CN104761095B - A kind of method of phenol wastewater Color removal - Google Patents
A kind of method of phenol wastewater Color removal Download PDFInfo
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- CN104761095B CN104761095B CN201510182326.5A CN201510182326A CN104761095B CN 104761095 B CN104761095 B CN 104761095B CN 201510182326 A CN201510182326 A CN 201510182326A CN 104761095 B CN104761095 B CN 104761095B
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Abstract
The present invention relates to a kind of method of phenol wastewater Color removal, is operated in accordance with the following steps：To in phenol wastewater, add formalin that condensation reaction is carried out, reacted condensation product is separated, obtains filtrate；To in filtrate, add alkali lye to adjust the Acidity of Aikalinity of waste water again, standing, after being stripped, activated carbon is added to be decolourized, activated carbon and various insoluble matters is filtered out after decolouring, waste water now is in colorless state, then above-mentioned colourless waste water is evaporated crystallization, obtain all qualified ammonium sulfate product of nitrogen content and organic matter.Phenol wastewater color shades before decolouring are 20,000 50000, and before laggard evaporation of decolourizing, waste water color shades are 0 25.The inventive method process is simple, can effective process industry phenol wastewater, again can using the ammonium salt in waste water as byproduct production out, while removing waste water color, it is ensured that the stablizing of ammonium sulfate product quality.
Description
Technical field：
The present invention relates to a kind of technique of phenol wastewater Color removal, more particularly to one kind is containing m-aminophenol and isophthalic
In the mixed phenol of diphenol, the method for Color removal, belongs to technical field of waste water processing.
Background technology：
Resorcinol and m-aminophenol, are important fine-chemical intermediates, have wide range of applications, can be used for rubber,
The industries such as medicine, agricultural chemicals.Meanwhile, phenol wastewater is a kind of industrial wastewater that harm is big, pollution range is wide, and Long Term Contact can be damaged
The nerve of people, the organ such as liver, kidney, drink the water source polluted by phenol for a long time, it may appear that slow poisoning, headache, dizziness, fatigue, mistake
The symptoms such as dormancy, tinnitus, white blood cell decline, anaemia and amnesia, the fish for eating carbdism can cause vomiting and suffer from diarrhoea.For this purpose,
How to handle phenol wastewater well is one of wastewater problem that China's emphasis is solved.
The existing method to phenolic wastewater treatment mainly includes four big class：Chemical oxidization method, bioanalysis, physical method,
Physical chemistry method.The most processing methods such as catalytic wet agent oxidizing process, extraction, biological degradation method and absorption method are enumerated,
But each method has the aspect of its pros and cons, though above method can also effectively remove the phenol organic matter in waste water,
But the feature of the produced waste water of technique of resorcinol is not prepared for m-phenylene diamine (MPD) Hydrolyze method：Isophthalic is not only contained in waste water
The phenol organic matters such as diphenol, m-aminophenol；Additionally, also have a small amount of tar and extractant etc. in waste water, and waste water color is relatively
Deep, also the ammonium sulfate in waste water need to be produced as a by-product come finally, while it is contemplated that financial cost etc. is asked
Topic.
The inventive method prepares the feature of the produced waste water of resorcinol with reference to Hydrolyze method, not only needs the phenols in waste water
Remove, most importantly accessory substance ammonium sulfate is stably produced, this requires that waste water is entering between evaporation to ensure face
Color is in colorless and transparent, to ensure the ammonium sulfate nondiscolouring for crystallizing out.
Content of the invention：
It is an object of the invention to overcoming the shortcoming of prior art, for specific phenol wastewater characteristic, one kind being provided and is contained
The method of phenol waste water Color removal.The inventive method is first got rid of the phenol organic matter in waste water, then by adjusting Acidity of Aikalinity
To ensure the mass fraction of ammonium sulfate, then the organic matter removal for introducing, finally again the Color removal of waste water, to ensure sulphur
The stability of sour ammonium product, the inventive method are reasonably processed to phenol wastewater, have not only reached water treatment effect, also
The stability of ammonium sulfate product in waste water is can guarantee that, while increased income.
