CN109111014A - A kind of resource utilization method of the aldehyde-containing sewage containing phenol - Google Patents
A kind of resource utilization method of the aldehyde-containing sewage containing phenol Download PDFInfo
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- CN109111014A CN109111014A CN201710494960.1A CN201710494960A CN109111014A CN 109111014 A CN109111014 A CN 109111014A CN 201710494960 A CN201710494960 A CN 201710494960A CN 109111014 A CN109111014 A CN 109111014A
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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
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G12/00—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen
- C08G12/02—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes
- C08G12/04—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds
- C08G12/10—Condensation polymers of aldehydes or ketones with only compounds containing hydrogen attached to nitrogen of aldehydes with acyclic or carbocyclic compounds with acyclic compounds having the moiety X=C(—N<)2 in which X is O, S or —N
- C08G12/12—Ureas; Thioureas
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G8/00—Condensation polymers of aldehydes or ketones with phenols only
- C08G8/04—Condensation polymers of aldehydes or ketones with phenols only of aldehydes
- C08G8/08—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ
- C08G8/10—Condensation polymers of aldehydes or ketones with phenols only of aldehydes of formaldehyde, e.g. of formaldehyde formed in situ with phenol
-
- 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
- C02F1/66—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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F2001/007—Processes including a sedimentation step
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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
- C02F2101/34—Organic compounds containing oxygen
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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
- C02F2101/34—Organic compounds containing oxygen
- C02F2101/345—Phenols
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F3/00—Biological treatment of water, waste water, or sewage
- C02F3/02—Aerobic processes
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Water Treatment By Sorption (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Phenolic Resins Or Amino Resins (AREA)
Abstract
The invention discloses a kind of resource utilization method of aldehyde-containing sewage containing phenol, method particularly includes: phenol is added into waste water according to the ratio, adjusts pH, is heated to reflux, lower-layer resin is discharged after polycondensation, obtain aqueous solution；Then urea is added into aqueous solution, room temperature is stood after stirring, reaction liquid layer, and lower sediment is discharged, recycles after drying；Upper layer reaction solution is through macroporous absorbent resin adsorption treatment；Aerobic treatment finally is carried out to adsorption liquid.The removal rate of the method for the present invention PARA FORMALDEHYDE PRILLS(91,95) and free phenol up to 100%, COD removal rate up to 99.5% or more.The method of the present invention first by the most of phenol and formaldehyde resource utilization in waste water, has not only saved processing cost, and be conducive to subsequent processing, changes phenolic resin industry wastewater treatment hardly possible, status at high cost.The method of the present invention simple process, small investment, treatment effect is good, and no solid waste generates, and reaction product is recyclable, has good economic benefit.
Description
Technical field
The present invention relates to a kind of resource utilization methods of aldehyde-containing sewage containing phenol, especially carry out advanced treating simultaneously to waste water
It is subject to the method for resource utilization to the product in treatment process.
Background technique
Phenol and formaldehyde belong to very harmful, intractable substance, have high bio-toxicity, the serious life for inhibiting microorganism
It is long, it is difficult to directly progress biochemical treatment.
Formaldehyde and phenol toxicity are high in aldehyde-containing sewage containing phenol, and processing difficulty is very big.Currently, the domestic processing side to this kind of waste water
Method has: extraction, rectifying, polycondensation, chemical oxidation, photochemical catalytic oxidation, wet oxidation etc., wherein most commonly used is condensation methods, i.e.,
In acid condition, the phenol in suitable formaldehyde or phenol, with waste water is added or formaldehyde occurs polycondensation and generates liquid resin removing,
But phenol and formaldehyde are still very high in processed waste water, can not carry out biochemical treatment, also need that above-mentioned other methods is combined further to locate
Reason, the disadvantage that these methods are big in the prevalence of investment, operating cost is high.
