CN106669658B - Wastewater treatment catalyst and preparation method thereof, wastewater treatment method - Google Patents
Wastewater treatment catalyst and preparation method thereof, wastewater treatment method Download PDFInfo
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/40—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals of the platinum group metals
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- B01J23/16—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
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- B01J23/30—Tungsten
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- B01J23/34—Manganese
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/72—Copper
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
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- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/74—Iron group metals
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- B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/85—Chromium, molybdenum or tungsten
- B01J23/888—Tungsten
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- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
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- B01J23/89—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with noble metals
- B01J23/8906—Iron and noble metals
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- 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
- C02F1/34—Treatment of water, waste water, or sewage with mechanical oscillations
- C02F1/36—Treatment of water, waste water, or sewage with mechanical oscillations ultrasonic vibrations
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- C—CHEMISTRY; METALLURGY
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- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/62—Heavy metal compounds
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- 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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- 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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Abstract
The invention discloses a kind of wastewater treatment catalysts and preparation method thereof, and using the wastewater treatment method of the wastewater treatment catalyst.Wastewater treatment catalyst includes the active layer of carrier and deposition on the carrier；The partial size of the carrier is 0.5mm~0.85mm, and the material of the reactive metal layer is selected from least one of palladium, cobalt, nickel, manganese, tungsten and copper, and the mass percent that the reactive metal layer accounts for the wastewater treatment catalyst is 0.5%~3%.This wastewater treatment catalyst can efficient catalytic reaction, it can be used for chemical nickle-plating wastewater processing, it is measured through test, the nickel ion of complex state can be made de- steady, the nickel of free state is formed, the Auto-decomposition of waste water complex compound is accelerated, free state nickel is reacted with reducing agents such as hypophosphites remaining in chemical nickle-plating wastewater, it is fierce to self-catalyzed reaction to occur in chemical nickle-plating wastewater, forms complicated insoluble chelating precipitation object with catalyst and phosphorus, alkali etc..
Description
Technical field
The present invention relates to field of waste water treatment, more particularly to a kind of wastewater treatment catalyst and preparation method thereof, and
Using the wastewater treatment method of the wastewater treatment catalyst.
Background technique
The conventional method of processing chemical nickle-plating wastewater has: chemical precipitation method, electrolysis method, ion-exchange, reverse osmosis and super
Filter etc., but the nickel metal that cannot be all effectively removed in waste water, while the nickel concentration of water outlet can not be reduced to greatest extent,
Less it is able to satisfy the requirement of qualified discharge.
Chemical nickle-plating wastewater is other than containing a large amount of nickel (1~7g/L), in order to guarantee bath stability, service life and plating
Layer quality, is often added the organic matters such as a large amount of complexing agent, stabilizer, buffer and brightener (10~30g/L)；These are organic
Object, especially complexing agent (citric acid, tartaric acid, malic acid, succinic acid, acetic acid etc.) have very strong complexing power to nickel, therewith
Stable comple is formed, there is a large amount of orthophosphite and a large amount of complexing agent in chemical nickle-plating wastewater, in turn result in chemistry
The difficulty of nickel-plating waste water processing.
Summary of the invention
Based on this, it is necessary to provide the wastewater treatment catalyst that can be used for chemical nickle-plating wastewater processing and its preparation side
Method, and the wastewater treatment method using the wastewater treatment catalyst.
A kind of wastewater treatment catalyst, the active layer including carrier and deposition on the carrier；
The partial size of the carrier is 0.5mm~0.85mm, and the material of the reactive metal layer is selected from palladium, cobalt, nickel, manganese, tungsten
At least one of with copper, the mass percent that the reactive metal layer accounts for the wastewater treatment catalyst is 0.5%~3%.
In one embodiment, the material of the carrier is selected from titanium dioxide, silica, di-iron trioxide or three oxidations
Two aluminium.
