CN108129516A - A kind of benzyl arsenic acid synthetic method - Google Patents
A kind of benzyl arsenic acid synthetic method Download PDFInfo
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- CN108129516A CN108129516A CN201711460526.8A CN201711460526A CN108129516A CN 108129516 A CN108129516 A CN 108129516A CN 201711460526 A CN201711460526 A CN 201711460526A CN 108129516 A CN108129516 A CN 108129516A
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Abstract
A kind of benzyl arsenic acid synthetic method, the method for the present invention press molar concentration rate ammonium hydrogen carbonate：Benzyl chloride：Arsenic trioxide is 3~5:1~1.2：1 preparation raw material；The mass concentration of the ammonium hydrogen carbonate is 10~30%；Arsenic trioxide is added in reaction kettle, adds water, stirring is started, sizes mixing；Then ammonium hydrogen carbonate is added in reaction kettle, 40~60 DEG C of reaction temperature, the reaction time is no more than 1h；Benzyl chloride is slowly added in reaction kettle again, 50~70 DEG C of reaction temperature, 5~8h of reaction time；Sulfuric acid is added in most backward reaction kettle and carries out acidizing crystal, after control liquid pH is 2~3, crystal is dehydrated, dry after obtain benzyl arsenic acid crystalline solid.The present invention have preparation process it is simple, without arsenic-containing waste residue, arsenic-containing waste water can reuse, production cost is low, the harmful and toxic gas that do not generate ammonia and nitrogen oxides etc., without using remarkable advantages such as high temperature or high pressure, energy conservation and environmental protections.
Description
Technical field
The invention belongs to field of chemical technology, and in particular to a kind of new method of benzyl arsenic acid synthesis.
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, are all as molten using sodium hydroxide
Sodium arsenite is reacted into agent with arsenic trioxide, and 70~80 DEG C of disposable benzyl chlorides that add in is kept to react into benzyl arsenic acid disodium
Salt, by stratification, the upper and lower are abandoned in shifting, and middle layer is acidified with sulfuric acid, washed, being dried to obtain benzyl arsenic acid product, are given up
The inorganic salts such as sodium sulphate are precipitated by concentration, cooling in water, and after filtering, filtrate, which returns to, prepares sodium arsenite solution.Upper strata 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 floor is nonreactive mixing residue, is mainly had containing inorganic salts, benzyl arsenic acid disodium salt and sodium arsenite etc., upper strata and under
Layer solution is difficult to handle, and lower floor is then directly entered in waste water system.There are more disproportionated reaction, arsine efficiency in this method
Low, also a large amount of inorganic arsenic is not involved in reacting；The introducing of sodium forms great amount of soluble sodium salt, and waste water and dregs intractability is big,
It is of high cost, environmental protection pressure is big, economic benefit is low, and great arsenic pollution will be caused by dealing with improperly, to society adverse effect it is huge.Cause
This, there is an urgent need to be broken through to existing benzyl arsenic acid synthetic method, to promote the industrial applications of benzyl arsenic acid.
Invention content
It is an object of the invention to arsenic-containing waste water waste residues existing for overcoming existing benzyl arsenic acid synthetic technology, cause cost
High, the problems such as environmental pollution is serious, provide a kind of preparation process it is simple, without arsenic-containing waste residue, containing recovering and reutilizing waste water, production cost
Low, energy-saving and environment-friendly benzyl arsenic acid synthetic method.
Realize that the technical solution that the object of the invention is taken is as follows：
A kind of benzyl arsenic acid synthetic method, method and step are as follows：
(1) raw material prepares：Raw materials used is ammonium hydrogen carbonate, benzyl chloride, arsenic trioxide, by molar concentration rate bicarbonate
Ammonium：Benzyl chloride：Arsenic trioxide is 3~5:1~1.2：1 preparation raw material；The mass concentration of the ammonium hydrogen carbonate is 10~30%
(2) arsenious acid reaction is carried out：Arsenic trioxide is added in reaction kettle, adds water, stirring is started, sizes mixing；Then
Ammonium hydrogen carbonate is added in reaction kettle, 40~60 DEG C of controlling reaction temperature, the reaction time is no more than 1h；
(3) arsine reaction is carried out：Benzyl chloride is slowly added in reaction kettle, 50~70 DEG C of controlling reaction temperature, during reaction
Between 5~8h；
(4) it is acidified, is dehydrated：Sulfuric acid is added in into reaction kettle and carries out acidizing crystal, after control liquid pH is 2~3, will be crystallized
Benzyl arsenic acid crystalline solid is obtained after object dehydration, drying.