Application No. is 201010229184.0 patents of invention to disclose a kind of method of comprehensive utilization of phenolic resin wastewater,
This method is that formaldehyde, acidic catalyst is added to phenolic resin wastewater to finally obtain free phenol by polycondensation, secondary polycondensation and contain
Amount is lower than 1% waste water, and the effluent part a part for producing water-soluble resin, a part is for absorbing formaldehyde exhaust-gas system
At industrial formol；This method is only applicable to the phenolic resin wastewater of the high phenol containing low aldehyde, is obviously not suitable for the waste water of the low phenol of high aldehyde.
Application No. is 200910015673.3 patent documents to disclose a kind of processing method of high density wastewater during phenolic resin production, should
Method is that phenolic resin hc effluent and industrial salt are mixed, stratification, upper layer crude phenols reuse, lower layer's saturated brine
Evaporative desalination, salinity recycling, is adsorbed after evaporating liquid condensing through adsorption column；This method seems simply, but 65%~78% crude phenols
It is unable to direct reuse in some phenolic resin domain variabilities, and evaporation process will cause formaldehyde volatilization, pollute environment, subsequent adsorbtion
It handles bad to high-concentration formaldehyde wastewater effect.
Summary of the invention
The present invention overcomes the above-mentioned problems in the prior art, on the basis of polycondensation, in conjunction with ureaformaldehyde, absorption, biochemistry
Etc. serial of methods, provide a kind of resource utilization method of aldehyde-containing sewage containing phenol, the removal rate of formaldehyde and free phenol reaches
The removal rate of 100%, COD can also be subject to resource utilization up to 99.5% or more, while to reaction product, have warp well
Ji benefit.
The resource utilization method of a kind of aldehyde-containing sewage containing phenol proposed by the present invention, comprising the following steps: useless containing aldehyde containing phenol
Phenol is added in water according to the ratio, and acidic catalyst is added and adjusts pH, after polycondensation reaction occurs for heating, lower-layer resin is periodically discharged,
Aqueous solution is obtained after reaction；Then urea is added into aqueous solution, room temperature is stood after stirring, reaction liquid layer, under discharge
Layer precipitating, is recycled after drying；Upper layer reaction solution is through macroporous absorbent resin adsorption treatment, further progress aerobic treatment.
Specifically, it the described method comprises the following steps:
(1) phenol is added into aldehyde-containing sewage containing phenol, and acidic catalyst is added and adjusts pH, heating carries out polycondensation reaction,
Lower-layer resin is discharged, obtains aqueous solution after reaction；
(2) aldehyde in the aqueous solution that determination step (1) obtains, is proportionally added into urea, and room temperature is stood after stirring, to
After reaction liquid layer, lower sediment is discharged, is recycled after drying；
(3) the remaining phase supernatant of step (2) is passed through into absorption resin adsorption；
(4) waste water after step (3) absorption is subjected to aerobic treatment, the waste water of emission request must be reached.
In step (1) of the present invention, the aldehyde-containing sewage containing phenol, aldehyde is 1000~80000mg/L, phenol content 150
~7000mg/L, COD are 1500~120000mg/L.
In step (1) of the present invention, the phenol and the molar ratio containing formaldehyde in phenolic wastewater are 1:5~1:15；Preferably,
For 1:5~1:10.
In step (1) of the present invention, the acidic catalyst be selected from hydrochloric acid, sulfuric acid, phosphoric acid, hypochlorous acid, p-methyl benzenesulfonic acid,
One of oxalic acid etc. is a variety of；It preferably, is the mixed acid of hydrochloric acid, p-methyl benzenesulfonic acid, hypochlorous acid or oxalic acid and sulfuric acid.
In step (1) of the present invention, it is between 1~2 that the acidic catalyst, which adjusts pH,.
In step (1) of the present invention, the temperature of the polycondensation reaction is 80~100 DEG C；It is further preferred that being 80 DEG C, 85
℃、90℃、100℃。
In step (1) of the present invention, the time of the polycondensation reaction is 6~10 hours；It preferably, is 6 hours, 7 hours, 8
Hour, 9 hours.