A kind of preparation method of above-mentioned wastewater treatment catalyst, includes the following steps:
Partial size is provided and is the carrier of 0.5mm~0.85mm, and the carrier is pre-processed；
Metal salt solution is configured, the pH of the metal salt solution is 2~6, contains palladium ion, cobalt in the metal salt solution
At least one of ion, nickel ion, manganese ion, tungsten ion and copper ion；
By the carrier impregnation in the metal salt solution, filters after the reaction was completed and retain filter residue；And
It will be roasted after the filter residue and drying, the wastewater treatment catalyst obtained after the completion of roasting.
In one embodiment, described that pretreated operation is carried out to the carrier are as follows: pickling or surfactant processing；
It is described by the operation roasted after the filter residue and drying, the temperature of the roasting is 300 DEG C~700 DEG C, institute
The time for stating roasting is 4h~8h.
A kind of wastewater treatment method, includes the following steps:
Adjust waste water to be processed pH be 9~13, then under conditions of 10 DEG C~40 DEG C ultrasonic disperse 15min~
60min；
Wastewater treatment catalyst is added into the waste water to be processed after ultrasonic disperse, is sufficiently reacted after reaction
Liquid, wherein the wastewater treatment catalyst is wastewater treatment catalyst according to any one of claims 1 to 2；And
By the reaction solution stratification, precipitated and supernatant.
In one embodiment, the waste water to be processed is chemical nickle-plating wastewater.
In one embodiment, the operation of the ultrasonic disperse is completed using the supersonic wave cleaning machine of 240W.
In one embodiment, wastewater treatment catalyst is added in the waste water to be processed to after ultrasonic disperse
Operation in, the additional amount of the wastewater treatment catalyst is 2g/L~14g/L.
In one embodiment, wastewater treatment catalyst is added in the waste water to be processed to after ultrasonic disperse
Operation in, the additional amount of the wastewater treatment catalyst is 5g/1.5L.
In one embodiment, obtained in the operation of reaction solution after the abundant reaction, the reaction time be 15min~
60min。
This wastewater treatment catalyst can efficient catalytic reaction, can be used for chemical nickle-plating wastewater processing, through test survey
It is fixed, the nickel ion of complex state can be made de- steady, the nickel of free state is formed, accelerate the Auto-decomposition of waste water complex compound, free state nickel
Reacted with reducing agents such as hypophosphites remaining in chemical nickle-plating wastewater, occur in chemical nickle-plating wastewater it is fierce to
Self-catalyzed reaction forms complicated insoluble chelating precipitation object with catalyst and phosphorus, alkali etc..
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, right combined with specific embodiments below
A specific embodiment of the invention is described in detail.Many details are explained in the following description in order to sufficiently manage
The solution present invention.But the invention can be embodied in many other ways as described herein, those skilled in the art can
To do similar improvement without violating the connotation of the present invention, therefore the present invention is not by the limit of following public specific implementation
System.
The invention discloses the wastewater treatment catalysts of an embodiment, including carrier and the activity being deposited on carrier
Layer.
The partial size of carrier is 0.5mm~0.85mm, and the material of reactive metal layer is selected from palladium, cobalt, nickel, manganese, tungsten or copper, activity
The mass percent for accounting for wastewater treatment catalyst of metal layer is 0.5%~3% (preferably 0.5%).
Preferably, the material of carrier is selected from titanium dioxide, silica, di-iron trioxide or aluminum oxide.
This wastewater treatment catalyst can efficient catalytic reaction, can be used for chemical nickle-plating wastewater processing so that complexing
The nickel ion of state is de- steady, forms the nickel of free state, accelerates the Auto-decomposition of waste water complex compound, free state nickel and chemical nickle-plating wastewater
The reducing agents such as the hypophosphite of middle remaining are reacted, and it is fierce to self-catalyzed reaction to occur in chemical nickle-plating wastewater, with
Catalyst and phosphorus, alkali etc. form complicated insoluble chelating precipitation object.
The invention also discloses the preparation methods of above-mentioned wastewater treatment catalyst, include the following steps:
S110, partial size is provided as the carrier of 0.5mm~0.85mm, and carrier is pre-processed.