In order to realize foregoing invention purpose, a kind of method of phenol wastewater Color removal of the present invention, in accordance with the following steps
Operation：
The first step, the disposable formalin for adding mass percent concentration for 35%-37%, formaldehyde in phenol wastewater
Mol ratio with phenol is 5-6, carries out formaldehyde condensation reaction, filter out insoluble after reaction under 30 DEG C -70 DEG C of steady temperature
Condensation product；
Phenol in the phenol wastewater refers to the mixed phenol of m-aminophenol and resorcinol；Also contain isophthalic two in waste water
Amine, ammonium sulfate and ammonium hydrogen sulfate mixed-ammonium salt, the color of waste water is in peony；Wherein, m-phenylene diamine (MPD) content is in 100-300mg/
L, m-aminophenol content is in 500-1500mg/l, the quality of resorcinol content sulfate in 500-2500mg/l, waste water
Degree is 10%-50%, the pH ＜ 1 of waste water；
Second step, in the clear liquid for filtering out, adds alkaline solution to adjust the pH value of clear liquid waste water for 5-9, standing
0.5h-2h, the content of formaldehyde is in 0-10mg/l；
Described alkaline solution is sodium hydrate aqueous solution, potassium hydroxide aqueous solution, industrial ammonia, liquefied ammonia, calcium hydroxide
The aqueous solution one or several；
3rd step, by the waste water heating after standing until boiling, the mistake of the 10%-40% water by evaporating waste water weight
Journey is further processed to waste water simulating air lift process；
4th step, adds activated carbon to be decolourized by the way of multiple on a small quantity in the waste water in step 3, decolouring institute
It is 30 DEG C -100 DEG C to need temperature, and activated carbon decolorizing time 0.5h-2h after the completion of decolorization, filters out activated carbon, obtains waste water
Clear liquid；
The number of times for adding activated carbon is 2-4 time, and required amounts of activated carbon is waste water weight 2 ‰ -8 ‰ every time；
5th step, is evaporated crystallization the waste water and clear liquid for obtaining, obtains white ammonia sulfate crystal.
In the inventive method step 2, the pH value of waste water after alkali lye adjustment is preferably 5-7, and the time of standing is preferably in 1h-
2h.
In the inventive method step 3, in the method for above-mentioned phenol wastewater Color removal, air lift process is the water for evaporating
The mode that divides, preferably evaporates the moisture of waste water weight 10%-30%.
In the inventive method step 4, the mode of required activated carbon decolorizing using a small amount of repeatedly add by the way of, preferably plus
Indegree is 3-4 time, and required amounts of activated carbon is preferably and accounts for the 3 ‰ -5 ‰ of waste water weight every time, and bleaching temperature is preferably 50 DEG C -80
DEG C, bleaching time is preferably 1h-1.5h, and activated carbon is powder or graininess or bar-shaped one or several.
The color shades before activated carbon is added of phenol wastewater described in the inventive method are 20000-50000, through activated carbon
After decolouring, before entering evaporation, waste water color shades are 0-25.
The ammonium sulfate color that the inventive method is crystallized out is white, and it is 0-25 to be dissolved in colourity after water, ammonium sulfate nitrogen content and
Content of organics meets national standard.
The industrial waste water containing phenol effectively can be processed, the color of waste water by the inventive method process is simple
Achromaticity and clarification shape is removed to, while stable accessory substance ammonium sulfate is obtained, the waste water after process can be effectively recycled again,
Achieve the scientific and effective imagination for processing waste water.
Specific embodiment：
The inventive method is further elaborated below by specific embodiment.
