CN109336244A - A method of processing carbon supported noble metal catalyst industrial wastewater - Google Patents
A method of processing carbon supported noble metal catalyst industrial wastewater Download PDFInfo
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- CN109336244A CN109336244A CN201811399216.4A CN201811399216A CN109336244A CN 109336244 A CN109336244 A CN 109336244A CN 201811399216 A CN201811399216 A CN 201811399216A CN 109336244 A CN109336244 A CN 109336244A
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- noble metal
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/76—Treatment of water, waste water, or sewage by oxidation with halogens or compounds of halogens
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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
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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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
- C02F2101/16—Nitrogen compounds, e.g. ammonia
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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
- C02F2101/30—Organic 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
- C02F2303/00—Specific treatment goals
- C02F2303/04—Disinfection
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- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
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- Treatment Of Water By Oxidation Or Reduction (AREA)
Abstract
The invention discloses a kind of methods for handling carbon supported noble metal catalyst industrial wastewater, belong to field of waste water treatment.By using the oxidizer treatments waste water such as sodium hypochlorite, sodium chlorate, hypochlorous acid, chloric acid, chlorine, make its organic matter degradation, COD is greatly lowered；Then it is neutralized using the acid waste water that Vehicle element is formed, adjusts pH value of waste water, reach in National Standard of the People's Republic of China GB21904-2008 " newly-built enterprise's Sewage Water Emissions concentration limit ".Due to sodium hypochlorite (sodium chlorate) to the oxidation of inorganic matter in waste water, the oxidation of organic matter and with the synergistic effect of dead catalyst, COD, the ammonia nitrogen, coloration in waste water can be reduced, and then reduce the indexs such as total organic carbon, total nitrogen, the qualified discharge for finally realizing waste water, realizes the technological gap of current carbon supported noble metal catalyst Industrial Wastewater Treatment.The main advantages of the present invention for process is short, process is simple, at low cost.
Description
Technical field
The present invention relates to a kind of methods for handling carbon supported noble metal catalyst industrial wastewater, are catalyzed especially suitable for palladium on carbon
The processing of industrial wastewater in agent preparation process.
Background technique
Carbon supported noble metal catalyst is a kind of excellent catalyst, and selectivity is good, and anti-poisoning capability is strong, and easily recycling, main
To be applied to add hydrogen, dehydrogenation, oxidation and electrochemical reaction etc., the feature with greenization chemical reaction.According to incomplete system
Meter, mainly there is palladium carbon, platinum carbon, ruthenium carbon, the catalysis of rhodium carbon by 10, more than 000 ton/year of China's carbon supported noble metal catalyst market demand
Agent etc., wherein the most widely used for palladium-carbon catalysts.
The main method for preparing carbon supported noble metal catalyst at present has: (1) precious metal salt solution infusion process: being placed in activity
Absorption is impregnated in carbon pastes, is prepared into palladium crystal grain under the effect of the reducing agents such as hydrogen, formaldehyde, hydrazine hydrate, formic acid, glucose, point
It is dispersed on carrier active carbon.(2) precious metal ion dipping-precipitation method: is converted first into insoluble noble metal at room temperature
Alkali or oxide, load on activated carbon again later, generate noble metal crystal grain under the effect of above-mentioned reducing agent, can prevent in this way
The migration of crystal grain and crystal grain are grown up.(3) sol method: the precious metal salt solution containing surfactant is prepared under reducing agent effect and is received
Rice colloidal sol, it is then immobilized into absorbent charcoal carrier again, it washes by drainage up to noble metal catalyst.
As described above, generally can be divided into pretreatment, dipping, reduction etc. three in carbon supported noble metal catalyst preparation process
The tandem of independent process, different method processes is inconsistent.It is main in preprocessing process by taking palladium-carbon catalyst as an example
Hydrochloric acid, nitric acid, alkali is added to handle active carbon；In dipping adsorption process, hydrochloric acid, nitric acid or acetic acid is added and adjusts and inhales
Attached liquid acidity；In reduction process, need to be added pH buffer solution or alkali, to promote the nucleus of noble metal to generate.These acid with
Alkali also generates some salt other than the generation reaction for completing palladium crystal grain.The latter and remaining alkali are closely adsorbed on active carbon
In the hole of carrier, and since active carbon specific surface area is huge, 1000m is commonly reached2/ g has stronger absorption property, because
It is also an important factor for influencing catalyst performance that how this, which removes the salt of absorption on the carbon carrier,.
