CN108147437A - The method that high-purity magnesium oxide is produced using magnesium arsenate as raw material - Google Patents
The method that high-purity magnesium oxide is produced using magnesium arsenate as raw material Download PDFInfo
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- CN108147437A CN108147437A CN201810158637.1A CN201810158637A CN108147437A CN 108147437 A CN108147437 A CN 108147437A CN 201810158637 A CN201810158637 A CN 201810158637A CN 108147437 A CN108147437 A CN 108147437A
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- magnesium
- arsenate
- magnesium arsenate
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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
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- Manufacture And Refinement Of Metals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a kind of methods that high-purity magnesium oxide is produced using magnesium arsenate as raw material, it is to handle the magnesium arsenate produced during arsenious waste solution as raw material, by being purified in processes such as acid molten, alkali is analysed, washing, drying to magnesium arsenate, the magnesium arsenate of purification produces high-purity magnesium oxide and elemental arsenic product after calcining.Deep processing is carried out to a large amount of magnesium arsenates produced in arsenious waste solution processing procedure, produce high-purity magnesium oxide and elemental arsenic direct distribution, reduce magnesium arsenate inventory, the economic benefit of arsenic-containing waste water processing business is improved, arsenic-containing waste water processing and the all-round popularization and operation of comprehensive utilization technique can be effectively facilitated.
Description
Technical field
The invention belongs to field of fine chemical, are related to a kind of production method of magnesium oxide, and in particular to a kind of to have handled
The magnesium arsenate obtained during non-ferrous metal smelting industry arsenious waste solution is the method that raw material prepares high-purity magnesium oxide.
Background technology
Magnesium arsenate is mainly used as insecticide or timber preservative.The China of Patent No. 2016109398598 authorizes hair
Bright patent is added suitable magnesia, is passed through using the arsenious waste solution formed in non-ferrous metal metallurgy enterprise production process as raw material
Control reaction process, step by step except elements such as de-iron, zinc, copper after, by hydrogen peroxide by the trivalent arsenic ionic oxide formation in liquid into
Divalent arsenic ion simultaneously carries out abundant chemical combination with magnesium ion, produces the crude product containing magnesium arsenate composition.Crude product is purified, is removed
Magnesium hydroxide composition is removed, the higher arsenic acid magnesium products of purity are obtained after drying, pulverization process.
Number of patent application is 2011103156291, entitled " arsenic-containing waste water generated during a kind of smelting copper it is comprehensive and
The Chinese invention patent application of the method utilized " discloses a kind of utilization magnesium arsenate and produces method of magnesium oxide, but there are following
Problem：First, magnesium arsenate purity is low, lead to not generate magnesia.Specifically, the master due to the magnesium arsenate in above-mentioned patent
Wanting composition, the arsenic acid content of magnesium after purification is still less than 50% for magnesium arsenate and the mixture of magnesium hydroxide.In roasting process, mistake
The magnesium hydroxide of amount decomposes generation arsenic with magnesium arsenate, and the magnesia chemical combination that this part arsenic generates again with roasting generates magnesium arsenide, no
It can realize the production of magnesia.Second is that calcination temperature is too low, magnesia can not be generated.
Under conditions of no reducing atmosphere, the decomposition temperature of magnesium arsenate substance is higher than 1350 DEG C, point in above-mentioned patent
Temperature is solved for 900 DEG C -1200 DEG C and without reducing atmosphere, magnesium arsenate cannot decompose, and can not produce magnesia.
Due to limitation of the China to the Pesticide use containing arsenic, cause the magnesium arsenate for handling arsenic-containing waste water production unsalable, great Liang Ku
It deposits.The appearance of this problem affects the economic benefit of arsenic-containing waste water processing and comprehensive utilization link to a certain extent.
On the other hand, high-purity magnesium oxide is because purity is high, particle is thin, be widely used in rubber, plastics, medicine, ceramics, coating,
The fields such as optical material, extraordinary steel production, the huge market demand.
Invention content
The technical problem to be solved by the invention is to provide a kind of sides that high-purity magnesium oxide is produced using magnesium arsenate as raw material
Method produces high-purity magnesium oxide, to carry to handle the magnesium arsenate produced during non-ferrous metal metallurgy industry arsenious waste solution as raw material
High arsenic-containing waste water
The economic benefit for the treatment of industry, so as to promote the popularization of arsenic-containing waste water treatment technology.