Embodiment 1,
Industrial phenol wastewater 500g is taken in there-necked flask, the index for analyzing the Organic substance in water that now gives up is m-aminophenol
1500mg/l, resorcinol 900mg/l, m-phenylene diamine (MPD) 300mg/l, the pH ＜ 1 of waste water, there-necked flask is placed in 30 DEG C of thermostatted waters
Toward in flask, formalin 1.25g of wt37% in bath, is added, phenol formaldehyde condensation reaction is carried out, precipitation after the completion of reaction, is leached, will
It is 6-7 that filtrate is poured in beaker and adds ammoniacal liquor adjustment pH value, stands 1h, afterwards after the 20% of wastewater quality is evaporated, puts
Put in 50 DEG C of thermostat water baths, when the temperature of waste water also reaches 50 DEG C, add amounts of activated carbon 1.5g to be decolourized, during decolouring
Between be 1h, filter out activated carbon after the completion of decolouring, now color be in peony, add 1.5g activated carbon and decolourized, decolourize
Time is 1h, filters out activated carbon after the completion of decolouring, and now color is once shallow earlier above, repeats this process once, carries out altogether
Decolouring number of times is three times, and waste water color now is in colourless, and colorimetric analysis is 20, and qualified waste water after decolouring is evaporated again
Crystal being crystallized out, the ammonium sulfate product nitrogen content for crystallizing out being analyzed 21%, organic impurities content is qualified, and product colour is in white
Color.
Embodiment 2,
Industrial phenol wastewater 500g is taken in there-necked flask, the index for analyzing the Organic substance in water that now gives up is m-aminophenol
500mg/l, resorcinol 2000mg/l, m-phenylene diamine (MPD) 100mg/l, the pH ＜ 1 of waste water, there-necked flask is placed in 40 DEG C of thermostatted waters
Toward in flask, formalin 1.02g of wt37% in bath, is added, phenol formaldehyde condensation reaction is carried out, precipitation after the completion of reaction, is leached, will
It is 6-7 that filtrate is poured in beaker and adds liquefied ammonia adjustment pH value, stands 1.5h, afterwards after the 40% of wastewater quality is evaporated,
It is placed in 60 DEG C of thermostat water baths, when the temperature of waste water also reaches 60 DEG C, adds amounts of activated carbon 2.0g to be decolourized, decolourize
Time is 75min, filters out activated carbon after the completion of decolouring, and now color is in peony, adds 2.0g activated carbon and is decolourized,
Bleaching time is 75min, filters out activated carbon after the completion of decolouring, and now color is once shallow earlier above, and it is secondary to repeat this process, always
Decolouring number of times is carried out altogether for four times, waste water color now is in colourless, and colorimetric analysis is 12, and qualified waste water after decolouring is entered again
Row evaporative crystallization goes out crystal, analyzes the ammonium sulfate product nitrogen content for crystallizing out 21%, and organic impurities content is qualified, product face
Color is white.
Embodiment 3,
Industrial phenol wastewater 500g is taken in there-necked flask, the index for analyzing the Organic substance in water that now gives up is m-aminophenol
1300mg/l, resorcinol 700mg/l, m-phenylene diamine (MPD) 230mg/l, the pH ＜ 1 of waste water, there-necked flask is placed in 70 DEG C of thermostatted waters
Toward in flask, formalin 2.02g of wt37% in bath, is added, phenol formaldehyde condensation reaction is carried out, precipitation after the completion of reaction, is leached, will
It is 6-7 that filtrate is poured in beaker and adds sodium hydroxide solution adjustment pH value, stands 1h, is evaporating wastewater quality afterwards
After 25%, it is placed in 70 DEG C of thermostat water baths, when the temperature of waste water also reaches 70 DEG C, adds amounts of activated carbon 2.5g to be taken off
Color, bleaching time are 1h, filter out activated carbon after the completion of decolouring, and now color is in peony, and adding 2.5g activated carbon is carried out
Decolourize, bleaching time is 1h, and activated carbon is filtered out after the completion of decolouring, carry out altogether decolouring number of times for secondary, waste water face now
Color is in colourless, and colorimetric analysis is 18, qualified waste water after decolouring is evaporated crystallizing out crystal again, analyzes the sulfuric acid for crystallizing out
, 21%, organic impurities content is qualified, and product colour is white for ammonium product nitrogen content.