In palladium-carbon catalyst industrial production, common washing methods is exactly to make it with a large amount of pure water catalyst
It is washed till neutrality.Due to the strong absorption property of active carbon, generally requires hundreds times of catalyst quality of water and cleaned, it can be by it
It is washed till neutrality.These are washed the waste water to get off and mainly contain NaCl, Na2CO3, NaOH, organic matter, suspended matter etc., belong to Low-salinity alkali
Property organic wastewater.These waste water must be accorded to ability qualified discharge after processing, at present about palladium-carbon catalyst Industrial Wastewater Treatment
It is rarely reported, it would be highly desirable to develop.Then traditional noble metal Fine Chemical wastewater treatment adjusts pH frequently with activated carbon adsorption
It is discharged after value.Although this method can handle low organic wastewater, but the amount of reagent consumed is big, and adsorption time is long, and active carbon
Modification is generally required, it is cumbersome.This programme is based under this background, proposes a kind of carbon supported noble metal catalyst industry
The processing method of waste water.
Summary of the invention
The present invention is difficult to handle for the Low-salinity alkalinity organic wastewater generated in current carbon supported noble metal catalyst industry
The problem of, a kind of method for proposing wastewater treatment reaches discharge standard or even part reuse.It is handled using this method useless
Water has the advantages that process is short, at low cost.
In order to solve the above-mentioned technical problem, The technical solution adopted by the invention is as follows: using sodium hypochlorite, chloric acid first
The oxidizer treatments waste water such as sodium, hypochlorous acid, chloric acid, chlorine, makes its organic matter degradation, and COD is greatly lowered；Then carrier is used
It pre-processes the acid waste water formed or other acid solutions neutralizes, adjust pH value of waste water, reach country of People's Republic of China (PRC) mark
In quasi- GB21904-2008 " newly-built enterprise's Sewage Water Emissions concentration limit ".
It is as follows that the present invention provides a kind of method for handling carbon supported noble metal catalyst industrial wastewater.
Using carbon supported noble metal industrial wastewater as raw material, oxidant, stirring, in certain temperature is added according to certain mass ratio
After lower oxidation a period of time, acid solution is added according to acidity, stirring is neutralized to pH in a certain range.
Wherein, the oxidant be one or more of sodium hypochlorite, sodium chlorate, hypochlorous acid, perchloric acid, chlorine,
Additional amount is the 0.05-1%, preferably 0.2-0.6% of industrial wastewater quality.
Wherein, the oxidization time is 0.5-5h, preferably 1-3h.
Wherein, the oxidizing temperature is 10-60 DEG C, preferably 20-40 DEG C.
Wherein, the acid solution is the spent acid after Vehicle element or the hydrochloric acid separately prepared, nitric acid solution, is rubbed
Your concentration is 0.05-6 M, preferably 0.5-2M.
Wherein, the spent acid after the Vehicle element, main component are nitric acid, hydrochloric acid.
Wherein, the pH, range is between 7-7.5.
Catalyst treatment waste water of the invention, its advantages have the following aspects.
1) to the oxidation of inorganic matter.
Ammoniacal nitrogen in waste water can add excessive sodium hypochlorite with oxidation removal.It is added in the aqueous solution containing ammonia nitrogen secondary
After sodium chlorate.Hypochlorous acid, hypochlorite ion can be reacted with the ammonia in water generates monochloro amine (NH2Cl), dichlormaine (NHCl2)
With three chloramines (NCl3).Due to NCl3Just can be stabilized in pH < 5.5 and solubility is very low in water, only 10-7
Mol/L, so in natural aqueous solution, NCl3It there's almost no.
2) to the oxidation of organic matter.
