesium oxide cannot be produced without a reducing atmosphere.
Due to the restriction of China on the use of arsenic-containing pesticides, magnesium arsenate produced by treating arsenic-containing wastewater is lost and stored in large quantities. The problem affects the economic benefits of the arsenic-containing wastewater treatment and comprehensive utilization links to a certain extent.
On the other hand, the high-purity magnesium oxide is widely used in the fields of rubber, plastics, medicine, ceramics, coating, optical materials, special steel production and the like due to high purity and fine particles, and the market demand is large.
Disclosure of Invention
The invention aims to solve the technical problem of providing a method for producing high-purity magnesium oxide by using magnesium arsenate as a raw material, which is used for producing the high-purity magnesium oxide by using the magnesium arsenate produced in the process of treating arsenic-containing waste liquid in the non-ferrous metal smelting industry as the raw material so as to improve the content of arsenic-containing waste water
The economic benefit of the treatment industry, thereby promoting the popularization of the arsenic-containing wastewater treatment technology.
The technical scheme of the invention is as follows:
a method for producing magnesium oxide by taking magnesium arsenate as a raw material is characterized by comprising the following steps:
1) acid dissolution: dissolving magnesium arsenate produced by treating arsenic-containing waste liquid in acidic liquid, adjusting pH of the liquid to completely dissolve the magnesium arsenate, and filtering the liquid to remove impurities;
2) alkali precipitation: adding alkali to adjust the pH of the filtered clear liquid in the step 1) to completely separate out magnesium arsenate, and filtering to obtain a magnesium arsenate filter cake;
3) and cleaning: adding clear water into the filter cake obtained in the step 2), stirring to completely disperse the magnesium arsenate, and filtering the liquid to obtain a washed magnesium arsenate filter cake;
4) and drying: drying and dehydrating the magnesium arsenate filter cake obtained in the step 3) to obtain magnesium arsenate particles;
5) and calcining: placing the magnesium arsenate particles obtained in the step 4) in a reducing atmosphere, and calcining at the temperature of 1000-1200 ℃ to decompose the magnesium arsenate; and collecting the calcined slag to obtain a magnesium oxide product, trapping decomposed flue gas, and cooling and crystallizing to obtain elemental arsenic powder.
Preferably, the liquid pH is adjusted <2 in step 1).
Preferably, in step 2), adding alkali to adjust the pH to be more than 10, so that all the magnesium arsenate is precipitated, and filtering to obtain a magnesium arsenate filter cake.
Preferably, the reducing atmosphere in step 5) refers to: the whole or part of the kiln hearth lining is made of graphite material.
Preferably, the graphite material lining occupies more than 30% of the area of the furnace hearth.
The invention has the following positive effects:
the invention aims at the magnesium arsenate produced by treating the arsenic-containing waste liquid, and the method comprises the steps of firstly carrying out acid dissolution, alkaline precipitation, cleaning and drying to obtain magnesium arsenate particles with higher purity, and then calcining the magnesium arsenate particles at the temperature of 1000-1200 ℃ in a reducing atmosphere to decompose the magnesium arsenate to obtain a high-purity magnesium oxide product and simple substance arsenic powder.
The method can solve the defects in the prior art for producing magnesium oxide by using magnesium arsenate, deeply process a large amount of magnesium arsenate produced in the arsenic-containing waste liquid treatment process, produce high-purity magnesium oxide and simple substance arsenic products for direct sale, reduce the inventory of magnesium arsenate, improve the economic benefit of arsenic-containing waste water treatment service, and effectively promote the comprehensive popularization and operation of arsenic-containing waste water treatment and comprehensive utilization technology.
Detailed Description
Example one
The invention is further illustrated by the following examples:
the first step is raw material preparation.
1. And (4) preparing magnesium arsenate slurry. Under normal temperature, 20Kg of magnesium arsenate prepared according to an embodiment of patent specification with patent number 2016109398598 is taken, the content of the magnesium arsenate is determined to be 92%, the magnesium arsenate is put into a stainless steel reaction tank A, 300 Kg of water is added, a stirring paddle of the stainless steel reaction tank A is started, and magnesium arsenate slurry is prepared after 20 minutes.