Embodiment 4,
Industrial phenol wastewater 500g is taken in there-necked flask, the index for analyzing the organic matter in now waste water is resorcinol
2456mg/l, m-phenylene diamine (MPD) 282mg/l, m-aminophenol 590mg/l, the pH ＜ 1 of waste water, there-necked flask is placed in 60 DEG C of constant temperature
Toward in flask, formalin 1.52g of wt37% in water-bath, is added, phenol formaldehyde condensation reaction is carried out, precipitation after the completion of reaction, is leached,
It is 6-7 filtrate to be poured in beaker and adds ammoniacal liquor adjustment pH value, stands 2h, afterwards after the 35% of wastewater quality is evaporated,
It is placed in 80 DEG C of thermostat water baths, when the temperature of waste water also reaches 80 DEG C, adds amounts of activated carbon 1.8g to be decolourized, decolourize
Time is 1h, filters out activated carbon after the completion of decolouring, and now color is in peony, adds 1.8g activated carbon and is decolourized, and takes off
The color time is 1h, filters out activated carbon after the completion of decolouring, and now color is once shallow earlier above, repeats this process once, Zong Gongjin
Row decolouring number of times is three times, and waste water color now is in colourless, and colorimetric analysis is 21%, and qualified waste water after decolouring is carried out again
Evaporative crystallization goes out crystal, analyzes the ammonium sulfate product nitrogen content for crystallizing out 21%, and organic impurities content is qualified, product colour
White.
Claims (4)
1. a kind of method of phenol wastewater Color removal, it is characterised in that operate in accordance with the following steps：The first step, in phenol wastewater
In the disposable formalin for adding mass percent concentration for 35%-37%, the mol ratio of formaldehyde and phenol is 5-6,30 DEG C-
Formaldehyde condensation reaction is carried out under 70 DEG C of steady temperature, filters out insoluble condensation product after reaction；Second step, is filtering out
In the clear liquid for coming, adding alkaline solution the pH value of clear liquid waste water to be adjusted for 5-9, standing 0.5h-2h, the content of formaldehyde is in 0-
10mg/l；3rd step, by the waste water heating after standing until boiling, the mistake of the 10%-40% water by evaporating waste water weight
Journey is further processed to waste water simulating air lift process；4th step, using side multiple on a small quantity in the waste water in step 3
Formula adds activated carbon to be decolourized, and it is 30 DEG C -100 DEG C to decolourize temperature required, activated carbon decolorizing time 0.5h-2h, decolorization
After the completion of, activated carbon is filtered out, obtains waste water and clear liquid；The number of times for adding activated carbon is 2-4 time, every time required amounts of activated carbon
For waste water weight 2 ‰ -8 ‰；5th step, is evaporated crystallization the waste water and clear liquid for obtaining, obtains white ammonia sulfate crystal, sulfuric acid
After ammonium is dissolved in water, colourity is 0-25.
2. a kind of method of phenol wastewater Color removal according to claim 1, it is characterised in that the phenol in phenol wastewater
Refer to the mixed phenol of m-aminophenol and resorcinol；Also contain m-phenylene diamine (MPD), ammonium sulfate and ammonium hydrogen sulfate mixing ammonium in waste water
Salt, the color of waste water is in peony；Wherein, in 100-300mg/l, m-aminophenol content is in 500- for m-phenylene diamine (MPD) content
1500mg/l, the mass percentage content of resorcinol content sulfate in 500-2500mg/l, waste water is 10%-50%,
The pH ＜ 1 of waste water；Phenol wastewater color shades before activated carbon is added are 20000-50000, after activated carbon decolorizing, enter to steam
Before sending out crystallization, waste water color shades are 0-25.
3. a kind of method of phenol wastewater Color removal according to claim 1, it is characterised in that the alkali described in second step
Property solution be sodium hydrate aqueous solution, potassium hydroxide aqueous solution, industrial ammonia, calcium hydroxide aqueous solution one or several.
4. a kind of method of phenol wastewater Color removal according to claim 1, it is characterised in that activated carbon in the 4th step
Number of times is preferably added to for 3-4 time, required amounts of activated carbon is preferably and accounts for the 3 ‰ -5 ‰ of waste water weight every time, and bleaching temperature is preferably
50 DEG C -80 DEG C, bleaching time is preferably 1h-1.5h, and activated carbon is powder or graininess or bar-shaped a kind of or several
Kind.
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| CN107572739A (en) * | 2017-11-12 | 2018-01-12 | 济宁市山化环保科技有限公司 | A kind of method for being used to prevent that Organic substance in water from contacting with water |
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