CN106430768B - A kind of processing method of phenolic resin aldehyde-containing sewage containing phenol - Google Patents
A kind of processing method of phenolic resin aldehyde-containing sewage containing phenol Download PDFInfo
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- CN106430768B CN106430768B CN201510485950.2A CN201510485950A CN106430768B CN 106430768 B CN106430768 B CN 106430768B CN 201510485950 A CN201510485950 A CN 201510485950A CN 106430768 B CN106430768 B CN 106430768B
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Abstract
The invention discloses a kind of processing methods of the aldehyde-containing sewage containing phenol generated in phenolic resin production process, phenolic resin wastewater is passed through reaction kettle, it is proportionally added into CaO, it is uniformly mixed by agitating device in kettle, it is after heat temperature raising reflux, reaction solution is cooling, it is proportionally added into NaOH, continue heat temperature raising reflux, distillation separates aqueous solution.It is handled through the method for the present invention, the removal rate of formaldehyde is up to 100%, and the removal rate of free phenol is up to 98% or more, to the reduction amplitude of COD up to 67% or more.Present invention process is simple, and operating cost is low, and treatment effeciency is high.
Description
Technical field
The present invention relates to the processing of waste water, specifically, being the phenolic resin generated in a kind of phenolic resin production process
The processing method of the aldehyde-containing sewage containing phenol.
Technical background
Phenol wastewater is a kind of seriously polluted, big, intractable industrial wastewater of harm, has bio-toxicity, inhibits micro- life
The growth of object, it is difficult to directly progress biochemical treatment.People take many methods and handle this kind of waste water for many years, mainly there is materialization
Method and biochemical method.Physico-chemical process includes extraction, rectifying, ion exchange, chemical oxidation, reverse osmosis, photochemical catalytic oxidation, electrodialysis etc..
Its common feature is the presence of secondary pollution, increases the difficulty of subsequent biochemical processing.The photochemistry that Soviet Union scholar proposes
Method can only handle low concentration phenol wastewater (50mg/L).
It is a kind of gas colourless, with penetrating odor under formaldehyde room temperature, it is soluble easily in water, the intracorporal egg of microorganism can be made
White matter solidification denaturation, inhibits its activity even to cause death.Physico-chemical process is broadly divided into about the treatment process of formaldehyde waste water at present
And biochemical method.Physico-chemical process mainly has polymerization, Fenton oxidation, electrochemical oxidation, wet oxidation etc., but higher cost.Biochemical method
Less expensive, but impact resistance is poor, impacts influence vulnerable to water quality.
Summary of the invention
The present invention overcomes the above-mentioned problems in the prior art, provides a kind of place of phenolic resin aldehyde-containing sewage containing phenol
Reason method.There is at low cost, high-efficient advantage using the method for the present invention processing high-concentration phenol urea formaldehyde aldehyde-containing sewage containing phenol.
The processing method of a kind of phenolic resin aldehyde-containing sewage containing phenol proposed by the present invention, by phenolic resin aldehyde-containing sewage containing phenol
It is passed through reaction kettle, CaO is added, is uniformly mixed by agitating device in kettle, then heat temperature raising flows back, and reaction solution is cooling, add
Enter NaOH, continue heat temperature raising reflux, the aqueous solution of low COD is isolated in distillation.
In the present invention, " the phenolic resin aldehyde-containing sewage containing phenol " refers to that is generated in phenolic resin production process contains containing phenol
The waste water of aldehyde.
Wherein, in the phenolic resin aldehyde-containing sewage containing phenol, contained COD (COD) is 100~100500mg/
L, contained aldehyde are 250~45900mg/L, and contained phenol content is 150~15300mg/L.Wherein, the aldehyde includes first
Aldehyde.
Wherein, the additional proportion of the CaO is the 0.5%~2.5% of phenolic resin aldehyde-containing sewage containing the phenol weight.
Wherein, the source CaO is quick lime.
Wherein, the heating temperature after CaO is added, that is, the temperature of first time heat temperature raising is 80~100 DEG C, when reaction
Between be 60~120min.
