CN112341496A - Method for recovering benzyl arsonic acid product by using benzyl arsonic acid waste residues - Google Patents
Method for recovering benzyl arsonic acid product by using benzyl arsonic acid waste residues Download PDFInfo
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- CN112341496A CN112341496A CN202011287346.6A CN202011287346A CN112341496A CN 112341496 A CN112341496 A CN 112341496A CN 202011287346 A CN202011287346 A CN 202011287346A CN 112341496 A CN112341496 A CN 112341496A
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- CN
- China
- Prior art keywords
- benzyl
- arsonic acid
- benzyl arsonic
- acid
- sodium
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- ODQMOSYKHALMPU-UHFFFAOYSA-N benzylarsonic acid Chemical compound O[As](O)(=O)CC1=CC=CC=C1 ODQMOSYKHALMPU-UHFFFAOYSA-N 0.000 title claims abstract description 66
- 239000002699 waste material Substances 0.000 title claims abstract description 40
- 238000000034 method Methods 0.000 title claims abstract description 16
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 33
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 22
- 238000001914 filtration Methods 0.000 claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 claims abstract description 13
- 229910052708 sodium Inorganic materials 0.000 claims abstract description 13
- 239000011734 sodium Substances 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 13
- 238000001816 cooling Methods 0.000 claims abstract description 12
- 230000020477 pH reduction Effects 0.000 claims abstract description 9
- 239000000498 cooling water Substances 0.000 claims abstract description 6
- 239000013078 crystal Substances 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 230000003472 neutralizing effect Effects 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 239000000203 mixture Substances 0.000 claims abstract description 3
- 239000007787 solid Substances 0.000 claims abstract description 3
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 8
- 239000000463 material Substances 0.000 claims description 7
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 4
- 238000004064 recycling Methods 0.000 claims description 4
- PTLRDCMBXHILCL-UHFFFAOYSA-M sodium arsenite Chemical compound [Na+].[O-][As]=O PTLRDCMBXHILCL-UHFFFAOYSA-M 0.000 claims description 4
- 239000011780 sodium chloride Substances 0.000 claims description 4
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 4
- 235000011152 sodium sulphate Nutrition 0.000 claims description 4
- 239000002351 wastewater Substances 0.000 claims description 4
- 238000002425 crystallisation Methods 0.000 claims description 3
- 230000008025 crystallization Effects 0.000 claims description 3
- 230000008901 benefit Effects 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 2
- QKYKNXMQZHKSOV-UHFFFAOYSA-L disodium benzyl-dioxido-oxo-lambda5-arsane Chemical compound [Na+].[Na+].[O-][As]([O-])(=O)Cc1ccccc1 QKYKNXMQZHKSOV-UHFFFAOYSA-L 0.000 description 3
- 229910052785 arsenic Inorganic materials 0.000 description 2
- RQNWIZPPADIBDY-UHFFFAOYSA-N arsenic atom Chemical compound [As] RQNWIZPPADIBDY-UHFFFAOYSA-N 0.000 description 2
- 238000005188 flotation Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 2
- HJTAZXHBEBIQQX-UHFFFAOYSA-N 1,5-bis(chloromethyl)naphthalene Chemical compound C1=CC=C2C(CCl)=CC=CC2=C1CCl HJTAZXHBEBIQQX-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- RBFQJDQYXXHULB-UHFFFAOYSA-N arsane Chemical compound [AsH3] RBFQJDQYXXHULB-UHFFFAOYSA-N 0.000 description 1
- GOLCXWYRSKYTSP-UHFFFAOYSA-N arsenic trioxide Inorganic materials O1[As]2O[As]1O2 GOLCXWYRSKYTSP-UHFFFAOYSA-N 0.000 description 1
- KCXMKQUNVWSEMD-UHFFFAOYSA-N benzyl chloride Chemical compound ClCC1=CC=CC=C1 KCXMKQUNVWSEMD-UHFFFAOYSA-N 0.000 description 1
- 229940073608 benzyl chloride Drugs 0.000 description 1
- -1 benzylarsonic acid sodium Chemical compound 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- ZXOKVTWPEIAYAB-UHFFFAOYSA-N dioxido(oxo)tungsten Chemical compound [O-][W]([O-])=O ZXOKVTWPEIAYAB-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000002440 industrial waste Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229910052761 rare earth metal Inorganic materials 0.000 description 1
- 150000002910 rare earth metals Chemical class 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07F—ACYCLIC, CARBOCYCLIC OR HETEROCYCLIC COMPOUNDS CONTAINING ELEMENTS OTHER THAN CARBON, HYDROGEN, HALOGEN, OXYGEN, NITROGEN, SULFUR, SELENIUM OR TELLURIUM
- C07F9/00—Compounds containing elements of Groups 5 or 15 of the Periodic System
- C07F9/66—Arsenic compounds
- C07F9/70—Organo-arsenic compounds
- C07F9/74—Aromatic compounds
