CN1101010A - Wet method for preparation of sodium arsenate from fume containing arsenic - Google Patents
Wet method for preparation of sodium arsenate from fume containing arsenic Download PDFInfo
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- CN1101010A CN1101010A CN 94107126 CN94107126A CN1101010A CN 1101010 A CN1101010 A CN 1101010A CN 94107126 CN94107126 CN 94107126 CN 94107126 A CN94107126 A CN 94107126A CN 1101010 A CN1101010 A CN 1101010A
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- arsenic
- add
- soda ash
- sodium
- slip
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- Inorganic Compounds Of Heavy Metals (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The present invention relates to a preparation method of sodium arsenate. It uses a tin-roasted dust as raw material, and mixes that with water to make pulp, and then adds an alkali liquor and an oxidant in the above-mentioned pulp. The above-mentioned mixed material is stirred at 50-75 deg.C, and then extracted filtered to remove residue, and then in the obtained filtrate NaOH is added, and the pH value of said solution is regulated to 12-14, said solution is boiled, filtered to remove sediment to obtain its purified liquor, further the purified liquor is concentrated and crystalized, so that the invented sodium aresenate can be made up. Said invention can implement the one-time arsenic extraction and oxydization processes, and can directly prepare sodium arsenate from arsenic contained dust by using full-wet method.
Description
The present invention relates to a kind of method of producing arsenate, particularly from arsenic-containing smoke dust, directly produce the method for sodium arseniate.
The traditional preparation process method of sodium arseniate is that arsenic-containing material is carried out oxidizing roasting, makes As
2O
3Distillation by condensation, captures, for producing purified As
2O
3, also need to carry out the secondary distillation sometimes, capture, make high-quality As
2O
3After, be equipped with NaOH and NaNO again
3, calcining (700 ℃) in stove under the high temperature.Water leaches calcinate, obtains the sodium arseniate product.
Another kind method is with nitric acid oxidation high quality white arsenic, adds alkali behind the output arsenic acid again and makes sodium arseniate.
Above-mentioned two kinds of methods all need be passed through white arsenic preparatory phase and oxidation neutralization stage, or claim two-step approach.Particularly first method prepares white arsenic needs to cause the distillation and the As of arsenic through high-temperature roasting
2O
3Flying upward of dust seriously polluted environment, and it is tediously long to show flow process again.
The objective of the invention is to overcome pyrogenic process and produce white arsenic and cause arsenic dust pollution and the tediously long shortcoming of flow process, propose the method that a kind of wet processing arsenic-containing smoke dust is directly produced sodium arseniate.
To achieve these goals, the present invention adopts after the pulp of arsenic-containing smoke dust water, under agitation slowly adds limestone powder, regulate slip pH value to 5～6, slip is heated up and maintain 50～75 ℃, add soda ash solution and industrial hydrogen peroxide, implement the leaching oxidation of arsenic, filter, filtrate adds NaOH, regulates pH value to 12～14, boils elimination sediment after 30 minutes, purify back liquid through condensing crystal, can output high-quality sodium arseniate.
Concrete grammar of the present invention is, with the stanniferous high-arsenic dust is raw material, water is 3～6 to carry out pulp by liquid-solid ratio, under condition of stirring, slowly add limestone powder, limestone powder gets with natural Wingdale abrasive dust, regulate slip pH value to 5～6, heat up and maintain 50～75 ℃, under stirring condition, soda ash solution (is contained Na
2CO
3200 grams per liters) and industrial superoxol slowly join in the slip simultaneously, leach, the arsenic in the oxidation slip.Reagent dosage is by the arsenic amount that drops into, wherein As: Na=1.40: the 1(weight ratio, down with), As: H
2O
2=1.8: 1.After finishing, reagent is warming up to 90～100 ℃ (to boiling) again, agitation leach 30 minutes, filter, filtrate adds the industrial NaOH solution about 300g/L, the filtrate pH value is transferred to 12-14, boil elimination sediment after 30 minutes, the NaOH add-on is pressed As: Na=5.0 adds, and purifies back liquid and promptly gets the product sodium arseniate through condensing crystal.
