CN114735846A - Method for deeply removing molybdenum in molybdenum-containing wastewater - Google Patents
Method for deeply removing molybdenum in molybdenum-containing wastewater Download PDFInfo
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B34/00—Obtaining refractory metals
- C22B34/30—Obtaining chromium, molybdenum or tungsten
- C22B34/34—Obtaining molybdenum
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/008—Wet processes by an alkaline or ammoniacal leaching
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/16—Nature of the water, waste water, sewage or sludge to be treated from metallurgical processes, i.e. from the production, refining or treatment of metals, e.g. galvanic wastes
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2301/00—General aspects of water treatment
- C02F2301/08—Multistage treatments, e.g. repetition of the same process step under different conditions
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention relates to the field of rare metal smelting, in particular to a method for deeply removing molybdenum from molybdenum smelting wastewater, which comprises the steps of adjusting pH to D318 resin for adsorption and pre-removing molybdenum, adjusting pH, deeply removing molybdenum from ferric salt precipitation, filtering, regenerating and the like. The method comprises the steps of firstly adjusting the pH value of molybdenum-containing wastewater from molybdenum smelting, then adsorbing by using D318 resin, removing molybdenum in advance, then adjusting the pH value, deeply removing molybdenum by using ferric salt, filtering, collecting and recycling filter residue, collecting and treating filtrate, and realizing deep removal of molybdenum in the molybdenum-containing wastewater.
Description
[ technical field ] A
The invention relates to the field of rare metal smelting, in particular to a method for deeply removing molybdenum in molybdenum-containing wastewater.
[ background of the invention ]
Molybdenum is a strategic metal and plays an important role in the fields of fine chemical engineering, major industry, medical appliances and the like. In the molybdenum smelting process, wastewater containing molybdenum is generated, and if molybdenum is not deeply removed, excessive molybdenum can enter an underground water system to pollute drinking water and bring about the safety problem of the drinking water. The biological properties of molybdenum, which is an essential trace element for not only plants but also animals, are also important. However, the concentration of molybdenum element in water is too high, which has great harm to the life health of human body, and can cause the obstruction of the energy metabolism process in vivo, myocardial hypoxia and focal necrosis, easy occurrence of kidney stone and urethral stone, increase of the incidence of iron deficiency anemia and cause dental caries. No control index for molybdenum exists in the current national standard discharge standard of sewage in China, but the Liaoning province is the main production place of molybdenum, so the mass concentration limit value of molybdenum in the direct discharge wastewater of the landmark is 1.5mg/L, and the concentration limit value of molybdenum discharged into a sewage treatment plant is 3 mg/L.
Aiming at the problem of difficult deep removal of molybdenum in molybdenum smelting wastewater, the invention develops a method which has high treatment efficiency and stable and simple process, realizes the deep removal of molybdenum in the molybdenum smelting wastewater and the regeneration of iron salt precipitation slag by the steps of adjusting pH-D318 resin for adsorption pre-removal of Mo, adjusting pH, deep removal of molybdenum by iron salt precipitation, filtration, regeneration and the like, and realizes the cyclic utilization of deep removal of molybdenum and iron salt.
[ summary of the invention ]
The invention aims to overcome the defects of the prior art and provides a method for deeply removing molybdenum from molybdenum smelting wastewater, which can deeply remove Mo in the molybdenum smelting wastewater, ensure that the Mo concentration in the wastewater is less than or equal to 0.003g/L, reduce the influence on the environment and solve the safety problem of Mo pollution to underground water.
The invention discloses a method for deeply removing molybdenum in molybdenum-containing wastewater, which comprises the following steps:
(1) adjusting the pH value: firstly, the pH value of the molybdenum-containing smelting wastewater is adjusted, the process is controlled to be 4-5, and then the next treatment link is carried out.
(2) D318 resin adsorption pre-molybdenum removal: and (2) adsorbing the feed liquid obtained by adjusting the pH value in the step (1) by using D318 resin, wherein the adsorption flow is controlled to be 0.51BV/h-1BV/h, and the concentration of Mo in the adsorbed effluent is controlled to be less than or equal to 0.05 g/L.
(3) Adjusting the pH value: and (3) adjusting the pH value of the obtained effluent through the step (2), and controlling the pH value to be 6-9.
