CN108358969A - A method of synthesizing benzyl arsenic acid with arsenic-containing smoke dust is smelted - Google Patents
A method of synthesizing benzyl arsenic acid with arsenic-containing smoke dust is smelted Download PDFInfo
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- CN108358969A CN108358969A CN201711457608.7A CN201711457608A CN108358969A CN 108358969 A CN108358969 A CN 108358969A CN 201711457608 A CN201711457608 A CN 201711457608A CN 108358969 A CN108358969 A CN 108358969A
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Abstract
A method of benzyl arsenic acid being synthesized with arsenic-containing smoke dust is smelted, the arsenic-containing smoke dust that the arsenic mass content that smelting non-ferrous metal generates is 20 70% is added in reaction kettle, water is added, stirs, sizes mixing；Molar concentration rate sodium hydroxide is pressed again:Arsenic is 5~7:1 is added to the sodium hydroxide solution of mass concentration 20~40% in reaction kettle, and controlling reaction temperature is 40~60 DEG C, reacts filtration, purification after 1h, and filtrate is stayed in a kettle；Molar concentration rate benzyl chloride is pressed again：Arsenic is 1.2~1.5：1 is slowly added in benzyl chloride to reaction kettle, and controlling reaction temperature is 80~100 DEG C, 5~8h of time；Finally into reaction kettle, addition sulfuric acid carries out acidizing crystal, after control pH value of solution is 2~3, will obtain benzyl arsenic acid crystalline solid after crystal dehydration, drying.The present invention have the arsenic-containing smoke dust that preparation process is simple, non-ferrous metal metallurgy can be made to generate carry out the valuable metal after dearsenification be recycled, be at low cost, arsenic-containing waste water can reuse, do not use the remarkable advantages such as high temperature or high pressure, energy conservation and environmental protection.
Description
Technical field
The invention belongs to technical field of smelting, and in particular to the new method for smelting arsenic-containing smoke dust synthesis benzyl arsenic acid.
Background technology
Benzyl arsenic acid is widely used in the flotation of cassiterite, wolframite and Rare Earth Mine a variety of as collecting agent and flotation
The collecting agent of metal oxide ore.There are many synthetic method relevant report of benzyl arsenic acid at present, and the sodium hydroxide all used is as molten
Sodium arsenite is reacted into agent with arsenic trioxide, is kept for 70~80 DEG C be added at one time benzyl chloride reaction into benzyl arsenic acid disodium
Salt, by stratification, the upper and lower are abandoned in shifting, and middle layer sulfuric acid is acidified, washs, being dried to obtain benzyl arsenic acid product, are given up
Water is by concentration, and cooling, the inorganic salts such as precipitation sodium sulphate, after filtering, filtrate, which returns to, prepares sodium arsenite solution.Upper layer is thick benzyl
Alcohol, be in strong alkali solution the disproportionated reaction of benzyl chloride and obtain, in ingredient contain benzylalcohol, benzyl arsenic acid disodium salt and sodium arsenite
Deng；Lower layer is nonreactive mixing residue, is mainly had containing inorganic salts, benzyl arsenic acid disodium salt and sodium arsenite etc., upper layer and under
Layer solution is difficult to handle, and lower layer is then directly entered in waste water system.The raw material arsenic trioxide used in this method is to pass through
Arsenic-containing material extracts to obtain, higher price, opposite to increase production cost.
Invention content
It is an object of the invention to solve the problems, such as that the prior art exists, provides simple using a kind of preparation process and can have
Effect recycling valuable metal, realize comprehensive utilization of resources in the non-ferrous metal metallurgies such as tin, copper, lead, zinc generate waste contain arsenic
New method of the flue dust as Material synthesis benzyl arsenic acid.
The purpose of the present invention is achieved through the following technical solutions：
A method of benzyl arsenic acid being synthesized with arsenic-containing smoke dust is smelted, method and step is as follows：
(1) arsenious acid reacts：The arsenic-containing smoke dust that the arsenic mass content that smelting non-ferrous metal generates is 20-70% is added to
In reaction kettle, add water, starts stirring, size mixing；Then molar concentration rate sodium hydroxide is pressed:Arsenic is 5~7:1 by mass concentration 20~
40% sodium hydroxide solution is added in reaction kettle, and controlling reaction temperature is 40~60 DEG C, reacts filtration, purification after 1h, filtrate
It stays in a kettle；
(2) arsineization is reacted：By molar concentration rate benzyl chloride：Arsenic is 1.2~1.5：1 is slowly added to benzyl chloride to reaction kettle
In, controlling reaction temperature is 80~100 DEG C, 5~8h of reaction time；
(3) it is acidified, is dehydrated：Sulfuric acid is added into reaction kettle and carries out acidizing crystal, after control pH value of solution is 2~3, crystal
Benzyl arsenic acid crystalline solid is obtained after dehydration, drying.
