CN112062363B - Treatment method of phenolic resin industrial wastewater - Google Patents
Treatment method of phenolic resin industrial wastewater Download PDFInfo
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- CN112062363B CN112062363B CN202010934196.7A CN202010934196A CN112062363B CN 112062363 B CN112062363 B CN 112062363B CN 202010934196 A CN202010934196 A CN 202010934196A CN 112062363 B CN112062363 B CN 112062363B
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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
- 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
- C02F1/46—Treatment of water, waste water, or sewage by electrochemical methods
- C02F1/461—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis
- C02F1/467—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction
- C02F1/4672—Treatment of water, waste water, or sewage by electrochemical methods by electrolysis by electrochemical disinfection; by electrooxydation or by electroreduction by electrooxydation
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
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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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- 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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Abstract
The invention relates to wastewater treatment, in particular to a method for treating phenolic resin industrial wastewater, which comprises the following steps: adding resorcinol residues into a reaction kettle filled with the phenolic resin wastewater, heating and continuously stirring; standing for precipitation, and discharging the bottom resin. Pumping the upper clear water into an iron-carbon tower by using a pump, and adding hydrogen peroxide to perform iron-carbon micro-electrolysis-Fenton oxidation; adjusting the pH value of the wastewater to 6-9 by alkali, and then adding a flocculating agent for flocculation and precipitation to obtain upper clear water. The method avoids the process of repeatedly adjusting the pH, reduces the content of cations such as potassium, sodium and the like in the wastewater, avoids the problem of equipment corrosion caused by chloride ions, and is beneficial to biochemical treatment. The method has the advantages of simple and convenient operation, good treatment effect and low cost, and is beneficial to industrial application.
Description
Technical Field
The invention relates to the treatment of wastewater, in particular to a treatment method of phenolic resin industrial wastewater.
Background
The phenolic resin industrial wastewater contains a large amount of phenol, aldehyde and micromolecular resin, is one of the industrial wastewater which is difficult to treat, and can be discharged after reaching the standard after being treated by multiple steps. The main treatment methods at present comprise delayed condensation, biochemistry and extraction and biochemistry. Patent ZL200710067295 discloses a delayed condensation and biochemical treatment process, wherein phenolic resin wastewater is subjected to three-section control to reduce phenol, aldehyde and COD to a certain value, then alkali is added to remove aldehyde, and finally biochemical treatment is carried out. However, the method needs to consume a large amount of acid and alkali, the pH of the wastewater after three-stage control treatment is below 0.8, a large amount of alkali needs to be added to adjust the pH to 10-12, the cost of raw materials is high, and formaldehyde is only converted into other substances for removing aldehyde, so that the COD cannot be reduced. The patent ZL200810000677 extracts phenol by a sulfuric acid acidification method after sodium phenolate distillation, but formaldehyde cannot be taken out, the concentration of the formaldehyde in the treated wastewater is still thousands to tens of thousands ppm, and biochemical treatment is difficult to carry out. The iron-carbon micro-electrolysis-Fenton oxidation is carried out by iron-carbon electrolysis and H under acidic conditions 2 O 2 The method for treating waste water by oxidation has obvious effect and low cost, but has the operation of repeatedly regulating pH, firstly, the pH is regulated to be acidic by using hydrochloric acid or sulfuric acid, then the waste water is regulated to be alkaline by using sodium hydroxide or potassium hydroxide, etc., the process is complicated, the cost is increased, and simultaneously, a large amount of cations or chloride ions are introduced into the waste water, so that the biochemical treatment effect is reduced, and the biochemical fluctuation is possibly caused. The resorcinol residue is residue left after resorcinol purification in the resorcinol production process, is mainly treated according to solid waste at present, has high treatment cost, mainly comprises resorcinol, hydroquinone, biphenol, hydroxyl phenoxy phenol and the like, and is heavier and heavier with the environment of peopleDue to the continuous consumption of resources, the rational disposal of these solid wastes is a major concern.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: provides a method for treating the phenolic resin industrial wastewater, which has the advantages of simple and convenient operation, reliable operation, less control conditions and low cost.
In order to solve the technical problems, the invention adopts the technical scheme that:
the method for treating the phenolic resin industrial wastewater comprises the following steps:
1) Adding resorcinol residues into a reaction kettle filled with the phenolic resin wastewater, heating and continuously stirring;
2) Standing for precipitation, and discharging the bottom resin.
3) Pumping the upper layer clear water into an iron-carbon tower by a pump, adding hydrogen peroxide, and performing iron-carbon micro-electrolysis-Fenton oxidation;
4) Adjusting the pH value of the wastewater to 6-9 by using alkali, and then adding a flocculating agent for flocculation and precipitation to obtain upper clear water;
the invention has the beneficial effects that: the invention does not need to add alkali to adjust the pH value of the wastewater with high aldehyde content, adopts the resorcinol residues to remove formaldehyde, and then directly carries out iron-carbon micro-electrolysis-Fenton oxidation, thereby avoiding the process of repeatedly adjusting the pH value, reducing the content of cations such as potassium, sodium and the like in the wastewater, avoiding the equipment corrosion problem caused by chloride ions and being beneficial to biochemical treatment. The industrial solid waste resorcinol residues are adopted to remove formaldehyde in the wastewater, so that the resorcinol residues are effectively utilized, the formaldehyde is recovered, the removal rate of the formaldehyde reaches more than 92 percent, the COD in the wastewater is reduced, and the precipitated resin can be further recycled. The method has the advantages of simple and convenient operation, good treatment effect and low cost, and is beneficial to industrial application.