Abstract
A method for recovering a benzyl arsonic acid product by using benzyl arsonic acid waste residues comprises the following steps of (1) mixing a dilute sodium hydroxide solution with the benzyl arsonic acid waste residues according to a liquid-to-solid ratio of (3-5): 1, adding the mixture into a stirring tank, heating to 70-80 ℃ under a stirring state, reacting for 1-2 h, introducing cooling water for cooling and cooling until crystals are precipitated, then carrying out centrifugal filtration to obtain a solution containing sodium benzyl arsonate, adding dilute sulfuric acid into the solution for acidification treatment, and neutralizing until the pH value is 2-3; controlling the reaction temperature below 50 ℃, reacting for 1-2 h, and then performing centrifugal filtration to obtain a benzyl arsonic acid product. The method improves the comprehensive yield of the benzyl arsonic acid product, reduces the production cost, realizes the reduction and resource utilization of waste residues, achieves the purpose of changing waste into valuable, solves the problem of environmental protection, and improves the economic benefit.
Description
Technical Field
The invention relates to the technical field of comprehensive recycling methods of arsenic-containing waste residues, in particular to a method for recycling a benzyl arsonic acid product by using benzyl arsonic acid waste residues.
Background
The benzyl arsonic acid is widely applied to the flotation of cassiterite, wolframite and rare earth ore as a collecting agent and is also used for the flotation of various metal oxide ores. The production of the benzyl arsonic acid adopts sodium hydroxide solution as a solvent to react with arsenic trioxide, benzyl chloride is added at one time to react to obtain the sodium benzyl arsonate, and the sodium benzyl arsonate product is obtained by acidification with sulfuric acid, washing and drying. The waste residue generated in the benzyl arsonic acid production process is mainly obtained by carrying out reduced pressure concentration or normal pressure concentration crystallization on waste water generated in a benzyl arsonic acid production system, and is obtained by sampling and analyzing the benzyl arsonic acid waste residue, wherein the waste residue contains 25-35% of benzyl arsonic acid, 10-20% of sodium benzyl arsonate, 1-5% of sodium arsenite and a large amount of sodium sulfate and sodium chloride. At present, the quantity of the benzyl arsonic acid waste residue generated each year is about 900 tons, and the benzyl arsonic acid waste residue is mainly mixed with other industrial waste residues, cured and pretreated and then enters a landfill for stockpiling, so that the comprehensive yield of the benzyl arsonic acid is low, the resources are wasted, the waste residue quantity is large, the difficulty of safe treatment is increased, and the curing treatment cost is high. Therefore, in order to improve the comprehensive yield of the benzylarsonic acid product, reduce the production cost and realize the reduction and resource treatment of waste residues, a method for effectively recycling the arsenic-containing slag generated by a benzylarsonic acid production system is urgently needed.
Disclosure of Invention
The invention aims to effectively solve the problems in the prior art and provides a method for recovering a benzyl arsonic acid product from benzyl arsonic acid waste residue, so as to improve the comprehensive yield of the benzyl arsonic acid product, reduce the production cost and realize the reduction and resource treatment of the waste residue.
The technical scheme adopted by the invention is as follows:
a method for recovering a benzyl arsonic acid product by using benzyl arsonic acid waste residues comprises the following steps:
(1) mixing a dilute sodium hydroxide solution and the benzyl arsonic acid waste residue according to a liquid-solid mass ratio of 3-5: 1, adding the mixture into a stirring tank, heating to 70-80 ℃ under a stirring state, reacting for 1-2 h, and then introducing cooling water for cooling until crystals are precipitated;
(2) carrying out centrifugal filtration on the material obtained by cooling in the step (1) to obtain a solution containing sodium benzyl arsonate;
(3) adding dilute sulfuric acid into the solution obtained by filtering in the step (2) for acidification treatment, and neutralizing until the pH value is 2-3; controlling the reaction temperature below 50 ℃ and reacting for 1-2 h;
(4) and (4) centrifugally filtering the material subjected to the acidification reaction in the step (3) to obtain a benzyl arsonic acid product.