Preferably, the material of carrier is selected from titanium dioxide, silica, di-iron trioxide or aluminum oxide.
The ball type carrier precursor that can be directly 2mm~4mm in the partial size of purchase commercialization, is obtained by filtration partial size after grinding
For the carrier of 0.5mm~0.85mm, obtained carrier is dried after deionized water repeatedly rinses can be spare.
Carrying out pretreated operation to the carrier is that pickling or surfactant are handled.Pickling can be with are as follows: by carrier with
The nitric acid solution that mass concentration is 5%~25% mixes, reflow treatment 1h~3h at 90 DEG C~100 DEG C.
S120, configuration metal salt solution.
The pH of metal salt solution is 2~6 (preferably 4), contains palladium ion, cobalt ions, nickel ion, manganese in metal salt solution
At least one of ion, tungsten ion and copper ion.
The pH of metal salt solution can be adjusted by hydrochloric acid, sulfuric acid or nitric acid.
Preferably, the concentration of metal salt is 0.1g/L~10g/L in metal salt solution.
S130, by carrier impregnation that S110 is obtained in the metal salt solution containing nitric acid that S120 is obtained, reaction is completed
After filter and retain filter residue.
Preferably, the time of carrier impregnation is 3h~9h (preferably 6h), and the temperature of carrier impregnation is 10 DEG C~30 DEG C (excellent
It is selected as 20 DEG C).
S140, it will be roasted after filter residue and drying that S130 is obtained, wastewater treatment catalyst obtained after the completion of roasting.
By in the operation roasted after filter residue and drying, the temperature of roasting is 300 DEG C~700 DEG C (preferably 600 DEG C), roasting
The time of burning is 4h~8h (preferably 6h).
Wastewater treatment catalyst made from the preparation method of this wastewater treatment catalyst can efficient catalytic reaction, can be with
For chemical nickle-plating wastewater processing, so that the nickel ion of complex state is de- steady, form the nickel of free state, accelerate waste water complex compound from
Hair decomposes, and free state nickel is reacted with reducing agents such as hypophosphites remaining in chemical nickle-plating wastewater, chemical nickle-plating wastewater
It is middle to occur fierce to self-catalyzed reaction, complicated insoluble chelating precipitation object is formed with catalyst and phosphorus, alkali etc..
The invention also discloses the wastewater treatment methods using above-mentioned wastewater treatment catalyst of an embodiment, including
Following steps:
S210, the pH for adjusting waste water to be processed are 9~13, then ultrasonic disperse under conditions of 10 DEG C~40 DEG C
15min~60min.
The operation that the pH for adjusting waste water to be processed is 9~13 can be by adding sodium hydroxide, potassium hydroxide, hydroxide
The substances such as calcium, calcium oxide are completed.
Preferably, waste water to be processed is chemical nickle-plating wastewater.Nickel in chemical nickle-plating wastewater containing 1g/L~7g/L with
And the organic matter of 10g/L~30g/L (organic matter includes complexing agent, stabilizer, buffer and brightener etc.).
The operation of ultrasonic disperse is completed using the supersonic wave cleaning machine of 240W.
S220, wastewater treatment catalyst is added into the waste water to be processed after the ultrasonic disperse that S210 is obtained, it is sufficiently anti-
Should after obtain reaction solution.
Wastewater treatment catalyst is as described above.
It is added into the waste water to be processed after ultrasonic disperse in the operation of wastewater treatment catalyst, wastewater treatment catalyst
Additional amount be 2g/L~14g/L.
Preferably, it is added into the waste water to be processed after ultrasonic disperse in the operation of wastewater treatment catalyst, at waste water
The additional amount for managing catalyst is 5g/1.5L.
It is sufficiently obtained in the operation of reaction solution after reaction, the reaction time is 15min~60min.
S230, the reaction solution stratification for obtaining S220, are precipitated and supernatant.