(4) Deep molybdenum removal by ferric salt precipitation: adding iron salt (Fe) into the feed liquid obtained in the step (3)2(SO4)3/FeCl3/Fe(NO3) The adding amount of the iron salt in each liter of feed liquid is 0.1g-0.2g, the reaction time is 30-60min, the stirring speed is 60-120r/min, the reaction temperature is room temperature, and the reaction chemical formula is as follows: 2Fe3++3MoO4 2-＝Fe2(MoO4)3After the reaction, filtering, controlling the concentration of Mo in the filtrate to be less than or equal to 0.003g/L, and carrying out the next reaction step on the iron slag obtained by the reaction.
(5) Regenerating, namely performing alkali decomposition on the iron slag, wherein the liquid-solid ratio is 1:1, the concentration of sodium hydroxide is 80-120 g/L, the leaching temperature is 140-160 ℃, the leaching time is 1-2 h, the leaching is finished, filtering is performed, filtrate is collected and used for recovering Mo, filter residue is washed by water, the pH value of washing effluent is 9.0-10.0, then 0.1mol/L hydrochloric acid solution is used for washing, the pH value of the washing effluent is 6-7, and the washed iron slag is dried and returned for use; the reaction equation of the iron slag and the sodium hydroxide is as follows: fe2(MoO4)3+6NaOH＝3Na2MoO4+2Fe(OH)3The leached residue is washed by hydrochloric acid solution, so that alkali in the leached residue is washed away, and Fe (OH) is simultaneously used3The stable state is changed into the unstable state, and the leached slag is activated, so that the Mo precipitation effect in the next period is facilitated.
Compared with the prior art, the invention has the following advantages:
the deep removal of molybdenum in the molybdenum smelting wastewater is completed by adjusting pH-D318 resin to adsorb and pre-remove molybdenum, adjusting pH, deeply removing molybdenum from ferric salt and regenerating, wherein the concentration of Mo in the removed wastewater is less than or equal to that of Mo
0.003g/L, solves the problems of difficult deep removal of molybdenum in the molybdenum-containing wastewater, influence on underground water and harm to ecological health, and is a method for efficiently and deeply removing Mo in the molybdenum smelting wastewater.
[ description of the drawings ]
Embodiments of the invention will be described in further detail below with reference to the accompanying drawings, in which:
FIG. 1 is a process flow diagram of the present invention;
[ detailed description ] embodiments
The invention is further illustrated by the following example and by the accompanying figure 1.
Example 1
This embodiment molybdenum smelting waste water comes from a certain tungsten smelter, sampling test, testing result: mo is 0.5g/L, and PH is 8-9.
(1) Adjusting the pH value: firstly, 10L of molybdenum smelting wastewater is measured, concentrated sulfuric acid is used for adjusting the pH value of the molybdenum smelting wastewater to 4-5, and the molybdenum smelting wastewater is uniformly mixed and then enters the next treatment link.
(2) D318 resin adsorption pre-molybdenum removal: and (2) adsorbing the feed liquid obtained by adjusting the pH value in the step (1) by using D318 resin, controlling the adsorption flow to be 0.5BV/h, collecting the adsorbed effluent, uniformly mixing, sampling and measuring the Mo concentration to be 0.04g/L, and then entering the next treatment link.
(3) Adjusting the pH value: and (3) adjusting the pH value of the obtained effluent by using a sodium hydroxide solution through the step (2), wherein the pH value is controlled to be 7.0.
(4) Deep molybdenum removal by ferric salt precipitation: adding iron salt (Fe) into the feed liquid obtained in the step (3)2(SO4)3The adding amount of the iron salt is 0.2g/L, the reaction time is 30-60min, the stirring speed is 60r/min, the reaction temperature is room temperature, after the reaction, the Mo concentration in the filtrate is 0.002g/L, and the iron slag obtained by the reaction enters the next reaction step.
(5) And (2) regeneration, namely collecting the iron slag after molybdenum is deeply removed for many times, then carrying out concentrated alkali decomposition, wherein the liquid-solid ratio is 1:1, the concentration of sodium hydroxide is 120g/L, the leaching temperature is 160 ℃, the leaching time is 2h, after the leaching is finished, filtering is carried out, filtrate is collected and used for recovering Mo, filter residue is washed by water, after the pH value of washing effluent is 9.0-10.0, the washing is carried out by using 0.1mol/L hydrochloric acid solution, the pH value of the washing effluent is 6-7, and the washed iron slag is dried and returned for use.