Further, the benzyl arsonic acid waste residue is a residue obtained by concentrating and crystallizing waste water generated by a benzyl arsonic acid production system under reduced pressure or normal pressure, and the residue contains 25-35 wt% of benzyl arsonic acid, 10-20 wt% of sodium benzyl arsonate, 1-5 wt% of sodium arsenite, sodium sulfate and sodium chloride.
Further, the concentration of the dilute sodium hydroxide solution is 3-10 wt%.
Further, the concentration of the dilute sulfuric acid is 30-40 wt%.
The invention effectively solves the problems of low comprehensive yield of the benzyl arsonic acid, resource waste, large amount of waste residues, high safety treatment difficulty and high curing treatment cost caused by the benzyl arsonic acid waste residues, improves the comprehensive yield of the benzyl arsonic acid product, reduces the production cost, realizes the reduction and resource utilization of the waste residues, achieves the aim of changing waste into valuable, solves the problem of environmental protection and improves the economic benefit.
The method has the advantages of simple process, low production cost, no generation of toxic and harmful gases such as acid gas, arsine and the like in the production process, and remarkable environment-friendly and energy-saving effects and social benefits.
Detailed Description
Example 1
A method for recovering a benzyl arsonic acid product by using benzyl arsonic acid waste residues comprises the following steps:
(1) adding 1.5Kg of 10 wt% sodium hydroxide solution and 0.5Kg of benzylarsonic acid waste residue into a stirring tank, heating to 70-80 ℃ under stirring, reacting for 1.5h, and introducing cooling water to the outside of the stirring tank for cooling until a large amount of crystals are precipitated. Centrifugally filtering the material obtained by cooling to obtain a solution mainly containing sodium benzyl arsonate;
(2) and adding 40 wt% of dilute sulfuric acid into the filtered solution of the sodium benzylarsonate for acidification treatment, neutralizing until the pH is 3, controlling the reaction temperature to be below 50 ℃, reacting for 1 hour, and then performing centrifugal filtration to obtain a product of the benzylarsonate.
The actual yield of the benzyl arsonic acid is 86.4 percent, and the waste residue is reduced by 25.3 percent.
Example 2
(1) Adding 2Kg of sodium hydroxide solution with the concentration of 5 wt% and 0.5Kg of benzylarsonic acid waste residue into a stirring tank, heating to 70-80 ℃ under stirring, reacting for 1h, and cooling with cooling water until a large amount of crystals are precipitated. Centrifugally filtering the material obtained by cooling to obtain a solution mainly containing sodium benzyl arsonate;
(2) and adding 30 wt% of dilute sulfuric acid into the filtered solution of the sodium benzylarsonate to perform acidification treatment, neutralizing until the pH is 2, controlling the reaction temperature to be below 50 ℃, reacting for 2 hours, and performing centrifugal filtration to obtain a product of the benzylarsonate.
The actual yield of the benzyl arsonic acid is 89.5 percent, and the waste residue is reduced by 36.6 percent.
Example 3
(1) Adding 2.5Kg of sodium hydroxide solution with the concentration of 3 wt% and 0.5Kg of benzyl arsonic acid waste residue into a stirring tank, heating to 70-80 ℃ under stirring, reacting for 2h, and cooling with cooling water until a large amount of crystals are separated out. Centrifugally filtering the material obtained by cooling to obtain a solution mainly containing sodium benzyl arsonate;
(2) and adding dilute sulfuric acid into the filtered solution of the sodium benzylarsonate for acidification treatment, neutralizing until the pH is 2-3, controlling the reaction temperature to be below 50 ℃, reacting for 1.5h, and then performing centrifugal filtration to obtain a product of the benzylarsonate.
The actual yield of the benzyl arsonic acid is 95.7 percent, and the waste residue is reduced by 53.8 percent.
The benzyl arsonic acid waste residue is generated by carrying out reduced pressure concentration or normal pressure concentration crystallization on waste water generated by a benzyl arsonic acid production system, and contains 25-35% of benzyl arsonic acid, 10-20% of sodium benzyl arsonate, 1-5% of sodium arsenite and a large amount of sodium sulfate and sodium chloride. The concentration of the dilute sodium hydroxide solution is 3-10%, and the dilute sodium hydroxide solution is mainly used for dissolving the benzyl arsonic acid in the benzyl arsonic acid waste residue to obtain the benzyl arsonic acid sodium solution. The concentration of the dilute sulfuric acid is 30-40%, and the dilute sulfuric acid is mainly used for acidifying the benzylarsonic acid sodium to finally obtain the benzylarsonic acid product.