2. 40 Kg of 30% hydrochloric acid was prepared.
3. 30 Kg of NaOH solution with a content of 40% was prepared.
Second step of acid dissolution
Hydrochloric acid was added to the stainless steel reaction tank a in portions and the pH of the liquid was measured, and stirring was stopped when the pH of the liquid was 0.1. Pumping the liquid into a centrifugal filter for filtering, pumping the filtrate into a stainless steel reaction tank B, and collecting and concentrating filter residues.
Third step of alkaline precipitation
Starting a dispersing slurry disk of a stainless steel reaction tank B, enabling the liquid in the reaction tank to flow at a constant speed, adding 40% NaOH solution in portions, measuring the pH value of the liquid, and stopping stirring when the pH value of the liquid is 13. Pumping the liquid into a plate-and-frame filter press for filtering to obtain a purified magnesium arsenate filter cake.
The fourth step of cleaning
500 Kg of clear water was added to the stainless steel reaction tank C, and the dispersion tray was started to allow the liquid in the tank to flow rapidly. And (4) putting the magnesium arsenate filter cake obtained in the third step into a stainless steel reaction tank C in batches to completely disperse the magnesium arsenate filter cake. After 1 hour, the liquid was pumped into a plate and frame filter press for filtration to obtain a washed magnesium arsenate filter cake.
The fifth step of drying
And putting the washed magnesium arsenate filter cake into a dryer, drying at 180 ℃ for 1 hour to obtain magnesium arsenate particles.
Sixth step of calcination
Putting the magnesium arsenate particles into a graphite lining calcining furnace for calcining at 1200 ℃ for 20 minutes to completely decompose the magnesium arsenate, collecting decomposed flue gas by using a flue gas catcher gas, and cooling and crystallizing the flue gas at 80 ℃ to generate 8.2 Kg of elemental arsenic powder; and collecting the calcined slag to obtain 11.5 Kg of high-purity magnesium oxide.
Example two
The first to fifth steps are the same as in embodiment one.
Sixth step of calcination
Putting magnesium arsenate particles into a part of graphite lining (the graphite material lining accounts for 30 percent of the area of a hearth of a kiln) to be calcined at 1200 ℃ for 20 minutes to completely decompose the magnesium arsenate, collecting decomposed flue gas by using a flue gas catcher gas, and cooling and crystallizing the flue gas at 80 ℃ to generate 8.0 Kg of simple substance arsenic powder; and collecting the calcined slag to obtain 11.2 Kg of high-purity magnesium oxide.
EXAMPLE III
The first to fifth steps are the same as in embodiment one.
Sixth step of calcination
Putting magnesium arsenate particles into a part of graphite lining (the graphite material lining accounts for 30 percent of the area of a hearth of a kiln) to be calcined at the calcining temperature of 1000 ℃ for 20 minutes to completely decompose the magnesium arsenate, collecting decomposed flue gas by using a flue gas catcher gas, and cooling and crystallizing the flue gas at the temperature of 80 ℃ to generate 7.8 Kg of simple substance arsenic powder; and collecting the calcined slag to obtain 10.7 Kg of high-purity magnesium oxide.
Claims (4)
1. A method for producing magnesium oxide by taking magnesium arsenate as a raw material is characterized by comprising the following steps:
1) acid dissolution: dissolving magnesium arsenate produced by treating arsenic-containing waste liquid in acidic liquid, adjusting pH of the liquid to completely dissolve the magnesium arsenate, and filtering the liquid to remove impurities;
2) alkali precipitation: adding alkali to adjust the pH of the filtered clear liquid in the step 1) to completely separate out magnesium arsenate, and filtering to obtain a magnesium arsenate filter cake;
3) and cleaning: adding clear water into the filter cake obtained in the step 2), stirring to completely disperse the magnesium arsenate, and filtering the liquid to obtain a washed magnesium arsenate filter cake;
4) and drying: drying and dehydrating the magnesium arsenate filter cake obtained in the step 3) to obtain magnesium arsenate particles;
5) and calcining: placing the magnesium arsenate particles obtained in the step 4) in a reducing atmosphere, and calcining at the temperature of 1000-1200 ℃ to decompose the magnesium arsenate; collecting the calcined slag to obtain a magnesium oxide product, trapping decomposed flue gas, and cooling and crystallizing to obtain elemental arsenic powder;
the reducing atmosphere is as follows: the whole or part of the kiln hearth lining is made of graphite material.