The lixiviate and the oxidation of arsenic are integrated, and the immersion liquid basic removing foreign matter is that two technology of the present invention are created point.The present invention is based on such principle: in the lixiviate oxidising process, with Na
2CO
3And H
2O
2Slowly join in the slip simultaneously, the arsenic in the flue dust is at first leached (reaction 1.) by water, because Na is arranged
2CO
3And H
2O
2Existence, the generation of oxidation of arsenic (reaction 2.) and sodium arseniate (reaction is 3.) is also just finished simultaneously.Its chemical reaction is roughly as follows:
Impurity such as the Sn in the flue dust, Fe, Zn, Pb have and enter immersion liquid on a small quantity when the lixiviate oxidation, and after adding NaOH solution, the pH value of immersion liquid raises, and these impurity all can form the insoluble compound precipitation and remove.Its process mechanism is roughly as follows:
In view of the above, in the sodium arseniate foreign matter content seldom, quality is guaranteed.
Produce sodium arseniate by method of the present invention; not only quality is guaranteed; and owing to adopt full wet process; removed the operation of high temperature pyrogenic process from, the distillation of no arsenic causes the harm of dust, water of productive use to comprise that the filter cloth wash water and the water of washing one's hands etc. all can return leaching and use; form the solution closed cycle; thereby Working environment obtains good improvement, and has protected physical environment.
The product that obtains is through sampling analysis, and its foreign matter content is as shown in the table:
Element S n Fe Pb Sb total impurities
Content % trace 0.21 trace 0.25＜1.0
Further specifying technology of the present invention with embodiment below constitutes.
Embodiment 1
Raw material, the high-arsenic dust of tin roasting output, its composition is:
（%）As??56.98，Sb??9.63，Pb??4.31，Zn?0.11，Sn?2.92，Fe?0.64。
Get described flue dust 50kg, add 150 liters of pulps of water, under agitation condition, go into limestone powder 6kg in slowly, slip is warming up to 60 ℃ after, slowly add described soda ash solution and industrial aqueous hydrogen peroxide solution simultaneously, wherein the alkaline solution add-on is 275 liters and (contains Na
2CO
3180g/L), the superoxol add-on is 60 liters and (contains H
2O
230%), finish and be warming up to 90～100 ℃ again, agitation leach 30 minutes is filtered, and goes into 40 liters of caustic soda solns (containing NaOH 25g/L) in the filtrate, boiled 30 minutes, and behind the elimination sediment, the filtrate condensing crystal, output sodium arseniate 132kg, product contains As
+ 519.24%.
Embodiment 2
Described material composition analytical results (%): 28.31 As, 6.78 Sn, 5.84 Sb, 6.43 Pb, 4.74Fe.Be the sedimentation dirt of tin roasting.
Get above-mentioned raw materials 950g, add water 5000ml and size mixing, under agitation go into limestone powder 95g in slowly; When treating slip temperature rise to 60 ℃, 450g soda ash is changed into 3000ml alkali lye and 1650ml industry H
2O
2, slowly add in the slip simultaneously, finish and promptly be warming up to 90 ℃, agitation leach 30 minutes is filtered, and filtrate adds industrial caustic soda 95g, boiled 30 minutes, behind the elimination sediment, the filtrate condensing crystal, output sodium arseniate 1011g, product contains As
+ 520.82%.
Embodiment 3
Raw material, tin calcination fume, its composition are (%): 25.14As, 25.17Sn, 2.13Sb, 4.25Pb, 1.17Zn, 8.67Fe.
Get above-mentioned raw materials 750g, with slowly adding limestone powder 70g after the 3000ml water slurryization, be warming up to 60 ℃ after, soda ash 320g is changed into 2000ml alkali lye, with 1200ml industry H
2O
2Slowly join in the slip simultaneously.Finish, be warming up to 90 ℃, agitation leach 30 minutes is filtered, and filtrate adds industrial caustic soda 65g, boils 30 minutes, and the elimination throw out is got filtrate, through condensing crystal, and output sodium arseniate 1036g, product contains As
+ 521.56%.