It, must be by the way of lower-layer resin periodically be discharged, when the periodicity of lower-layer resin is discharged in step (1) of the present invention
Between be 1~2 hour, specific method is every 1~2 hour openings bottom valve, and observation white oil resin closes after being completely exhausted out
Valve closing door.
In step (2) of the present invention, the urea is carbamide.
In step (2) of the present invention, the molar ratio of formaldehyde in aqueous solution and urea that step (1) obtains is 1:1~1:4；It is excellent
Selection of land is 1:1~1:2.
In step (3) of the present invention, the absorption resin is preferably macroporous absorbent resin, and aperture is between 0.3~1.2mm；
As D113, D201, D101, D900, H103, HPD100, one of HPD400 or a variety of can be selected in model；Preferably, it is
D113, HPD100, D900 and H103 are uniformly mixed by weight the mixed uniformly resin of 1:2 or D900 and H103 by weight 1:2
The resin of conjunction.
In step (4) of the present invention, aerobic treatment is carried out using conventional method.
A kind of resource utilization method of the aldehyde-containing sewage containing phenol of the present invention, specifically includes the following steps:
(1) waste water that tire is generated with function production of resins process, phenol are subjected to ingredient by phenolic aldehyde molar ratio, are placed in
It in batch condensation polymerization reactor, is uniformly mixed by agitating device in polycondensation vessel, acidic catalyst is then added and adjusts pH to 1~2, heating
To reflux state, polycondensation reaction is carried out, lower-layer resin is periodically discharged, obtains aqueous solution after reaction.
(2) aldehyde in the aqueous solution that determination step (1) obtains, is proportionally added into urea, and room temperature is stood after stirring, to
After reaction liquid layer, lower sediment is discharged, is recycled after drying；
(3) the remaining phase of step (2) is passed through into absorption resin adsorption；
(4) waste water after step (3) absorption is subjected to aerobic treatment, reaches emission request.
The resource utilization method of the aldehyde-containing sewage provided by the invention containing phenol, principle are: phenol gives up with containing phenol containing aldehyde
Polycondensation reaction occurs in acid condition for the formaldehyde in water, generates liquid resin, isolates liquid resin, recycle most of phenol and
Fraction formaldehyde；The formaldehyde contained in remaining aqueous solution occurs ureaformaldehyde with urea and reacts, and generates Lauxite, further recycles
Formaldehyde；The remaining macroporous resin adsorption that communicated removes most of phenol；It further degrades COD, reaches finally by aerobic biochemical pool
Emission request.
The present invention provides a kind of resource utilization methods of aldehyde-containing sewage containing phenol, firstly, will contain phenol using polycondensation reaction
Most of phenol recycling in aldehyde-containing sewage, obtains the liquid resin of use value；Then remaining useless using ureaformaldehyde reaction recycling
Most of formaldehyde in water, obtains the Lauxite of use value；Again by macroporous resin adsorption phenol, biodegradability is improved
Enter biochemical treatment afterwards.Compared with art methods, the method for the present invention is not to consider using phenol and formaldehyde as waste processing, and
Be its resource utilization has not only been saved into processing cost, and be conducive to subsequent processing first, meanwhile, by high-concentration waste water
During processing is low concentration wastewater, obtained reaction product can be further employed, and no solid waste generates, and be had good
Economic benefit changes phenolic resin industry wastewater treatment hardly possible, status at high cost.
The beneficial effects of the present invention are it is (main for 1500~120000mg/L, aldehyde that the method for the present invention is able to bear COD
For formaldehyde) content is 1000~80000mg/L, phenol content is 150~7000mg/L aldehyde-containing sewage containing phenol.First in waste water
After formaldehyde and phenol are adequately recycled and pre-processed, the biodegradability of waste water is substantially increased.It is generated in treatment process
Liquid resin and Lauxite can recycle, resource utilization.Using processing method of the invention, PARA FORMALDEHYDE PRILLS(91,95) and free phenol are gone
Except rate up to 100%, COD removal rate up to 99.5% or more.The required equipment of the present invention is reaction kettle, adsorption column and biochemistry
Pond, equipment is simple, at low cost, and treatment effect is good, and no solid waste generates, and reaction product is recyclable, has good economic benefit.