What is obtained is precipitated as complicated insoluble chelating precipitation object, and so as to landfill disposal, nickel is most preferably gone in supernatant
Except rate can reach 99.5%.
The following are specific embodiments.
Drug is used in specific embodiment and instrument is this field conventional selection.The chemical-electrical used in embodiment 2~6
Waste electroplating comes from certain electroplate factory, includes: nickel concentration 1.7g/L, CODcr=56000mg/L, TP=in electroless plating waste water
29500mg/L, pH 3.5.
Embodiment 1
Buy the SiO that partial size is 2~4mm2, ground and be sieved by laboratory room small-sized grinder, the partial size of system is
The carrier of 0.5mm~0.85mm.Obtained carrier is further purified into impurity elimination, deionized water is added and carries out repeated multiple times rinsing,
Final water is limpid without miscellaneous, and the carrier after cleaning is placed in in 110 degree of baking oven to dry 12h spare.
Carrier after drying is placed in the nitric acid solution of 10wt%, reflow treatment 1h at 90 DEG C, after filtering to filter residue into
Row washing and drying, obtain pretreated carrier.
Configuration concentration is the palladium chloride solution that 1g/L, pH are 4.The pH of palladium chloride solution is adjusted using hydrochloric acid.
Pretreated carrier is that the palladium chloride solution that 1g/L, pH are 4 mixes with concentration, the static quiet stain 6h at 20 DEG C,
Then filter residue is filtered and retains, will be dry at 100 DEG C of filter residue, obtain presoma.
Presoma is placed in Muffle kiln roasting, maturing temperature is 600 DEG C, calcining time 4h, is obtained after the completion of roasting
Wastewater treatment catalyst.
Embodiment 2
It takes out 1.5L electroless plating waste water to be placed in supersonic wave cleaning machine, adds 30% (mass fraction) sodium hydroxide solution
The pH for adjusting electroless plating waste water is 13, and temperature is 28 DEG C, ultrasound 20 minutes.
Wastewater treatment catalyst made from 5g embodiment 1 is added, reacts 30min, stratification, filtering, finally in measurement
Nickel concentration in clear liquid is 7.6mg/L, and nickel ion removal rate is 99.5%.
Embodiment 3
It takes out 1.5L electroless plating waste water to be placed in supersonic wave cleaning machine, adds 30% (mass fraction) sodium hydroxide solution
The pH for adjusting electroless plating waste water is 13, and temperature is 28 DEG C, ultrasound 20 minutes.
Wastewater treatment catalyst made from 3g embodiment 1 is added, reacts 30min, stratification, filtering, finally in measurement
Nickel concentration in clear liquid is 561mg/L, and nickel ion removal rate is 67%.
Embodiment 4
It takes out 1.5L electroless plating waste water to be placed in supersonic wave cleaning machine, adds 30% (mass fraction) sodium hydroxide solution
The pH for adjusting electroless plating waste water is 10, and temperature is 28 DEG C, ultrasound 20 minutes.
Wastewater treatment catalyst made from 5g embodiment 1 is added, reacts 30min, stratification, filtering, finally in measurement
Nickel concentration in clear liquid is 221mg/L, and nickel ion removal rate is 87%.
Embodiment 5
It takes out 1.5L electroless plating waste water to be placed in supersonic wave cleaning machine, adds 30% (mass fraction) sodium hydroxide solution
The pH for adjusting electroless plating waste water is 13, and temperature is 28 DEG C, ultrasound 20 minutes.
Wastewater treatment catalyst made from 5g embodiment 1 is added, reacts 30min, stratification, filtering, finally in measurement
Nickel concentration in clear liquid is 110mg/L, and nickel ion removal rate is 96%.
Embodiment 6
It takes out 1.5L electroless plating waste water to be placed in supersonic wave cleaning machine, adds 30% (mass fraction) sodium hydroxide solution
The pH for adjusting electroless plating waste water is 13, and temperature is 28 DEG C, ultrasound 20 minutes.
