CN111892138A - Molybdenum removal treatment process for molybdenum-containing wastewater in molybdenum smelting - Google Patents
Molybdenum removal treatment process for molybdenum-containing wastewater in molybdenum smelting Download PDFInfo
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Abstract
The invention discloses a molybdenum removal treatment process for molybdenum-containing wastewater in molybdenum smelting, which comprises the following steps: s1, adding hydroxide ions into the molybdenum smelting wastewater, precipitating, and filtering to obtain a first filtrate and a first filter residue; s2, adding soluble sulfide salt or hydrosulfide salt or soluble organic vulcanizing agent into the first filtrate, vulcanizing and precipitating, and filtering to obtain a second filtrate and a second filter residue; s3, adding soluble ferrous salt or ferric salt into the second filtrate, stirring and carrying out colloid adsorption; s4, after colloid adsorption for several hours, adding a flocculating agent and a filter aid, fully mixing, settling, and discharging or recycling the filtered filtrate after reaching the standard through detection. The invention improves the treatment effect of the molybdenum-containing wastewater by adopting a mode of vulcanization treatment and ferric salt flocculation and sedimentation, reduces the molybdenum content in the treated wastewater to be below 0.1mg/L, meets the requirements of discharge standard and recycling, and overcomes the defects of the existing molybdenum-containing wastewater treatment process.
Description
Technical Field
The invention relates to the technical field of molybdenum-containing wastewater treatment, in particular to a molybdenum-removing treatment process for molybdenum-containing wastewater in molybdenum smelting.
Background
During the deep processing of molybdenum, a large amount of molybdenum-containing wastewater is generated, such as acid precipitation mother liquor generated by a classical method, acid/alkali post-copulation liquor generated by an ion exchange method and acid/alkali washing wastewater generated by the deep processing of molybdenum.
For the treatment of molybdenum-containing wastewater, at present, the conventional method for treating molybdenum-containing wastewater generated by molybdenum smelting comprises the following steps: activated carbon adsorption, extraction, ion exchange, inorganic salt processes, RO reverse osmosis, electrodialysis, and the like are used in many cases, and the methods are mature, and RO reverse osmosis and electrodialysis are the methods which have been recently developed. The processes of activated carbon adsorption, extraction, ion exchange method, inorganic salt process and the like are complex, and the extraction method needs to be matched with corresponding oil removal equipment and process, otherwise, oil pollution can be caused; the investment of ion exchange equipment and resin is large. Several methods for treating molybdenum smelting wastewater focus on recovery, and the wastewater after treatment still contains several milligrams per liter to dozens of milligrams per liter of molybdenum, so that the problem of wastewater pollution is difficult to completely solve. The RO reverse osmosis membrane and the electrodialysis membrane jointly treat inorganic salt water, the content of molybdenum in water can be reduced to below 1mg/l to achieve recycling water, but the treatment capacity of equipment is limited, key membrane components of the RO reverse osmosis membrane and the electrodialysis membrane are easy to lose in the operation process, and the material consumption cost is high.
Disclosure of Invention
The invention aims to: aiming at the existing problems, the molybdenum-removing treatment process for molybdenum-containing wastewater from molybdenum smelting is provided, and by adopting a mode of vulcanization treatment and ferric salt flocculation and sedimentation, under the condition of using common equipment and low consumption of auxiliary materials, the treatment effect of the molybdenum-containing wastewater is improved, so that the molybdenum content in the treated wastewater is reduced to be below 0.1mg/L, the requirements of discharge standard and recycling are met, and the defects of the existing molybdenum-containing wastewater treatment process are overcome.