Compared with prior art, the invention has the advantages that
(1) the waste arsenic-containing smoke dust generated using non-ferrous metal metallurgies such as tin, copper, lead, zinc passes through substep as primary raw material
Pulp leaches, purification, reaction synthesis, obtain benzyl arsenic acid by layering, acidification, dehydration synthesis, have that preparation method is simple, contains
The remarkable advantages such as arsenic recovering and reutilizing waste water, production cost be low, safe preparation process, energy conservation and environmental protection.
(2) building-up process is easily controllable, and benzyl arsenic acid synthetic ratio is high.
(3) so that tin, copper, lead, zinc etc. is smelted valuable metal after arsenic-containing smoke dust carries out dearsenification and be recycled utilization, production is used
Cost containing arsenic raw material substantially reduces, and realizes comprehensive utilization of resources, may advantageously facilitate the sound development of non-ferrous metal metallurgy industry
With the industrialized production for realizing benzyl arsenic acid.
Specific implementation mode
With reference to embodiment, the invention will be further described.
Embodiment 1
100g is smelted arsenic-containing smoke dust (arsenic mass content be 66.8%) in arsenic-containing smoke dust to be added in reaction kettle, with suitable
Amount water be tuned into pulpous state, then by mass concentration be 40% sodium hydroxide solution be added in reaction kettle, sodium hydroxide with contain arsenic
The molar ratio of arsenic is 5 in flue dust:1, stirring is started, controlling reaction temperature is to react 1h at 50 DEG C.Filtration, purification after reaction,
Filtrate is stayed in a kettle, and filter residue returns to smelting procedure.Backward reaction kettle in be slowly added to benzyl chloride, benzyl chloride and arsenic rub
You are than being 1.2:1,7h is reacted at being 90 DEG C in reaction temperature, then the sulfuric acid progress acid of mass concentration 40% is added into reaction kettle
Change crystallization after control pH value of solution is 3, will obtain benzyl arsenic acid crystalline solid, the synthetic ratio of benzyl arsenic acid after crystal dehydration, drying
It is 45.6%.
Embodiment 2
100g is smelted arsenic-containing smoke dust (arsenic mass content be 20%) in arsenic-containing smoke dust to be added in reaction kettle, with appropriate
Water is tuned into pulpous state, and then the sodium hydroxide solution that mass concentration is 40% is added in reaction kettle, sodium hydroxide and cigarette containing arsenic
The molar ratio of arsenic is 5 in dirt:1, stirring is started, controlling reaction temperature is to react 1h at 40 DEG C.Filtration, purification after reaction, filter
Liquid stays in a kettle, and filter residue returns to smelting procedure.Backward reaction kettle in be slowly added to benzyl chloride, mole of benzyl chloride and arsenic
Than being 1.3:1,8h is reacted at being 80 DEG C in reaction temperature, then the sulfuric acid of addition mass concentration 40% is acidified into reaction kettle
Crystallization after control pH value of solution is 2, will obtain benzyl arsenic acid crystalline solid, the synthetic ratio of benzyl arsenic acid is after crystal dehydration, drying
58.1%.
Embodiment 3
100g is smelted arsenic-containing smoke dust (arsenic mass content be 71.2%) in arsenic-containing smoke dust to be added in reaction kettle, with suitable
Amount water be tuned into pulpous state, then by mass concentration be 40% sodium hydroxide solution be added in reaction kettle, sodium hydroxide with contain arsenic
The molar ratio of arsenic is 6 in flue dust:1, stirring is started, controlling reaction temperature is to react 1h at 60 DEG C.Filtration, purification after reaction,
Filtrate is stayed in a kettle, and filter residue returns to smelting procedure.Backward reaction kettle in be slowly added to benzyl chloride, benzyl chloride and arsenic rub
You are than being 1.4:1,5h is reacted at being 100 DEG C in reaction temperature, then the sulfuric acid progress of mass concentration 40% is added into reaction kettle
Acidizing crystal after control pH value of solution is 3, will obtain benzyl arsenic acid crystalline solid, the synthesis of benzyl arsenic acid after crystal dehydration, drying
Rate is 63.4%.