When chloranion is reduced, easily obtains electronics and there is very strong oxidisability, in the solution hypochlorite from
The neutral molecule state of very little is presented in conjunction with hydrogen ion in son, is electrically easily diffused into bacterium surface since it is not externally aobvious,
Then it is penetrated into inside bacterium by cell wall, destroys its enzyme system, lead to the death of cell.
Sodium hypochlorite also acts as disinfectant, is widely used in disinfection and sterilization.Sodium hypochlorite is to seven kinds of cause of diseases such as excrement coccus
The Disinfection Effect of microorganism is more preferable, and so that the amount of pathogenic microorganism is dropped to the hydrogen peroxide pharmaceutical quantities that original 10% is added is time chlorine
3.8 times of sour sodium.
3) with the coordinating effect of catalyst.
Loaded noble metal catalyst obtains widely because having the characteristics that catalytic performance is strong, stability is good, the service life is long
Feature is widely used for handling toxic, harmful, high concentrated organic wastewater in Wet Catalytic Oxidation Method.Carbon supported noble metal Industry Waste
Water inherently contains some catalyst suspended matters, and main component is subtle active carbon particle and noble metal active component；Active carbon
With stronger suction-operated, the pollutant local concentration of adsorption is higher, it is easy to by the oxidants oxygen such as sodium hypochlorite
Change, the surface of active carbon provides many activated centres, is easy to carry out redox reaction at these activated centres.
In conclusion since strong oxidizers such as sodium hypochlorite, sodium chlorate itself have strong oxidizing property, with carbon supported noble metal work
Catalyst generates coordinating effect in industry waste water, and better effect is prominent, and inorganic matter, organic matter, decoloration in oxidized waste water reduce
COD, ammonia nitrogen in waste water, coloration, and then the indexs such as total organic carbon, total nitrogen are reduced, finally realize the qualified discharge of waste water.
Below by specific embodiment, the invention will be further described.It is total according to the Chinese people in following scheme
It is detected with method specified in state standard GB/T 21904-2008 " chemical synthesis class pharmaceuticals industry pollution discharge standard "
The water quality of waste water.Water pH value is measured according to GB/T 6920-1986；It is aerobic that GB/T7488-1987 measures water quality biochemistry on the five
Amount；The ammonia nitrogen of HJ/T195-2005 measurement waste water；The total nitrogen of HJ/T199-2005 measurement waste water；GB/T11893-1989 measurement is useless
Water total phosphorus；The suspended matter of GB/T11901-1989 measurement waste water；The coloration of GB/T11903-1989 measurement waste water；GB/T11914-
The COD of 1989 measurement waste water；The total organic carbon of GB/T13193-1991 measurement waste water.
Specific embodiment
Embodiment 1.
By 5% palladium-carbon catalyst industrial wastewater of 100kg, 50g sodium hypochlorite is added, 1L is added after stirring 1h in a kettle
Absorbent charcoal carrier preprocessing solution (nitric acid containing 2M) stirs and measures its pH value, suspended matter, coloration, COD, BOD5, total after 10min
Nitrogen, total phosphorus, ammonia nitrogen, total organic carbon, acquired results are as shown in table 1.
Embodiment 2.
By 5% platinum carbon Catalyst waste water of 100kg, 1kg sodium chlorate is added, is added 0.5 after stirring 5h in a kettle
L absorbent charcoal carrier preprocessing solution (nitric acid containing 6M) stirs and measures its pH value, suspended matter, coloration, COD, BOD5, total after 10min
Nitrogen, total phosphorus, ammonia nitrogen, total organic carbon, acquired results are as shown in table 1.
Embodiment 3.
By 3% ruthenium C catalyst industrial wastewater of 100kg, 0.5kg hypochlorous acid is added, is added after stirring 3h in a kettle
0.8 L absorbent charcoal carrier preprocessing solution (nitric acid containing 4M), stir 10min after measure its pH value, suspended matter, coloration, COD,
BOD5, total nitrogen, total phosphorus, ammonia nitrogen, total organic carbon, acquired results are as shown in table 1.
Embodiment 4.