The technical scheme adopted by the invention is as follows: a molybdenum removal treatment process for molybdenum-containing wastewater from molybdenum smelting is characterized by comprising the following steps:
s1, neutralization and sedimentation: adding hydroxyl ions into the molybdenum smelting wastewater, adjusting the pH value of the wastewater to 6-9, precipitating, and filtering to obtain a first filtrate and a first filter residue;
s2, sulfurizing and precipitating: adding soluble sulfide salt or hydrosulfide salt or soluble organic vulcanizing agent into the first filtrate, adjusting the pH value to 6-9, vulcanizing and precipitating, and filtering to obtain a second filtrate and a second filter residue;
s3, colloid adsorption: adding soluble ferrous salt or ferric salt into the second filtrate, adjusting the pH value to 4-6.5, and stirring for colloid adsorption;
s4, flocculation and sedimentation: adding a measured flocculating agent and a measured filter aid after colloid adsorption for several hours, fully mixing, settling, filtering after supernatant is clear and transparent, and discharging or recycling filtered filtrate after the filtrate reaches the standard through detection.
In the present invention, the purpose of the neutralization sedimentation is: the molybdenum smelting wastewater generally contains more molybdenum and metal/nonmetal ions, the consumption of auxiliary materials is increased due to the direct addition of a vulcanizing agent for treatment, and the treatment effect cannot be expected, so that the pretreatment is needed, and Ca (OH) is added2Or other soluble hydroxides are introduced into hydroxyl ions, the pH value is adjusted to 6-9 by HCl/NaOH to produce calcium molybdate and metal hydroxides to form coprecipitation so as to remove most molybdenum and metal non-metal ions in the wastewater, and filter residue is recovered after filter pressing. The purpose of the sulfidation precipitation is: the filtrate after neutralization and sedimentation has less molybdenum content and other metal/non-metal ion content, and is not easy to precipitate and separate in a chemical precipitation method, therefore, the invention changes the treatment idea, and adds soluble sulfide salt or hydrosulfide salt (including H) into the filtrate2S) or is solubleOrganic vulcanizing agent (structural general formula R-CS), S2－With metal ions to produce sulfide precipitates and with MoO4 2－Generating MoS4 2－Remaining in solution, the pH of the filtrate increases due to hydrolysis of the added soluble sulfide or hydrosulfide salt, which is detrimental to the interaction with metal ions and MoO4 2－The pH value of the reaction is required to be controlled within the range of 6-9, after filtration, filter residues are recovered and treated, and the filtrate mainly contains MoS4 2－An aqueous solution of (a). The purpose of colloid adsorption is as follows: adding soluble 2-valent/3-valent iron salt such as FeSO into the filtrate after vulcanization4、FeCl3Etc. of Fe3 +Hydrolysis to Fe (OH)3Colloids, colloids with a large surface area, Fe (OH)3During colloid polymerization, part of positive charges have stronger adsorption effect on anions; MoS4 2－Is easy to be adsorbed, and the molybdenum is in the form of MoO in solution when the pH value is more than 6.54 2－When the pH is less than 6.5, molybdate radicals begin to polymerize into polymolybdate/heteropolyate radicals and the molecules become larger, which is advantageous for adsorption, so that the pH must be controlled to be less than 6.5, preferably in the range of 4 to 6.5, and the adsorption effect is better. In addition, if Fe is introduced2+，Fe2+Hydrolysis to Fe (OH)2Stirring the colloid under natural/aeration or adding an oxidant such as H2O2Readily oxidized to Fe (OH) under equal conditions3It can therefore also be used as an iron salt, with Fe (OH)2The colloid itself also has some adsorption. Furthermore, because the formed colloid is less and is dispersed in the waste water, in order to achieve the ideal separation effect, a flocculating agent and a filter aid are added into the waste water (filtrate), after filter pressing, the content of molybdenum in the filtrate is reduced to be below 0.1mg/L, and filter residues are mainly Fe (OH)3It can be used as iron-making raw material.
The treatment process of the present invention is combined with conventional iron-molybdenum coprecipitation method (Gary R. LeGendre, DonaldD. Runnelle. Removal of dissolved molybdenum from water by precipitation of ferric ion [ J]) Compared with MoO subjected to vulcanization treatment4 2－Into macromolecular anion MoS4 2－It further comprisesThe method is favorable for adsorption of colloid, the adsorption effect of the colloid is remarkably improved, the content of molybdenum in the wastewater can be reduced to be below 0.1mg/L, the index is directly improved by 1 order of magnitude, and the treated wastewater is favorable for standard discharge and recycling.