Example 2
This embodiment molybdenum smelting waste water comes from a certain tungsten smelter, sampling test, testing result: mo is 1.5g/L, and PH is 8-9.
(1) Adjusting the pH value: firstly, 10L of molybdenum smelting wastewater is measured, concentrated sulfuric acid is used for adjusting the pH value of the molybdenum smelting wastewater to 4-5, and the molybdenum smelting wastewater is uniformly mixed and then enters the next treatment link.
(2) D318 resin adsorption pre-molybdenum removal: and (2) adsorbing the feed liquid obtained by adjusting the pH value in the step (1) by using D318 resin, controlling the adsorption flow to be 1BV/h, collecting the adsorbed effluent, uniformly mixing, sampling and measuring the Mo concentration to be 0.05g/L, and then entering the next treatment link.
(3) Adjusting the pH value: and (3) adjusting the pH value of the obtained effluent by using a sodium hydroxide solution through the step (2), and controlling the pH value to be 8.0.
(4) Deep molybdenum removal by ferric salt precipitation: adding FeCl salt into the feed liquid obtained in the step (3)3The adding amount of the iron salt is 0.2g/L, the reaction time is 60min, the stirring speed is 60r/min, the reaction temperature is room temperature, after the reaction, the Mo concentration in the filtrate is 0.003g/L, and the iron slag obtained by the reaction enters the next reaction step.
(5) And (2) regeneration, namely collecting the iron slag after molybdenum is deeply removed for many times, then carrying out concentrated alkali decomposition, wherein the liquid-solid ratio is 1:1, the concentration of sodium hydroxide is 80g/L, the leaching temperature is 160 ℃, the leaching time is 2h, after the leaching is finished, filtering is carried out, filtrate is collected and used for recovering Mo, filter residue is washed by water, after the pH value of washing effluent is 9.0-10.0, the washing is carried out by using 0.1mol/L hydrochloric acid solution, the pH value of the washing effluent is 6-7, and the washed iron slag is dried and returned for use.
Example 3
This embodiment molybdenum smelting waste water comes from a certain tungsten smelter, sampling test, the testing result: mo is 0.69g/L, and PH is 8-9.
(1) Adjusting the pH value: firstly, 10L of molybdenum smelting wastewater is measured, concentrated sulfuric acid is used for adjusting the pH value of the molybdenum smelting wastewater to 4-5, and the molybdenum smelting wastewater is uniformly mixed and then enters the next treatment link.
(2) D318 resin adsorption pre-molybdenum removal: and (2) adsorbing the feed liquid obtained by adjusting the pH value in the step (1) by using D318 resin, controlling the adsorption flow to be 0.8BV/h, collecting the adsorbed effluent, uniformly mixing, sampling and measuring the Mo concentration to be 0.04g/L, and then entering the next treatment link.
(3) Adjusting the pH value: and (3) adjusting the pH value of the obtained effluent by using a sodium hydroxide solution through the step (2), wherein the pH value is controlled to be 8.0.
(4) Deep molybdenum removal by ferric salt precipitation: adding iron salt Fe (NO) into the feed liquid obtained in the step (3)3)3The adding amount of the catalyst is 0.2g/L, the reaction time is 60min, the stirring speed is 60r/min, the reaction temperature is room temperature, after the reaction, the Mo concentration in the filtrate is 0.002g/L, and the iron slag obtained by the reaction enters the next reaction step.
(5) And (2) regeneration, namely collecting the iron slag after molybdenum is deeply removed for many times, then carrying out concentrated alkali decomposition, wherein the liquid-solid ratio is 1:1, the concentration of sodium hydroxide is 120g/L, the leaching temperature is 140 ℃, the leaching time is 2h, after the leaching is finished, filtering is carried out, filtrate is collected and used for recovering Mo, filter residue is washed by water, after the pH value of washing effluent is 9.0-10.0, the washing is carried out by using 0.1mol/L hydrochloric acid solution, the pH value of the washing effluent is 6-7, and the washed iron slag is dried and returned for use.