Wherein, the additional proportion of the NaOH is the 0.5%~2.5% of phenolic resin aldehyde-containing sewage containing the phenol weight.
Wherein, the source of the NaOH is liquid alkaline or solid sodium hydroxide.
Wherein, the heating temperature after NaOH is added, that is, the temperature for continuing heat temperature raising is 80~100 DEG C, the reaction time
For 60~120min.
Wherein, the temperature that reaction solution is cooling is 0~30 DEG C.
Wherein, after the method for the present invention is handled, low COD water phase is obtained, the removal rate of PARA FORMALDEHYDE PRILLS(91,95) is up to 100%, to free
The removal rate of phenol is up to 98% or more, to the reduction amplitude of COD up to 67% or more.
Processing method of the present invention comprising the following specific steps
(1) phenolic resin aldehyde-containing sewage containing phenol is passed through reaction kettle, is proportionally added into CaO, it is mixed by agitating device in kettle
It closes uniform；
(2) heat temperature raising flows back step (1) afterwards, and the formaldehyde in polymerization reaction and disproportionated reaction removal waste water occurs；
(3) reaction solution to step (2) is cooled to room temperature, and is proportionally added into NaOH；
(4) reaction solution of step (3) is continued into heat temperature raising reflux, removes the phenol in waste water；
(5) step (4) is distilled afterwards, isolates low COD water phase, wherein the removal rate of the low COD water phase formaldehyde is reachable
100%, the removal rate of free phenol is up to the reduction amplitude of 98% or more, COD up to 67% or more.
Wherein, COD contained in phenolic resin aldehyde-containing sewage containing phenol is 100~100500mg/L, and contained aldehyde is
250~45900mg/L, contained phenol content are 150~15300mg/L.
Wherein, in step (1), the ratio of CaO is 0.5%~2.5%；Preferably, the additional proportion of CaO be 0.5%~
1%.
Wherein, in step (2), heating temperature is 80~100 DEG C, and the reaction time is 60~120min；Preferably, heating temperature
Degree is 80~90 DEG C, and the reaction time is 60~90min.
Wherein, in step (3), the ratio of NaOH is 0.5%~2.5%；Preferably, the additional proportion of NaOH be 1%~
2%.
Wherein, in step (4), heating temperature is 80~100 DEG C, and the reaction time is 60~120min；Preferably, heating temperature
Degree is 90~100 DEG C, and the reaction time is 60~90min.
The invention proposes a kind of novel process, using the such high-concentration phenol urea formaldehyde aldehyde-containing sewage containing phenol of alkali process,
Principle is: using alkali respectively with the phenol and aldehyde reaction in phenolic resin aldehyde-containing sewage containing phenol, water temperature be higher than 80 DEG C when, a side
Face, oxymethylene polymerization is at the formose of no biotoxicity, and on the other hand disproportionation generates methanol and formates；Free phenol and alkali generate
Phenates；Under the catalysis of alkali, free phenol and formaldehyde generate polymer.Alkali is from a wealth of sources, cheap, the expense of the method for the present invention
Well below general physico-chemical process, and subsequent microbiological treatment will not be had an impact.
Beneficial effect of the present invention further include: it is 100~100500mg/L, content of formaldehyde that the method for the present invention, which is able to bear COD,
The phenolic wastewater for being 150~15300mg/L for 250~45900mg/L, phenol content reduces operation without adding fresh water dilution
Cost.Processing method of the present invention, the removal rate of PARA FORMALDEHYDE PRILLS(91,95) are right to the removal rate of free phenol up to 98% or more up to 100%
The reduction amplitude of COD is up to 67% or more.Present invention process is simple, and treated, and waste water can direct biochemical treatment.
Detailed description of the invention
Fig. 1 is the schematic diagram of processing method of the present invention.
Specific embodiment
In conjunction with following specific embodiments and attached drawing, the present invention is described in further detail, protection content of the invention
It is not limited to following embodiment.Without departing from the spirit and scope of the invention, those skilled in the art it is conceivable that change
Change and advantage is all included in the present invention, and using appended claims as protection scope.Implement process of the invention,
Condition, reagent, experimental method etc. are among the general principles and common general knowledge in the art in addition to what is specifically mentioned below,
There are no special restrictions to content by the present invention.