Detailed description of the invention
Fig. 1 is the schematic diagram of the resource utilization method of the aldehyde-containing sewage of the invention containing phenol.
Specific embodiment
In conjunction with following specific embodiments and attached drawing, the present invention is described in further detail.Implement process of the invention,
Condition, experimental method etc. are among the general principles and common general knowledge in the art, this hair in addition to what is specifically mentioned below
It is bright that there are no special restrictions to content.
Examples 1 to 4
7t aldehyde-containing sewage containing phenol is placed in batch condensation polymerization reactor, phenol is added by phenolic aldehyde molar ratio and carries out ingredient, and passes through
Agitating device is uniformly mixed in kettle, and acidic catalyst is then added and adjusts pH to 1~2, is heated to reflux state, periodically
Be discharged lower-layer resin, react 6~10 hours, after obtain aqueous solution, measure the content of formaldehyde of aqueous solution, be proportionally added into urine
Element, room temperature is stood after stirring, after reaction liquid layer, lower sediment is discharged, recycles after drying, and supernatant is passed through to be inhaled equipped with macropore
It is adsorbed in the adsorption column of attached resin (aperture is between 0.3~1.2mm), the waste water after absorption is directly entered at aerobic biochemical
Reason.
Table 1
For waste water after a series of processing such as polycondensation reaction, ureaformaldehyde reaction, resin adsorption, the concentration of free phenol can be down to 1mg/
L is hereinafter, formaldehyde can be down to 50mg/L or less；After subsequent biochemical processing, the removal rate of COD is up to 99.5% or more, in treatment process
The liquid resin and Lauxite of generation are total to 13~1444 yuan of income (processing 7t waste water) and differ.
In the present invention, using other acidic catalysts, as hydrochloric acid, sulfuric acid, phosphoric acid, hypochlorous acid, p-methyl benzenesulfonic acid,
One of oxalic acid or it is a variety of when, can also reach above-mentioned same technical effect.
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 (10)
1. a kind of resource utilization method of aldehyde-containing sewage containing phenol, which is characterized in that comprise the steps of:
(1) phenol is added into aldehyde-containing sewage containing phenol, and acidic catalyst is added and adjusts pH, heating carries out polycondensation reaction, discharge
Lower-layer resin obtains aqueous solution after reaction；
(2) aldehyde in the aqueous solution that determination step (1) obtains, is proportionally added into urea, and room temperature is stood after stirring, wait react
After liquid layering, lower sediment is discharged, is recycled after drying；
(3) the remaining phase of step (2) is passed through into absorption resin adsorption；
(4) waste water after step (3) absorption is subjected to aerobic treatment, the waste water of emission request must be reached.
2. the method according to claim 1, wherein described containing in phenolic wastewater, aldehyde is 1000~
80000mg/L, phenol content are 150~7000mg/L, and COD is 1500~120000mg/L.
3. the method according to claim 1, wherein in step (1), added phenol with containing formaldehyde in phenolic wastewater
Molar ratio be 1:5~1:15.
4. the method according to claim 1, wherein the acidic catalyst is selected from hydrochloric acid, sulphur in step (1)
One of acid, phosphoric acid, hypochlorous acid, p-methyl benzenesulfonic acid, oxalic acid are a variety of.
5. the method according to claim 1, wherein in step (1), the acidic catalyst adjust pH be 1~
2。
6. the method according to claim 1, wherein in step (1), the temperature of the polycondensation reaction is 80~
100℃。
7. the method according to claim 1, wherein the time of the polycondensation reaction is 6~10 in step (1)
Hour；The periodical time that lower-layer resin by the way of lower-layer resin periodically is discharged, must be discharged is 1~2 hour.