Technical scheme is as follows：
One kind produces method of magnesium oxide by raw material of magnesium arsenate, it is characterised in that includes the following steps:
1）, acid it is molten：The magnesium arsenate for handling arsenious waste solution production is dissolved in acidic liquid, liquid pH is adjusted, makes magnesium arsenate complete
Portion is dissolved, and filtering liquid removes impurity；
2）, alkali analysis：Add alkali set-up procedure 1）In cross cleaner liquid pH, make magnesium arsenate all be precipitated, it is filtered, obtain magnesium arsenate filter
Cake；
3）, cleaning：By step 2）Gained filter cake adds clear water to be stirred, and is completely dispersed magnesium arsenate, filters liquid, is washed
Magnesium arsenate filter cake afterwards；
4）, drying：By step 3）Gained magnesium arsenate filter cake drying and dewatering, obtains arsenic acid magnesium granules；
5）, calcining：By step 4）Gained arsenic acid magnesium granules are placed under reducing atmosphere, are forged under 1000 DEG C~1200 DEG C environment
It burns, decomposes magnesium arsenate；It collects calcining slag and obtains magnesium oxide product, trapping decomposes flue gas, elemental arsenic is obtained after crystallisation by cooling
Powder.
Preferably, step 1）Middle adjustment liquid pH<2.
Preferably, step 2）In plus alkali adjustment pH>10, magnesium arsenate is made all to be precipitated, it is filtered, obtain magnesium arsenate filter cake.
Preferably, step 5）The reducing atmosphere refers to：Kiln hearth inner lining is graphite material in whole or in part.
Preferably, graphite material liner accounts for more than the 30% of kiln burner hearth area.
The good effect that the present invention has:
The present invention carries out molten acid, alkali analysis, cleaning and drying, obtains purity first for the magnesium arsenate of processing arsenious waste solution production
Higher obtains magnesium arsenate pellet, is then calcined under 1000 DEG C~1200 DEG C environment under reducing atmosphere, makes magnesium arsenate
Decomposition obtains high-purity magnesium oxide product and elemental arsenic powder.
By using the method for the present invention, deficiency present in current magnesium arsenate production magnesia technology can be solved, to containing
The a large amount of magnesium arsenates produced in arsenic waste solution processing procedure carry out deep processing, produce high-purity magnesium oxide and elemental arsenic product is directly sold
It sells, reduces magnesium arsenate inventory, improve the economic benefit of arsenic-containing waste water processing business, arsenic-containing waste water processing can be effectively facilitated
With the all-round popularization and operation of comprehensive utilization technique.
Specific embodiment
Embodiment one
It is further illustrated the present invention with reference to embodiment：
First step raw material prepares.
1st, magnesium arsenate slurry is modulated.Under normal temperature environment, the patent specification according to Patent No. 2016109398598 is taken
Magnesium arsenate 20Kg prepared by embodiment, arsenic acid content of magnesium is 92% after measured, adds 300 Kg of water after input stainless steel reaction tank A, opens
Dynamic stainless steel reaction tank A agitating paddles, are made magnesium arsenate slurry after twenty minutes.
2nd, prepare 30% hydrochloric acid of concentration, 40 Kg.
3rd, prepare 30 Kg of content 40%NaOH solution.
Second step acid is molten
Hydrochloric acid is added in stainless steel reaction tank A by several times and measure liquid pH value, stop stirring when liquid pH value=0.1.By liquid
Body is pumped into centrifugal filter and is filtered, and filtrate is pumped into stainless steel reaction tank B, collects filter residue centralized processing.
Third step alkali analysis
Start stainless steel reaction tank B dispersion pulp disks, the liquid in retort is made at the uniform velocity to flow, add in 40%NaOH solution simultaneously by several times
Liquid pH value is measured, stops stirring when liquid pH value=13.Liquid is pumped into plate and frame type filter-press to be filtered, is purified
Magnesium arsenate filter cake afterwards.
4th step is cleaned
Add 500 Kg of clear water to stainless steel reaction tank C, start dispersion pulp disk, the liquid in tank is made quickly to flow.By third step
Obtained magnesium arsenate filter cake puts into stainless steel reaction tank C by several times, is completely dispersed magnesium arsenate filter cake.It, will be by liquid pump after 1 hour
Enter plate and frame type filter-press to be filtered, the magnesium arsenate filter cake after being cleaned.
5th step is dried
By the magnesium arsenate filter cake after cleaning, drying machine is put into, 180 DEG C of drying temperature, obtains magnesium arsenate at 1 hour drying time
Material.
6th step is calcined
Arsenic acid magnesium granules are put into graphite liner calcining furnace to calcine, 1200 DEG C of calcination temperature, calcination time 20 minutes makes
Magnesium arsenate decomposes completely, is collected with Fume collector gas and decomposes flue gas, at a temperature of 80 DEG C, flue gas cooling, crystallization generation simple substance
8.2 Kg of arsenic powder end；Calcining slag is collected, obtains 11.5 Kg of high-purity magnesium oxide.
Embodiment two
First to the 5th step is the same as embodiment one.