Embodiment 1
Pilot scale is carried out in reaction kettle of the 10t with agitating device, takes 7t phenolic resin (certain phenolic resin of aldehyde-containing sewage containing phenol
Factory's waste water, measuring water sample pH is 2.72, COD 67500mg/L, and contained concentration of formaldehyde is 24300mg/L, and phenol concentration is
It 11400mg/L) is uniformly mixed in a kettle, adds the quick lime of 35kg, be sufficiently mixed by agitating device in kettle, started
Reaction kettle heating, after being warming up to 80 DEG C, maintains the reflux for 90min, is then turned off heating and reflux, naturally cool to reaction kettle
0~30 DEG C, the solid sodium hydroxide of 70kg is added, after stirring sufficiently, reaction kettle heating is again started up, is protected after being warming up to 90 DEG C
Reflux 90min is held, distillation process is then started, separation aqueous solution is recycled by condenser pipe.It is analyzed, obtained aqueous solution
COD is 13300mg/L (i.e. the reduction amplitude of COD is about 80.3%), and (i.e. the removal rate of formaldehyde up to 100%) is not detected in formaldehyde,
Phenol concentration is 3mg/L (i.e. the removal rate of free phenol close to 100%).
Embodiment 2
Pilot scale is carried out in reaction kettle of the 10t with agitating device, takes 7t phenolic resin (certain phenolic resin of aldehyde-containing sewage containing phenol
Factory's waste water, measuring water sample pH is 2.66, COD 90400mg/L, and contained concentration of formaldehyde is 37100mg/L, and phenol concentration is
5100mg/L), it is uniformly mixed in a kettle, adds the quick lime of 35kg, be uniformly mixed by agitating device in kettle, starting
Reaction kettle heating, after being warming up to 85 DEG C, maintains the reflux for 60min, is then turned off heating and reflux, naturally cool to reaction kettle
0~30 DEG C, the solid sodium hydroxide of 105kg is added, after stirring sufficiently, reaction kettle heating is again started up, after being warming up to 100 DEG C
120min is maintained the reflux for, distillation process is then started, separation aqueous solution is recycled by condenser pipe.It is isolated through analyzing
Water phase COD is 20900mg/L (i.e. the reduction amplitude of COD is about 76.9%), and formaldehyde is not detected that (i.e. the removal rate of formaldehyde reaches
100%), phenol concentration is 58mg/L (i.e. the removal rate of free phenol up to 98.8%).
Embodiment 3
Pilot scale is carried out in reaction kettle of the 10t with agitating device, takes 7t phenolic resin (certain phenolic resin of aldehyde-containing sewage containing phenol
Factory's waste water, measuring water sample pH is 2.45, COD 100500mg/L, and contained concentration of formaldehyde is 25200mg/L, and phenol concentration is
15300mg/L), it is uniformly mixed in a kettle, adds the quick lime of 70kg, be uniformly mixed, opened by agitating device in kettle
Dynamic reaction kettle heating, after being warming up to 90 DEG C, maintains the reflux for 90min, is then turned off heating and reflux, make reaction kettle natural cooling
To 0~30 DEG C, the solid sodium hydroxide of 105kg is added, after stirring sufficiently, reaction kettle heating is again started up, is warming up to 95 DEG C
After maintain the reflux for 60min, then start distillation process, pass through condenser pipe recycling separation aqueous solution.It is isolated through analyzing
Water phase COD is 33600mg/L (i.e. the reduction amplitude of COD is about 66.6%), and formaldehyde is not detected that (i.e. the removal rate of formaldehyde reaches
100%), phenol concentration is 60mg/L (i.e. the removal rate of free phenol up to 99.6%).