Wastewater treatment catalyst made from 1g embodiment 1 is added, reacts 30min, stratification, filtering, finally in measurement
Nickel concentration in clear liquid is 1037mg/L, and nickel ion removal rate is 39%.
Embodiment 7
Analog configuration water is taken, nickel concentration is 50mg/L, pH 6 in analog configuration water.
It takes 1.5L analog configuration water to be placed in supersonic wave cleaning machine, adds the adjusting of 30% (mass fraction) sodium hydroxide solution
The pH of electroless plating waste water is 13, and temperature is 28 DEG C, ultrasound 20 minutes.
0.5g catalyst is added, reacts 30 minutes, stratification, filtering finally measures supernatant nickel concentration 0.45mg/L,
Nickel ion removal rate is 99.1%.
Each technical characteristic of embodiment described above can be combined arbitrarily, for simplicity of description, not to above-mentioned reality
It applies all possible combination of each technical characteristic in example to be all described, as long as however, the combination of these technical characteristics is not deposited
In contradiction, all should be considered as described in this specification.
The embodiments described above only express several embodiments of the present invention, and the description thereof is more specific and detailed, but simultaneously
It cannot therefore be construed as limiting the scope of the patent.It should be pointed out that coming for those of ordinary skill in the art
It says, without departing from the inventive concept of the premise, various modifications and improvements can be made, these belong to protection of the invention
Range.Therefore, the scope of protection of the patent of the invention shall be subject to the appended claims.
Claims (7)
1. a kind of wastewater treatment catalyst, which is characterized in that including the active layer of carrier and deposition on the carrier；
The partial size of the carrier is 0.5mm ~ 0.85mm, and the material of the carrier is selected from titanium dioxide, silica, three oxidations two
The material of iron or aluminum oxide, the reactive metal layer is palladium, and the reactive metal layer accounts for the wastewater treatment catalyst
Mass percent is 0.5% ~ 3%, and the wastewater treatment catalyst can be used in chemical nickle-plating wastewater processing.
2. a kind of preparation method of wastewater treatment catalyst described in claim 1, which comprises the steps of:
Partial size is provided and is the carrier of 0.5mm ~ 0.85mm, and the carrier is pre-processed；
Metal salt solution is configured, the pH of the metal salt solution is 2 ~ 6, contains palladium ion in the metal salt solution；
By the carrier impregnation in the metal salt solution, filters after the reaction was completed and retain filter residue；And
It will be roasted after the filter residue and drying, the wastewater treatment catalyst obtained after the completion of roasting.
3. the preparation method of wastewater treatment catalyst according to claim 2, which is characterized in that it is described to the carrier into
The pretreated operation of row are as follows: pickling or surfactant processing；
It is described by the operation roasted after the filter residue and drying, the temperature of the roasting is 300 DEG C ~ 700 DEG C, the roasting
Time be 4h ~ 8h.
4. a kind of wastewater treatment method, which comprises the steps of:
The pH for adjusting waste water to be processed is 9 ~ 13, then ultrasonic disperse 15min ~ 60min under conditions of 10 DEG C ~ 40 DEG C；
Wastewater treatment catalyst is added into the waste water to be processed after ultrasonic disperse, sufficiently obtains reaction solution after reaction,
Wherein, the wastewater treatment catalyst is wastewater treatment catalyst described in claim 1, the wastewater treatment catalyst
Additional amount is 5g/1.5L；And
By the reaction solution stratification, precipitated and supernatant.
5. wastewater treatment method according to claim 4, which is characterized in that the waste water to be processed is useless for chemical nickel plating
Water.
6. wastewater treatment method according to claim 4, which is characterized in that the operation of the ultrasonic disperse is using 240W's
Supersonic wave cleaning machine is completed.
7. wastewater treatment method according to claim 4, which is characterized in that obtain the behaviour of reaction solution after the abundant reaction
In work, the reaction time is 15min ~ 60min.
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| CN110759521B (en) * | 2019-10-16 | 2020-09-25 | 中南大学 | Method for treating low-concentration copper-containing wastewater |
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