Further, in S1, hydroxide ions are introduced by adding calcium hydroxide, and the pH of the wastewater is adjusted with hydrochloric acid or sodium hydroxide. Preferably, calcium hydroxide is introduced to the hydroxide ion to facilitate the formation of a calcium molybdate precipitate to remove molybdenum.
In the present invention, the content of metal ions in the first filtrate is calculated according to the molar ratio Mo: 1, S: 1-20 adding soluble sulfide salt or hydrosulfide salt or soluble organic vulcanizing agent.
Further, the soluble sulfide salts are selected from one or more of sodium sulfide, potassium sulfide and barium sulfide; the hydrosulfide salt is selected from sodium hydrosulfide or/and potassium hydrosulfide.
In the invention, according to the content of molybdenum in the second filtrate, the content of molybdenum in a molar ratio of Mo: fe is 1: 1-500 adding soluble ferrous or ferric salts.
Further, in S3, sodium hydroxide is used to adjust the pH.
Preferably, the flocculating agent is polyacrylamide, and the filter aid is diatomite.
In the invention, the first filter residue, the second filter residue and the filter residue obtained after flocculation and sedimentation are all recovered and further treated.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that: according to the invention, by adopting the modes of neutralization and sedimentation, vulcanization treatment and ferric salt flocculation and sedimentation, under the condition of using common equipment and low consumption of auxiliary materials, the treatment effect of the molybdenum-containing wastewater is improved, the molybdenum content in the treated wastewater is reduced to be below 0.1mg/L, the treatment index is directly improved by 1 order of magnitude, the requirements of discharge standard and recycling are met, the obtained solid filter residue can be used for smelting raw materials of molybdenum, iron, copper and the like, and the defects of the existing molybdenum-containing wastewater treatment process are overcome.
Drawings
FIG. 1 is a schematic diagram of a molybdenum removal treatment process for molybdenum-containing wastewater from molybdenum smelting.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
As shown in figure 1, the molybdenum removal treatment process for molybdenum-containing wastewater from molybdenum smelting comprises the following steps:
s1, neutralization and sedimentation: adding calcium hydroxide into the molybdenum smelting wastewater, adjusting the pH value of the wastewater to 6-9 by using HCl/NaOH, precipitating, performing pressure filtration to obtain a first filtrate and a first filter residue, and recovering the first filter residue;
s2, sulfurizing and precipitating: according to the content of molybdenum and metal ions in the first filtrate, according to the mol ratio of Mo: 1, S: 1-20, adding soluble sulfide salt or hydrosulfide salt or soluble organic vulcanizing agent into the first filtrate, adjusting and keeping the pH value at 6-9, stirring for several hours, performing vulcanization and precipitation, performing pressure filtration to obtain a second filtrate and a second filter residue, and recovering the second filter residue;
s3, colloid adsorption: according to the content of molybdenum in the second filtrate, according to the mol ratio of Mo: fe is 1: 1-500 adding soluble ferrous salt or ferric salt into the second filtrate, adjusting by using sodium hydroxide and keeping the pH value at 4-6.5, stirring for several hours and then carrying out colloid adsorption;
s4, flocculation and sedimentation: after colloid adsorption for several hours, adding metered polyacrylamide (used as a flocculating agent) and diatomite (used as a filter aid), stirring for tens of minutes, fully mixing, settling, performing filter pressing after supernatant is clear and transparent, discharging or recycling filtered filtrate after the filtrate reaches the standard through detection, and recycling filter residues.