6th step is calcined
Arsenic acid magnesium granules are put into part graphite liner（Graphite material liner accounts for the 30% of kiln burner hearth area）Calcining furnace carries out
Calcining, 1200 DEG C of calcination temperature, calcination time 20 minutes make magnesium arsenate decompose completely, are collected with Fume collector gas and decompose cigarette
Gas, at a temperature of 80 DEG C, flue gas cooling, 8.0 Kg of crystallization generation elemental arsenic powder；Calcining slag is collected, obtains high-purity magnesium oxide
11.2 Kg。
Embodiment three
First to the 5th step is the same as embodiment one.
6th step is calcined
Arsenic acid magnesium granules are put into part graphite liner（Graphite material liner accounts for the 30% of kiln burner hearth area）Calcining furnace carries out
Calcining, 1000 DEG C of calcination temperature, calcination time 20 minutes make magnesium arsenate decompose completely, are collected with Fume collector gas and decompose cigarette
Gas, at a temperature of 80 DEG C, flue gas cooling, 7.8 Kg of crystallization generation elemental arsenic powder；Calcining slag is collected, obtains high-purity magnesium oxide
10.7 Kg。
Claims (5)
1. a kind of produce method of magnesium oxide by raw material of magnesium arsenate, it is characterised in that includes the following steps:
1）, acid it is molten：The magnesium arsenate for handling arsenious waste solution production is dissolved in acidic liquid, liquid pH is adjusted, makes magnesium arsenate complete
Portion is dissolved, and filtering liquid removes impurity；
2）, alkali analysis：Add alkali set-up procedure 1）In cross cleaner liquid pH, make magnesium arsenate all be precipitated, it is filtered, obtain magnesium arsenate filter
Cake；
3）, cleaning：By step 2）Gained filter cake adds clear water to be stirred, and is completely dispersed magnesium arsenate, filters liquid, is washed
Magnesium arsenate filter cake afterwards；
4）, drying：By step 3）Gained magnesium arsenate filter cake drying and dewatering, obtains arsenic acid magnesium granules；
5）, calcining：By step 4）Gained arsenic acid magnesium granules are placed under reducing atmosphere, are forged under 1000 DEG C~1200 DEG C environment
It burns, decomposes magnesium arsenate；It collects calcining slag and obtains magnesium oxide product, trapping decomposes flue gas, elemental arsenic is obtained after crystallisation by cooling
Powder.
2. method of magnesium oxide is produced by raw material of magnesium arsenate as described in claim 1, it is characterised in that：Step 1）Middle adjustment
Liquid pH<2.
3. method of magnesium oxide is produced by raw material of magnesium arsenate as described in claim 1, it is characterised in that：Step 2）In plus alkali
Adjust pH>10, magnesium arsenate is made all to be precipitated, it is filtered, obtain magnesium arsenate filter cake.
4. method of magnesium oxide is produced by raw material of magnesium arsenate as described in claim 1, it is characterised in that：Step 5）It is described to go back
Primordial Qi atmosphere refers to：Kiln hearth inner lining is graphite material in whole or in part.
5. method of magnesium oxide is produced by raw material of magnesium arsenate as claimed in claim 4, it is characterised in that：Graphite material liner
Account for more than 30% kiln burner hearth area.
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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 CN108147437B (en) | 2019-12-27 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114836635A (en) * | 2022-03-25 | 2022-08-02 | 中南大学 | Method for preparing high-purity metal arsenic by using non-ferrous smelting arsenic-containing solid waste short process |
Citations (5)
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|---|---|---|---|---|
| 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 |
| US20140273147A1 (en) * | 2013-03-12 | 2014-09-18 | Ut-Battelle, Llc | Method for synthesizing metal oxide particles |
| CN106495215A (en) * | 2016-11-02 | 2017-03-15 | 林子柯 | A kind of method for producing magnesium arsenate containing arsenic waste solution |
-
2018
- 2018-02-26 CN CN201810158637.1A patent/CN108147437B/en active Active
Patent Citations (5)
| 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 |
| US20140273147A1 (en) * | 2013-03-12 | 2014-09-18 | Ut-Battelle, Llc | Method for synthesizing metal oxide particles |
| 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 |
|---|
| 万新宇等: "含砷铜渣N2-CO气氛中还原焙烧脱砷新工艺", 《矿冶工程》 * |
| 万新宇等: "含砷铜渣预脱砷过程的热力学分析", 《矿冶工程》 * |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114836635A (en) * | 2022-03-25 | 2022-08-02 | 中南大学 | Method for preparing high-purity metal arsenic by using non-ferrous smelting arsenic-containing solid waste short process |
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