Embodiment 4
100g is smelted arsenic-containing smoke dust (arsenic mass content be 70%) in arsenic-containing smoke dust to be added in reaction kettle, with appropriate
Water is tuned into pulpous state, and then the sodium hydroxide solution that mass concentration is 30% is added in reaction kettle, sodium hydroxide and cigarette containing arsenic
The molar ratio of arsenic is 6 in dirt:1, stirring is started, controlling reaction temperature is to react 1h at 55 DEG C.Filtration, purification after reaction, filter
Liquid stays in a kettle, and filter residue returns to smelting procedure.Backward reaction kettle in be slowly added to benzyl chloride, mole of benzyl chloride and arsenic
Than being 1.5:1,6h is reacted at being 85 DEG C in reaction temperature, then the sulfuric acid of addition mass concentration 40% is acidified into reaction kettle
Crystallization after control pH value of solution is 2, will obtain benzyl arsenic acid crystalline solid, the synthetic ratio of benzyl arsenic acid is after crystal dehydration, drying
78.9%.
Embodiment 5
100g is smelted arsenic-containing smoke dust (arsenic mass content in arsenic-containing smoke dust is 32,5%) to be added in reaction kettle, with suitable
Amount water be tuned into pulpous state, then by mass concentration be 20% sodium hydroxide solution be added in reaction kettle, sodium hydroxide with contain arsenic
The molar ratio of arsenic is 7 in flue dust:1, stirring is started, controlling reaction temperature is to react 1h at 50 DEG C.Filtration, purification after reaction,
Filtrate is stayed in a kettle, and filter residue returns to smelting procedure.Backward reaction kettle in be slowly added to benzyl chloride, benzyl chloride and arsenic rub
You are than being 1.5:1,5h is reacted at being 95 DEG C in reaction temperature, then the sulfuric acid progress acid of mass concentration 40% is added into reaction kettle
Change crystallization after control pH value of solution is 3, will obtain benzyl arsenic acid crystalline solid, the synthetic ratio of benzyl arsenic acid after crystal dehydration, drying
It is 85.2%.
Claims (1)
1. a kind of method for smelting arsenic-containing smoke dust synthesis benzyl arsenic acid, which is characterized in that method and step is as follows：
(1) arsenious acid reacts：The arsenic-containing smoke dust that the arsenic mass content that smelting non-ferrous metal generates is 20-70% is added to reaction
In kettle, add water, starts stirring, size mixing；Then molar concentration rate sodium hydroxide is pressed:Arsenic is 5~7:1 by mass concentration 20~40%
Sodium hydroxide solution be added in reaction kettle, controlling reaction temperature is 40~60 DEG C, reacts filtration, purification after 1h, filtrate stays in
In reaction kettle；
(2) arsineization is reacted：By molar concentration rate benzyl chloride：Arsenic is 1.2~1.5：1 is slowly added in benzyl chloride to reaction kettle, control
Reaction temperature processed is 80~100 DEG C, 5~8h of reaction time；
(3) it is acidified, is dehydrated：Sulfuric acid is added into reaction kettle and carries out acidizing crystal, after control pH value of solution is 2~3, crystal is de-
Benzyl arsenic acid crystalline solid is obtained after water, drying.
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| CN201711457608.7A CN108358969A (en) | 2017-12-28 | 2017-12-28 | A method of synthesizing benzyl arsenic acid with arsenic-containing smoke dust is smelted |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109182764A (en) * | 2018-09-30 | 2019-01-11 | 昆明理工大学 | A kind of soda acid joint clean method of Copper making flue dust synthetical recovery |
| CN109265483A (en) * | 2018-10-11 | 2019-01-25 | 云南省环境工程评估中心 | A kind of method of arsenic sulfide slag comprehensive utilization |
| CN109306408A (en) * | 2018-11-29 | 2019-02-05 | 中南大学 | A kind of ilmenite flue dust arsenic removal and the method for recycling valuable metal |
| CN110282805A (en) * | 2019-07-22 | 2019-09-27 | 红河砷业有限责任公司 | A kind of method of comprehensive utilization of waste acid containing arsenic that flue gas during smelting generates |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109182764A (en) * | 2018-09-30 | 2019-01-11 | 昆明理工大学 | A kind of soda acid joint clean method of Copper making flue dust synthetical recovery |
| CN109265483A (en) * | 2018-10-11 | 2019-01-25 | 云南省环境工程评估中心 | A kind of method of arsenic sulfide slag comprehensive utilization |
| CN109306408A (en) * | 2018-11-29 | 2019-02-05 | 中南大学 | A kind of ilmenite flue dust arsenic removal and the method for recycling valuable metal |
| CN109306408B (en) * | 2018-11-29 | 2019-12-31 | 中南大学 | Method for removing arsenic from ilmenite smoke dust and recycling valuable metals |
| CN110282805A (en) * | 2019-07-22 | 2019-09-27 | 红河砷业有限责任公司 | A kind of method of comprehensive utilization of waste acid containing arsenic that flue gas during smelting generates |
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Application publication date: 20180803 |