To better illustrate the effectiveness of the treatment process of the present invention, specific examples are set forth below:
example 1
The molybdenum content in certain molybdenum-smelting molybdenum-containing wastewater is about 5g/L, and the molybdenum-smelting molybdenum-containing wastewater is treated by the following process:
s1, neutralization and sedimentation: adding calcium hydroxide into the molybdenum-containing wastewater, adjusting the pH value of the wastewater to 6-8 by using HCl/NaOH, precipitating, performing pressure filtration to obtain a first filtrate and a first filter residue, and recovering the first filter residue;
s2, sulfurizing and precipitating: according to the content of molybdenum and metal ions in the first filtrate, according to the mol ratio of Mo: 1, S: 15 adding sodium sulfide into the first filtrate, adjusting and maintaining the pH value to be 6-9, stirring for 2-3 h, then performing sulfide precipitation, performing filter pressing to obtain a second filtrate and a second filter residue, and recovering the second filter residue;
s3, colloid adsorption: according to the content of molybdenum in the second filtrate, according to the mol ratio of Mo: fe is 1: 300 adding ferric chloride into the second filtrate, adjusting with sodium hydroxide and keeping the pH value at 4-6.5, stirring for 3h and then carrying out colloid adsorption;
s4, flocculation and sedimentation: after colloid adsorption for 2-3 h, adding a small amount of polyacrylamide and diatomite, adding according to the adding amount of a normal flocculating agent, stirring for 20-30 min, settling, performing filter pressing after the supernatant is clear and transparent, and detecting that the molybdenum content of the filtered filtrate is only 0.1 mg/L.
Example 2
In certain molybdenum smelting molybdenum-containing wastewater, the molybdenum content is about 100mg/L, and the treatment is carried out by the following processes:
s1, neutralization and sedimentation: adding calcium hydroxide into the molybdenum-containing wastewater, adjusting the pH value of the wastewater to 6-8 by using HCl/NaOH, precipitating, performing pressure filtration to obtain a first filtrate and a first filter residue, and recovering the first filter residue;
s2, sulfurizing and precipitating: according to the content of molybdenum and metal ions in the first filtrate, according to the mol ratio of Mo: 1, S: 10, adding sodium sulfide into the first filtrate, adjusting and maintaining the pH value to be 6-9, stirring for 2-3 h, then performing sulfide precipitation, performing filter pressing to obtain a second filtrate and a second filter residue, and recovering the second filter residue;
s3, colloid adsorption: according to the content of molybdenum in the second filtrate, according to the mol ratio of Mo: fe is 1: 200 adding ferric chloride into the second filtrate, adjusting with sodium hydroxide, keeping the pH value at 4-6.5, stirring for 3h, and performing colloid adsorption;
s4, flocculation and sedimentation: after colloid adsorption for 2-3 h, adding a small amount of polyacrylamide and diatomite, adding according to the adding amount of a normal flocculating agent, stirring for 20-30 min, settling, performing filter pressing after the supernatant is clear and transparent, and detecting that the molybdenum content of the filtered filtrate is below 0.1 mg/L.
Example 3
The molybdenum content in certain molybdenum smelting molybdenum-containing wastewater is about 20mg/L, and the molybdenum smelting wastewater is treated by the following process:
s1, neutralization and sedimentation: adding calcium hydroxide into the molybdenum-containing wastewater, adjusting the pH value of the wastewater to 6-8 by using HCl/NaOH, precipitating, performing pressure filtration to obtain a first filtrate and a first filter residue, and recovering the first filter residue;
s2, sulfurizing and precipitating: according to the content of molybdenum and metal ions in the first filtrate, according to the mol ratio of Mo: 1, S: 5 adding sodium sulfide into the first filtrate, adjusting and maintaining the pH value to be 6-9, stirring for 2-3 h, then performing sulfide precipitation, performing filter pressing to obtain a second filtrate and a second filter residue, and recovering the second filter residue;
s3, colloid adsorption: according to the content of molybdenum in the second filtrate, according to the mol ratio of Mo: fe is 1: 50 adding ferric chloride into the second filtrate, adjusting with sodium hydroxide, keeping pH at 4-6.5, stirring for 3h, and performing colloid adsorption;