Compared with prior art, the invention has the advantages that：
(1) using arsenic trioxide, ammonium hydrogen carbonate, benzyl chloride as raw material, stepwise reaction synthesis, by being layered, being acidified, taking off
Water synthesizes benzyl arsenic acid under lower temperature normal pressure, have preparation method it is simple, can reuse, life without arsenic-containing waste residue, arsenic-containing waste water
Produce it is at low cost, do not generate the harmful poisonous gas such as ammonia and nitrogen oxides, without using high temperature or high pressure, safe preparation process, section
The remarkable advantages such as energy environmental protection.
(2) building-up process is easily controllable, and benzyl arsenic acid synthetic ratio is high.
Specific embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
100g arsenic trioxides are added in reaction kettle, pulpous state is tuned into suitable quantity of water, are then 10% by mass concentration
Ammonium bicarbonate soln be added in reaction kettle, the molar ratio of arsenic trioxide and ammonium hydrogen carbonate is 3:1, stirring is started, is controlled
Reaction temperature is to react 0.5h at 50 DEG C, and mole of benzyl chloride, benzyl chloride and arsenic trioxide is slowly added into above-mentioned system
Than being 1.1:1,7h is reacted at being 60 DEG C in reaction temperature, acidizing crystal is carried out with the sulfuric acid of mass concentration 30%, controls solution
After pH is 3, crystal is dehydrated, dry after obtain benzyl arsenic acid crystalline solid, the synthetic ratio of benzyl arsenic acid is 32.7%.
Embodiment 2
100g arsenic trioxides are added in reaction kettle, pulpous state is tuned into suitable quantity of water, are then 20% by mass concentration
Ammonium bicarbonate soln be added in reaction kettle, the molar ratio of arsenic trioxide and ammonium hydrogen carbonate is 3:1, stirring is started, is controlled
Reaction temperature is to react 1h at 40 DEG C, and the molar ratio of benzyl chloride, benzyl chloride and arsenic trioxide is slowly added into above-mentioned system
It is 1.2:1,8h is reacted at being 50 DEG C in reaction temperature, acidizing crystal is carried out with the sulfuric acid of mass concentration 30%, controls pH value of solution
After 2, crystal is dehydrated, dry after obtain benzyl arsenic acid crystalline solid, the synthetic ratio of benzyl arsenic acid is 48.1%.
Embodiment 3
100g arsenic trioxides are added in reaction kettle, pulpous state is tuned into suitable quantity of water, are then 10% by mass concentration
Ammonium bicarbonate soln be added in reaction kettle, the molar ratio of arsenic trioxide and ammonium hydrogen carbonate is 4:1, stirring is started, is controlled
Reaction temperature is to react 0.5h at 45 DEG C, and mole of benzyl chloride, benzyl chloride and arsenic trioxide is slowly added into above-mentioned system
Than being 1.2:1,5h is reacted at being 70 DEG C in reaction temperature, acidizing crystal is carried out with the sulfuric acid of mass concentration 30%, controls solution
After pH is 3, crystal is dehydrated, dry after obtain benzyl arsenic acid crystalline solid, the synthetic ratio of benzyl arsenic acid is 83.9%.