Claims (6)
1, a kind of method for preparing sodium arseniate, it is characterized in that the pulp of arsenic-containing smoke dust water, add limestone powder and regulate slip pH value to 5～6, be 50～75 ℃ at slurry temperature and add soda ash solution and industrial superoxol down, filtrate adds NaOH, regulates PH to 12～14, boils, the elimination sediment purifies back liquid and is prepared into sodium arseniate through condensing crystal.
2, according to the process of claim 1 wherein that described arsenic-containing smoke dust is the tin calcination fume.
3, according to the process of claim 1 wherein that described limestone powder is that natural limestone grinds powder process and gets.
4, according to the process of claim 1 wherein that described soda ash solution contains Na
2CO
3180～200g/L, described H
2O
2Solution contains H
2O
2The 30%(volume ratio).
5, according to the process of claim 1 wherein that reagent dosage is: add slip soda ash amount and press As: Na=1.40, hydrogen peroxide is pressed As: H
2O
2=1.80(is weight ratio) add, filtrate adds the amount of NaOH and presses As: Na=5.0.
6, according to the wash water closed cycle use that the process of claim 1 wherein that process produces.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94107126 CN1101010A (en) | 1994-06-10 | 1994-06-10 | Wet method for preparation of sodium arsenate from fume containing arsenic |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 94107126 CN1101010A (en) | 1994-06-10 | 1994-06-10 | Wet method for preparation of sodium arsenate from fume containing arsenic |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1101010A true CN1101010A (en) | 1995-04-05 |
Family
ID=5032833
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 94107126 Pending CN1101010A (en) | 1994-06-10 | 1994-06-10 | Wet method for preparation of sodium arsenate from fume containing arsenic |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1101010A (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000005438A1 (en) * | 1998-07-21 | 2000-02-03 | Fernz Timber Protection Limited | Electrochemical conversion of transition metal cations to anions at a higher oxidation state |
| CN103449517A (en) * | 2013-08-27 | 2013-12-18 | 昆明理工大学 | Method for preparing white arsenic from arsenic-containing dust in evaporation-free manner |
| CN105063376A (en) * | 2015-08-10 | 2015-11-18 | 中南大学 | Method for removing arsenic from arsenic-contained solution |
| CN108842170A (en) * | 2018-07-19 | 2018-11-20 | 湖南腾驰环保科技有限公司 | A kind of technique of arsenic trioxide fusion electrolysis elemental arsenic |
-
1994
- 1994-06-10 CN CN 94107126 patent/CN1101010A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000005438A1 (en) * | 1998-07-21 | 2000-02-03 | Fernz Timber Protection Limited | Electrochemical conversion of transition metal cations to anions at a higher oxidation state |
| CN103449517A (en) * | 2013-08-27 | 2013-12-18 | 昆明理工大学 | Method for preparing white arsenic from arsenic-containing dust in evaporation-free manner |
| CN103449517B (en) * | 2013-08-27 | 2014-12-31 | 昆明理工大学 | Method for preparing white arsenic from arsenic-containing dust in evaporation-free manner |
| CN105063376A (en) * | 2015-08-10 | 2015-11-18 | 中南大学 | Method for removing arsenic from arsenic-contained solution |
| CN105063376B (en) * | 2015-08-10 | 2017-10-13 | 中南大学 | A kind of method that arsenic is removed from arsenic containing solution |
| CN108842170A (en) * | 2018-07-19 | 2018-11-20 | 湖南腾驰环保科技有限公司 | A kind of technique of arsenic trioxide fusion electrolysis elemental arsenic |
| CN108842170B (en) * | 2018-07-19 | 2019-07-30 | 湖南腾驰环保科技有限公司 | A kind of technique of arsenic trioxide fusion electrolysis elemental arsenic |
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| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
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