Claims (4)
1. A method for recovering a benzyl arsonic acid product by using benzyl arsonic acid waste residues is characterized by comprising the following steps:
(1) mixing a dilute sodium hydroxide solution and the benzyl arsonic acid waste residue according to a liquid-solid mass ratio of 3-5: 1, adding the mixture into a stirring tank, heating to 70-80 ℃ under a stirring state, reacting for 1-2 h, and then introducing cooling water for cooling until crystals are precipitated;
(2) carrying out centrifugal filtration on the material obtained by cooling in the step (1) to obtain a solution containing sodium benzyl arsonate;
(3) adding dilute sulfuric acid into the solution obtained by filtering in the step (2) for acidification treatment, and neutralizing until the pH value is 2-3; controlling the reaction temperature below 50 ℃ and reacting for 1-2 h;
(4) and (4) centrifugally filtering the material subjected to the acidification reaction in the step (3) to obtain a benzyl arsonic acid product.
2. The method for recycling the benzyl arsonic acid product by using the benzyl arsonic acid waste residue as claimed in claim 1, wherein the benzyl arsonic acid waste residue is a residue obtained by performing reduced pressure concentration or normal pressure concentration crystallization on wastewater generated by a benzyl arsonic acid production system, and the residue contains 25-35 wt% of benzyl arsonic acid, 10-20 wt% of sodium benzyl arsonate, 1-5 wt% of sodium arsenite, sodium sulfate and sodium chloride.
3. The method for recovering the benzylarsonic acid product by using the benzylarsonic acid waste residue as claimed in claim 1 or 2, wherein the concentration of the dilute sodium hydroxide solution is 3-10 wt%.
4. The method for recovering the benzylarsonic acid product by using the benzylarsonic acid waste residue as claimed in claim 1 or 2, wherein the concentration of the dilute sulfuric acid is 30-40 wt%.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011287346.6A CN112341496A (en) | 2020-11-17 | 2020-11-17 | Method for recovering benzyl arsonic acid product by using benzyl arsonic acid waste residues |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011287346.6A CN112341496A (en) | 2020-11-17 | 2020-11-17 | Method for recovering benzyl arsonic acid product by using benzyl arsonic acid waste residues |
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| CN112341496A true CN112341496A (en) | 2021-02-09 |
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| CN202011287346.6A Pending CN112341496A (en) | 2020-11-17 | 2020-11-17 | Method for recovering benzyl arsonic acid product by using benzyl arsonic acid waste residues |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5356644A (en) * | 1976-11-04 | 1978-05-23 | Seimi Kagaku Kk | Method of recovering phenyl arsonic acid or derivative thereof |
| US5068372A (en) * | 1990-07-16 | 1991-11-26 | Cvd Incorporated | Method for the synthesis of primary arsines |
| WO2009011320A1 (en) * | 2007-07-13 | 2009-01-22 | Dowa Metals & Mining Co., Ltd. | Method of treating arsenical matter with alkali |
| CN107954562A (en) * | 2017-11-21 | 2018-04-24 | 红河砷业有限责任公司 | A kind of method of efficient process arsenic wastewater from chemical industry |
| CN108623035A (en) * | 2017-03-15 | 2018-10-09 | 郑州大学 | The recovery method of arsenic in a kind of arsenious waste solution |
-
2020
- 2020-11-17 CN CN202011287346.6A patent/CN112341496A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS5356644A (en) * | 1976-11-04 | 1978-05-23 | Seimi Kagaku Kk | Method of recovering phenyl arsonic acid or derivative thereof |
| US5068372A (en) * | 1990-07-16 | 1991-11-26 | Cvd Incorporated | Method for the synthesis of primary arsines |
| WO2009011320A1 (en) * | 2007-07-13 | 2009-01-22 | Dowa Metals & Mining Co., Ltd. | Method of treating arsenical matter with alkali |
| CN108623035A (en) * | 2017-03-15 | 2018-10-09 | 郑州大学 | The recovery method of arsenic in a kind of arsenious waste solution |
| CN107954562A (en) * | 2017-11-21 | 2018-04-24 | 红河砷业有限责任公司 | A kind of method of efficient process arsenic wastewater from chemical industry |
Non-Patent Citations (3)
| Title |
|---|
| DU PREEZ, J. G. H.，等: "Organoarsenic ligands as potential f-transition metal ion extractants. Part 1. The synthesis of some new organofluorine arsonic and arsinic acids", 《SOLVENT EXTRACTION AND ION EXCHANGE》 * |
| 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》 * |
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Application publication date: 20210209 |