Embodiment 4
100g arsenic trioxides are added in reaction kettle, pulpous state is tuned into suitable quantity of water, are then 30% by mass concentration
Ammonium bicarbonate soln be added in reaction kettle, the molar ratio of arsenic trioxide and ammonium hydrogen carbonate is 4:1, stirring is started, is controlled
Reaction temperature is to react 0.5h at 60 DEG C, and mole of benzyl chloride, benzyl chloride and arsenic trioxide is slowly added into above-mentioned system
Than being 1.2:1,7h is reacted at being 60 DEG C in reaction temperature, acidizing crystal is carried out with the sulfuric acid of mass concentration 30%, controls solution
After pH is 2, crystal is dehydrated, dry after obtain benzyl arsenic acid crystalline solid, the synthetic ratio of benzyl arsenic acid is 76.9%.
Embodiment 5
100g arsenic trioxides are added in reaction kettle, pulpous state is tuned into suitable quantity of water, are then 30% by mass concentration
Ammonium bicarbonate soln be added in reaction kettle, the molar ratio of arsenic trioxide and ammonium hydrogen carbonate is 5:1, stirring is started, is controlled
Reaction temperature is to react 1h at 50 DEG C, and the molar ratio of benzyl chloride, benzyl chloride and arsenic trioxide is slowly added into above-mentioned system
It is 1:1,5h is reacted at being 65 DEG C in reaction temperature, carries out acidizing crystal with the sulfuric acid of mass concentration 30%, control pH value of solution is 3
Afterwards, crystal is dehydrated, dry after obtain benzyl arsenic acid crystalline solid, the synthetic ratio of benzyl arsenic acid is 79.2%.
Claims (1)
1. a kind of benzyl arsenic acid synthetic method, which is characterized in that method and step is as follows：
(1) raw material prepares：Raw materials used is ammonium hydrogen carbonate, benzyl chloride, arsenic trioxide, by molar concentration rate ammonium hydrogen carbonate：Chlorine
Change benzyl：Arsenic trioxide is 3~5:1~1.2：1 preparation raw material；The mass concentration of the ammonium hydrogen carbonate is 10~30%；
(2) arsenious acid reaction is carried out：Arsenic trioxide is added in reaction kettle, adds water, stirring is started, sizes mixing；Then by carbon
Sour hydrogen ammonium is added in reaction kettle, 40~60 DEG C of controlling reaction temperature, and the reaction time is no more than 1h；
(3) arsine reaction is carried out：Benzyl chloride is slowly added in reaction kettle, 50~70 DEG C of controlling reaction temperature, the reaction time 5~
8h；
(4) it is acidified, is dehydrated：Sulfuric acid is added in into reaction kettle and carries out acidizing crystal, after control liquid pH is 2~3, crystal is taken off
Benzyl arsenic acid crystalline solid is obtained after water, drying.
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| CN201711460526.8A CN108129516A (en) | 2017-12-28 | 2017-12-28 | A kind of benzyl arsenic acid synthetic method |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN113307828A (en) * | 2021-04-26 | 2021-08-27 | 林西金易来砷业有限公司 | Synthesis process of benzyl arsonic acid |
| CN114989220A (en) * | 2022-06-28 | 2022-09-02 | 红河砷业有限责任公司 | Synthesis method of disodium methyl arsonate |
-
2017
- 2017-12-28 CN CN201711460526.8A patent/CN108129516A/en active Pending
Non-Patent Citations (3)
| Title |
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| QUICK A.J.等: "Aliphatic arsonic and arsinic acids, and aliphatic-aromatic arsinic acids", 《JOURNAL OF THE AMERICAN CHEMICAL SOCIETY》 * |
| 张洪 等: "苄基胂酸合成研究", 《云南化工》 * |
| 朱建光 等: "锡石、黑钨细泥捕收剂苄基胂酸的研制", 《中南矿冶学院学报》 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| CN113307828A (en) * | 2021-04-26 | 2021-08-27 | 林西金易来砷业有限公司 | Synthesis process of benzyl arsonic acid |
| CN114989220A (en) * | 2022-06-28 | 2022-09-02 | 红河砷业有限责任公司 | Synthesis method of disodium methyl arsonate |
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Application publication date: 20180608 |