s4, flocculation and sedimentation: after colloid adsorption for 2-3 h, adding a small amount of polyacrylamide and diatomite, adding according to the adding amount of a normal flocculating agent, stirring for 20-30 min, settling, performing filter pressing after the supernatant is clear and transparent, and detecting that the molybdenum content of the filtered filtrate is below 0.1 mg/L.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (8)
1. A molybdenum removal treatment process for molybdenum-containing wastewater from molybdenum smelting is characterized by comprising the following steps:
s1, neutralization and sedimentation: adding hydroxyl ions into the molybdenum smelting wastewater, adjusting the pH value of the wastewater to 6-9, precipitating, and filtering to obtain a first filtrate and a first filter residue;
s2, sulfurizing and precipitating: adding soluble sulfide salt or hydrosulfide salt or soluble organic vulcanizing agent into the first filtrate, adjusting the pH value to 6-9, vulcanizing and precipitating, and filtering to obtain a second filtrate and a second filter residue;
s3, colloid adsorption: adding soluble ferrous salt or ferric salt into the second filtrate, adjusting the pH value to 4-6.5, and stirring for colloid adsorption;
s4, flocculation and sedimentation: adding a measured flocculating agent and a measured filter aid after colloid adsorption for several hours, fully mixing, settling, filtering after supernatant is clear and transparent, and discharging or recycling filtered filtrate after the filtrate reaches the standard through detection.
2. The molybdenum-removing treatment process for molybdenum-containing wastewater from molybdenum smelting according to claim 1, wherein in S1, hydroxide ions are introduced by adding calcium hydroxide, and the pH value of the wastewater is adjusted by using hydrochloric acid or sodium hydroxide.
3. The molybdenum-removing treatment process for molybdenum-containing wastewater from molybdenum smelting according to claim 2, wherein in S2, according to the content of metal ions in the first filtrate, the ratio of Mo: 1, S: 1-20 adding soluble sulfide salt or hydrosulfide salt or soluble organic vulcanizing agent.
4. The molybdenum-removing treatment process for molybdenum-containing wastewater from molybdenum smelting according to claim 3, wherein the soluble sulfide salt is selected from one or more of sodium sulfide, potassium sulfide and barium sulfide; the hydrosulfide salt is selected from sodium hydrosulfide or/and potassium hydrosulfide.
5. The molybdenum-removing treatment process for molybdenum-containing wastewater from molybdenum smelting according to claim 4, wherein in S3, according to the content of molybdenum in the second filtrate, the ratio of Mo: fe is 1: 1-500 adding soluble ferrous or ferric salts.
6. The molybdenum-removing treatment process for molybdenum-containing wastewater from molybdenum smelting according to claim 5, wherein in S3, sodium hydroxide is used to adjust the pH.
7. The molybdenum-removing treatment process for molybdenum-containing wastewater from molybdenum smelting according to claim 1, wherein the flocculating agent is polyallylamine, and the filter aid is diatomite.
8. The molybdenum-removing treatment process for molybdenum-containing wastewater from molybdenum smelting according to any one of claims 1 to 7, wherein the first filter residue, the second filter residue and the filter residue obtained after flocculation and sedimentation are recovered and further treated.
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| CN112897752A (en) * | 2021-01-26 | 2021-06-04 | 北京师范大学 | Treatment method of domestic drinking water |
| CN114735846A (en) * | 2022-03-29 | 2022-07-12 | 信丰华锐钨钼新材料有限公司 | Method for deeply removing molybdenum in molybdenum-containing wastewater |
| CN115010185A (en) * | 2022-06-10 | 2022-09-06 | 马钢(合肥)钢铁有限责任公司 | Production method of battery-grade ferrous chloride |
| TWI794065B (en) * | 2022-03-25 | 2023-02-21 | 福誼企業股份有限公司 | Treatment method of molybdenum-containing wastewater |
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| CN109534533A (en) * | 2018-11-06 | 2019-03-29 | 金堆城钼业股份有限公司 | A kind of administering method of molybdenum calcining pickling waste waters |
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| TWI794065B (en) * | 2022-03-25 | 2023-02-21 | 福誼企業股份有限公司 | Treatment method of molybdenum-containing wastewater |
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