8. the method according to claim 1, wherein in step (2), in the aqueous solution that the step (1) obtains
The molar ratio of formaldehyde and urea is 1:1~1:4.
9. the method according to claim 1, wherein the absorption resin is macroporous absorption tree in step (3)
Rouge, aperture is between 0.3~1.2mm.
10. the method according to claim 1, wherein in step (3), the macroporous absorbent resin be selected from D113,
One of D201, D101, D900, H103, HPD100, HPD400 or a variety of.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710494960.1A CN109111014B (en) | 2017-06-26 | 2017-06-26 | Resource utilization method of phenol-containing and aldehyde-containing wastewater |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710494960.1A CN109111014B (en) | 2017-06-26 | 2017-06-26 | Resource utilization method of phenol-containing and aldehyde-containing wastewater |
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| CN109111014A true CN109111014A (en) | 2019-01-01 |
| CN109111014B CN109111014B (en) | 2021-08-27 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111533377A (en) * | 2020-05-11 | 2020-08-14 | 恩宜瑞(江苏)环境发展有限公司 | High-concentration phenolic resin wastewater recycling treatment system and process |
| CN112062363A (en) * | 2020-09-08 | 2020-12-11 | 沙县宏盛塑料有限公司 | Treatment method of phenolic resin industrial wastewater |
| CN112062362A (en) * | 2020-09-08 | 2020-12-11 | 沙县宏盛塑料有限公司 | Treatment method of high-concentration aldehyde-containing phenolic resin wastewater |
| CN114213610A (en) * | 2022-01-13 | 2022-03-22 | 彤程电子材料(镇江)有限公司 | Powder phenolic resin and production process thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86107846A (en) * | 1986-11-19 | 1988-06-01 | 化工部第三设计院 | The methyne urea precipitator method are removed the formaldehyde in the trade effluent |
| RU2028978C1 (en) * | 1992-02-03 | 1995-02-20 | Юрий Георгиевич Скрыпник | Method of sewage treatment from phenol |
| CN101037283A (en) * | 2007-02-27 | 2007-09-19 | 海盐华强树脂有限公司 | Treatment method of hydroxybenzene-containing wastewater |
-
2017
- 2017-06-26 CN CN201710494960.1A patent/CN109111014B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN86107846A (en) * | 1986-11-19 | 1988-06-01 | 化工部第三设计院 | The methyne urea precipitator method are removed the formaldehyde in the trade effluent |
| RU2028978C1 (en) * | 1992-02-03 | 1995-02-20 | Юрий Георгиевич Скрыпник | Method of sewage treatment from phenol |
| CN101037283A (en) * | 2007-02-27 | 2007-09-19 | 海盐华强树脂有限公司 | Treatment method of hydroxybenzene-containing wastewater |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111533377A (en) * | 2020-05-11 | 2020-08-14 | 恩宜瑞(江苏)环境发展有限公司 | High-concentration phenolic resin wastewater recycling treatment system and process |
| CN112062363A (en) * | 2020-09-08 | 2020-12-11 | 沙县宏盛塑料有限公司 | Treatment method of phenolic resin industrial wastewater |
| CN112062362A (en) * | 2020-09-08 | 2020-12-11 | 沙县宏盛塑料有限公司 | Treatment method of high-concentration aldehyde-containing phenolic resin wastewater |
| CN112062362B (en) * | 2020-09-08 | 2023-02-03 | 沙县宏盛塑料有限公司 | Treatment method of high-concentration aldehyde-containing phenolic resin wastewater |
| CN112062363B (en) * | 2020-09-08 | 2023-02-03 | 沙县宏盛塑料有限公司 | Treatment method of phenolic resin industrial wastewater |
| CN114213610A (en) * | 2022-01-13 | 2022-03-22 | 彤程电子材料(镇江)有限公司 | Powder phenolic resin and production process thereof |
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