By 1% gold medal C catalyst industrial wastewater of 100kg, 0.2kg hypochlorous acid is added, is added 1 after stirring 2h in a kettle
L absorbent charcoal carrier preprocessing solution (hydrochloric acid containing 3M) stirs and measures its pH value, suspended matter, coloration, COD, BOD5, total after 10min
Nitrogen, total phosphorus, ammonia nitrogen, total organic carbon, acquired results are as shown in table 1.
Embodiment 5.
By 10% palladium-carbon catalyst industrial wastewater of 100kg, 0.8kg chlorine (pressure is 10 MPa) is added, in a kettle
1 L absorbent charcoal carrier preprocessing solution (hydrochloric acid containing 3M) is added after stirring 5h, measures its pH value, suspended matter, color after stirring 10min
Degree, COD, BOD5, total nitrogen, total phosphorus, ammonia nitrogen, total organic carbon, acquired results are as shown in table 1.
Comparative example 1.
By 10% palladium-carbon catalyst industrial wastewater of 100kg, 5kg active carbon is added, is added 1 after stirring 5h in a kettle
L absorbent charcoal carrier preprocessing solution (hydrochloric acid containing 3M) stirs and measures its pH value, suspended matter, coloration, COD, BOD5, total after 10min
Nitrogen, total phosphorus, ammonia nitrogen, total organic carbon, acquired results are as shown in table 1.
As can be seen from Table 1, after this programme is handled, all waste water quality indexs meet GB21904-2008 and " change
In synthesis class pharmaceuticals industry pollution discharge standard " table 2 " newly-built enterprise's Sewage Water Emissions concentration limit ", that is, reach
To wastewater discharge standard.And waste water described in comparative example 1 is after processing, discharge standard has not been reached yet in COD and total organic carbon,
Compared with comparative example 1, this programme process is short, process is simple, at low cost, has effectively handled palladium on carbon noble metal industrial wastewater,
Breach the technological gap of current carbon supported noble metal catalyst Industrial Wastewater Treatment.
Claims (7)
1. a kind of method for handling carbon supported noble metal catalyst industrial wastewater, it is characterised in that:
Using carbon supported noble metal industrial wastewater as raw material, oxidant is added according to certain mass ratio, stirs, at a certain temperature oxygen
After changing a period of time, acid solution is added according to acidity, stirring is neutralized to pH in a certain range.
2. the method for processing carbon supported noble metal catalyst industrial wastewater according to claim 1, wherein the oxidant is
One or more of sodium hypochlorite, sodium chlorate, hypochlorous acid, perchloric acid, chlorine, additional amount are the 0.05- of industrial wastewater quality
1%, preferably 0.2-0.6%.
3. the method for processing carbon supported noble metal catalyst industrial wastewater according to claim 1, wherein the oxidization time
For 0.5-5h, preferably 1-3h.
4. the method for processing carbon supported noble metal catalyst industrial wastewater according to claim 1, wherein the oxidizing temperature
It is 10-60 DEG C, preferably 20-40 DEG C.
5. the method for processing carbon supported noble metal catalyst industrial wastewater according to claim 1, wherein the acid solution
The hydrochloric acid for the spent acid after Vehicle element or separately prepared, nitric acid solution, molar concentration is 0.05-6 M, preferably 0.5-
2M。
6. the spent acid after Vehicle element according to claim 5, main component is nitric acid, hydrochloric acid.
7. the method for processing carbon supported noble metal catalyst industrial wastewater according to claim 1, wherein the pH, model
It is trapped among between 7-7.5.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118430678A (en) * | 2024-07-01 | 2024-08-02 | 山东知林新材料有限公司 | Intelligent wastewater treatment management platform based on precious metal refining |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN118430678A (en) * | 2024-07-01 | 2024-08-02 | 山东知林新材料有限公司 | Intelligent wastewater treatment management platform based on precious metal refining |
| CN118430678B (en) * | 2024-07-01 | 2024-08-27 | 山东知林新材料有限公司 | Intelligent wastewater treatment management platform based on precious metal refining |
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Application publication date: 20190215 |