Example 4
This embodiment molybdenum smelting waste water comes from a certain tungsten smelter, sampling test, testing result: mo is 0.89g/L, and PH is 8-9.
(1) Adjusting the pH value: firstly, 10L of molybdenum smelting wastewater is measured, concentrated sulfuric acid is used for adjusting the pH value of the molybdenum smelting wastewater to 4-5, and the molybdenum smelting wastewater is uniformly mixed and then enters the next treatment link.
(2) D318 resin adsorption pre-molybdenum removal: and (2) adsorbing the feed liquid obtained by adjusting the pH value in the step (1) by using D318 resin, controlling the adsorption flow to be 1BV/h, collecting the adsorbed effluent, uniformly mixing, sampling and measuring the Mo concentration to be 0.04g/L, and then entering the next treatment link.
(3) Adjusting the pH value: and (3) adjusting the pH value of the obtained effluent by using a sodium hydroxide solution through the step (2), and controlling the pH value to be 8.0.
(4) Deep molybdenum removal by ferric salt precipitation: adding iron salt Fe (NO) into the feed liquid obtained in the step (3)3)30.1g/L and Fe2(SO4)30.1g/L, 60min of reaction time, 60r/min of stirring speed, room temperature of reaction, 0.0015g/L of Mo concentration in the filtrate after reaction, and the iron slag obtained by the reaction enters the next reaction step.
(5) And (2) regeneration, namely collecting the iron slag after molybdenum is deeply removed for many times, then carrying out concentrated alkali decomposition, wherein the liquid-solid ratio is 1:1, the concentration of sodium hydroxide is 80g/L, the leaching temperature is 160 ℃, the leaching time is 2h, after the leaching is finished, filtering is carried out, filtrate is collected and used for recovering Mo, filter residue is washed by water, after the pH value of washing effluent is 9.0-10.0, the washing is carried out by using 0.1mol/L hydrochloric acid solution, the pH value of the washing effluent is 6-7, and the washed iron slag is dried and returned for use.
The above description is only a preferred embodiment of the present invention, and it should be noted that a person skilled in the art can make various changes, modifications, substitutions and alterations to the embodiments without departing from the technical principles of the present invention, and such changes, modifications, substitutions and alterations should also be regarded as the protection scope of the present invention.
Claims (1)
1. A method for deeply removing molybdenum in molybdenum-containing wastewater is characterized by comprising the following steps: comprises the following steps:
(1) adjusting the pH value: firstly, adjusting the pH value of the molybdenum-containing smelting wastewater, controlling the process to be 4-5, and then entering the next treatment link;
(2) d318 resin adsorption pre-molybdenum removal: the feed liquid obtained by adjusting the pH value in the step (1) is adsorbed by D318 resin, the adsorption flow is controlled to be 0.51BV/h-1BV/h, the effluent liquid is adsorbed, and the concentration of Mo in the effluent feed liquid is controlled to be less than or equal to 0.05 g/L;
(3) adjusting the pH value: adjusting the pH value of the obtained effluent through the step (2), and controlling the pH value to be 6-9;
(4) deep molybdenum removal by ferric salt precipitation: adding iron salt (Fe) into the feed liquid obtained in the step (3)2(SO4)3/FeCl3/Fe(NO3)3The adding amount of the iron salt in each liter of feed liquid is 0.1g-0.2g, the reaction time is 30-60min, the stirring speed is 60-120r/min, the reaction temperature is room temperature, and the reaction chemical formula is as follows: 2Fe3++3MoO4 2-＝Fe2(MoO4)3After the reaction, filtering, controlling the concentration of Mo in the filtrate to be less than or equal to 0.003g/L, and carrying out the next reaction step on the iron slag obtained by the reaction;
(5) and (2) regenerating, carrying out alkali decomposition on the iron slag, wherein the liquid-solid ratio is 1:1, the concentration of sodium hydroxide is 80-120 g/L, the leaching temperature is 140-160 ℃, the leaching time is 1-2 h, the leaching is completed, filtering is carried out, filtrate is collected and used for recovering Mo, filter residue is washed by water, the pH value of washing effluent is 9.0-10.0, then the washing effluent is washed by 0.1mol/L hydrochloric acid solution, the pH value of the washing effluent is 6-7, and the washed iron slag is dried and returned for use.
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