2. The method of claim 1, wherein the magnesium arsenate is used as a raw material for producing magnesium oxide, and the method comprises the following steps: adjusting the pH of the liquid to be less than 2 in the step 1).
3. The method of claim 1, wherein the magnesium arsenate is used as a raw material for producing magnesium oxide, and the method comprises the following steps: adding alkali in the step 2) to adjust the pH value to be more than 10, so that the magnesium arsenate is completely separated out, and filtering to obtain a magnesium arsenate filter cake.
4. The method of claim 1, wherein the magnesium arsenate is used as a raw material for producing magnesium oxide, and the method comprises the following steps: the graphite material lining accounts for more than 30% of the area of the furnace hearth.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810158637.1A CN108147437B (en) | 2018-02-26 | 2018-02-26 | Method for producing high-purity magnesium oxide by taking magnesium arsenate as raw material |
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| CN201810158637.1A CN108147437B (en) | 2018-02-26 | 2018-02-26 | Method for producing high-purity magnesium oxide by taking magnesium arsenate as raw material |
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| CN108147437B true CN108147437B (en) | 2019-12-27 |
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| CN114836635B (en) * | 2022-03-25 | 2023-05-16 | 中南大学 | Method for preparing high-purity metal arsenic by nonferrous smelting arsenic-containing solid waste short process |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5002740A (en) * | 1987-09-21 | 1991-03-26 | Gte Products Corporation | Process for purifying molybdenum |
| CN1978992A (en) * | 2005-12-02 | 2007-06-13 | 中国科学院地理科学与资源研究所 | Safety burning method for matter containing arsenic |
| CN103031442A (en) * | 2011-10-09 | 2013-04-10 | 林建忠 | Method for comprehensively utilizing arsenious waste liquor produced in copper-smelting process |
| CN106495215A (en) * | 2016-11-02 | 2017-03-15 | 林子柯 | A kind of method for producing magnesium arsenate containing arsenic waste solution |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20140273147A1 (en) * | 2013-03-12 | 2014-09-18 | Ut-Battelle, Llc | Method for synthesizing metal oxide particles |
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- 2018-02-26 CN CN201810158637.1A patent/CN108147437B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5002740A (en) * | 1987-09-21 | 1991-03-26 | Gte Products Corporation | Process for purifying molybdenum |
| CN1978992A (en) * | 2005-12-02 | 2007-06-13 | 中国科学院地理科学与资源研究所 | Safety burning method for matter containing arsenic |
| CN103031442A (en) * | 2011-10-09 | 2013-04-10 | 林建忠 | Method for comprehensively utilizing arsenious waste liquor produced in copper-smelting process |
| CN106495215A (en) * | 2016-11-02 | 2017-03-15 | 林子柯 | A kind of method for producing magnesium arsenate containing arsenic waste solution |
Non-Patent Citations (3)
| Title |
|---|
| 含砷铜渣N2-CO气氛中还原焙烧脱砷新工艺;万新宇等;《矿冶工程》;20171231;第37卷(第6期);第80-83页 * |
| 含砷铜渣预脱砷过程的热力学分析;万新宇等;《矿冶工程》;20170228;第37卷;第73-76页 * |
| 含砷铜渣高温焙烧过程中砷的挥发行为;万新宇等;《有色金属工程》;20170831;第7卷(第4期);第40-45页 * |
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