Embodiment 4
Pilot scale is carried out in reaction kettle of the 10t with agitating device, takes 7t phenolic resin (certain phenolic resin of aldehyde-containing sewage containing phenol
Factory's waste water, measuring water sample pH is 2.50, COD 84200mg/L, and contained concentration of formaldehyde is 45900mg/L, and phenol concentration is
8300mg/L), it is uniformly mixed in a kettle, adds the quick lime of 175kg, be uniformly mixed, opened by agitating device in kettle
Dynamic reaction kettle heating, after being warming up to 80 DEG C, maintains the reflux for 60min, is then turned off heating and reflux, make reaction kettle natural cooling
To 0~30 DEG C, the solid sodium hydroxide of 35kg is added, after stirring sufficiently, reaction kettle heating is again started up, after being warming up to 95 DEG C
90min is maintained the reflux for, distillation process is then started, separation aqueous solution is recycled by condenser pipe.Through analyzing, isolated water
Phase COD is 17800mg/L (i.e. the reduction amplitude of COD is about 78.9%), and formaldehyde is not detected that (i.e. the removal rate of formaldehyde reaches
100%), phenol concentration is 113mg/L (i.e. the removal rate of free phenol up to 98.6%).
Embodiment 5
Pilot scale is carried out in reaction kettle of the 10t with agitating device, takes 7t phenolic resin (certain phenolic resin of aldehyde-containing sewage containing phenol
Factory's waste water, measuring water sample pH is 2.84, COD 82800mg/L, and contained concentration of formaldehyde is 24300mg/L, and phenol concentration is
1140mg/L), it is uniformly mixed in a kettle, adds the quick lime of 70kg, be uniformly mixed by agitating device in kettle, starting
Reaction kettle heating, after being warming up to 90 DEG C, maintains the reflux for 60min, is then turned off heating and reflux, naturally cool to reaction kettle
0~30 DEG C, the solid sodium hydroxide of 175kg is added, after stirring sufficiently, reaction kettle heating is again started up, after being warming up to 90 DEG C
60min is maintained the reflux for, distillation process is then started, separation aqueous solution is recycled by condenser pipe.Through analyzing, isolated water
Phase COD is 26300mg/L (i.e. the reduction amplitude of COD is about 68.2%), and formaldehyde is not detected that (i.e. the removal rate of formaldehyde reaches
100%), phenol concentration is 22mg/L (i.e. the removal rate of free phenol up to 98%).
Protection content of the invention is not limited to above embodiments.Without departing from the spirit and scope of the invention, originally
Field technical staff it is conceivable that variation and advantage be all included in the present invention, and with appended claims be protect
Protect range.
Claims (5)
1. a kind of processing method of phenolic resin aldehyde-containing sewage containing phenol, it is characterised in that: lead to phenolic resin aldehyde-containing sewage containing phenol
Enter reaction kettle, CaO is added, be uniformly mixed by agitating device in kettle, carries out the reflux of first time heat temperature raising, it then will be wait react
But, NaOH is added in liquid cooling, carries out second of heat temperature raising reflux, and distillation separates aqueous solution；The additional proportion of the CaO is
The 0.5%~2.5% of phenolic resin aldehyde-containing sewage containing the phenol weight, the additional proportion of the NaOH are that the phenolic resin contains
The 0.5%~2.5% of phenol aldehyde-containing sewage weight.
2. the method according to claim 1, wherein in the phenolic resin aldehyde-containing sewage containing phenol, contained aldehyde
Content is 250~45900mg/L, and contained phenol content is 150~15300mg/L, and contained COD is 100~100500mg/L.
3. the method according to claim 1, wherein the temperature of the first time heat temperature raising be 80~100 DEG C,
Reaction time is 60~120min.
4. the method according to claim 1, wherein the temperature of second of heat temperature raising be 80~100 DEG C,
Reaction time is 60~120min.
5. the method according to claim 1, wherein the removal rate of PARA FORMALDEHYDE PRILLS(91,95) is reachable after the method processing
100%, to the removal rate of free phenol up to 98% or more, to the reduction amplitude of COD up to 67% or more.
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| CN109179628A (en) * | 2018-09-14 | 2019-01-11 | 中国科学院青岛生物能源与过程研究所 | A method of reducing phenol wastewater phenol content |
| CN113620499A (en) * | 2021-09-07 | 2021-11-09 | 南京齐超环保科技有限公司 | Phenolic aldehyde wastewater pretreatment combined process |
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