Detailed Description
In order to explain the technical content, the objects and the effects of the present invention in detail, the following description will be given with reference to the embodiments.
The method for treating the phenolic resin industrial wastewater comprises the following steps:
1) Adding resorcinol residues into a reaction kettle filled with the phenolic resin wastewater, heating and continuously stirring;
2) Standing and precipitating, and discharging bottom resin;
3) Pumping the upper clear water into an iron-carbon tower by using a pump, and adding hydrogen peroxide to perform iron-carbon micro-electrolysis-Fenton oxidation;
4) Adjusting the pH value of the wastewater to 6-9 by alkali, and then adding a flocculating agent for flocculation and precipitation to obtain upper clear water;
the method utilizes industrial waste resorcinol residues to remove high-concentration formaldehyde in phenolic resin acidic industrial wastewater, and then carries out iron-carbon micro-electrolysis-Fenton oxidation. Utilizing the acidic condition of the wastewater, generating small molecular resin by resorcinol residues and formaldehyde in the wastewater, discharging from the bottom after precipitation, further performing iron-carbon micro-electrolysis and Fenton oxidation on acidic upper clear water, and performing biochemical treatment after flocculation precipitation. The resorcinol residues can not only remove formaldehyde, but also recover resin, thereby realizing reasonable utilization of resources. The operation flow is reduced, and the production cost is reduced. The repeated acid-base blending process is reduced, so that the content of cations in the wastewater can be effectively reduced, the salinity in the wastewater is reduced, the pH value in the aerobic process is reduced, and the aerobic efficiency is improved. The anion content is reduced, and particularly the corrosion problem caused by chloride ions is avoided.
The method for treating the phenolic resin industrial wastewater comprises the steps of firstly reacting phenolic resin acidic wastewater with resorcinol residues under a heating condition, standing and precipitating, then discharging bottom resin, carrying out iron-carbon micro-electrolysis-Fenton oxidation reaction on acidic upper clear water and hydrogen peroxide in an iron-carbon tower, finally adding alkali to adjust the pH value, then adding a flocculating agent, and carrying out flocculation and precipitation to obtain upper clear water, wherein the method is suitable for next biochemical treatment.
The invention adopts resorcinol residue solid waste to carry out aldehyde removal treatment on the phenolic resin industrial wastewater after secondary condensation, removes formaldehyde in the wastewater, and recovers precipitated resin, thereby not only reducing the formaldehyde content, but also reducing the COD content. The resorcinol residue is used as waste residue generated in the resorcinol production process, and contains resorcinol, hydroquinone, biphenol, phenol (hydroxyphenoxy), and the like. The substances have good reactivity with formaldehyde, and are important bases for selecting the formaldehyde removing agent.
According to the invention, the pH of the waste water with high aldehyde content is not adjusted by adding alkali, the resorcinol residues are residues left after resorcinol purification, formaldehyde is removed by the resorcinol residues, and then iron-carbon micro-electrolysis-Fenton oxidation is directly carried out, so that the process of repeatedly adjusting the pH is avoided, the content of cations such as potassium and sodium in the waste water is reduced, the problem of equipment corrosion caused by chloride ions is also avoided, and the biochemical treatment is facilitated. The industrial solid waste resorcinol residues are adopted to remove formaldehyde in the wastewater, so that the resorcinol residues are effectively utilized, the formaldehyde is recovered, the removal rate of the formaldehyde reaches more than 92 percent, the COD in the wastewater is reduced, and the precipitated resin can be further recycled. The method has the advantages of simple and convenient operation, good treatment effect and low cost, and is beneficial to industrial application.
Further, the control indexes of the upper clear water in the step 3) are that the phenol content is less than or equal to 600ppm, the aldehyde content is less than or equal to 50ppm, the COD is less than or equal to 15000ppm, and the pH is 0.6-2.5. The wastewater after aldehyde removal is still strong in acidity and can be directly subjected to iron-carbon micro-electrolysis-Fenton oxidation. The clear water is pumped into the iron-carbon tower by a pump, and the hydrogen peroxide are added in a mode that a water inlet pipeline is added before the clear water enters the iron-carbon tower and then enters the iron-carbon tower together with the wastewater, or the clear water and the wastewater can be added at the bottom of the iron-carbon tower, preferably the mode of adding the clear water into the water inlet pipeline. The dosage of the hydrogen peroxide is 0.5-3 per mill of the mass of the water. The invention carries out iron-carbon micro-electrolysis and Fenton oxidation in the same tower, reduces the process and equipment and has simple and convenient operation.
Further, the effluent of the iron-carbon tower is strongly acidic, and needs to be subjected to pH adjustment by adopting alkali, wherein the alkali is one of sodium hydroxide, potassium hydroxide, calcium hydroxide, sodium carbonate and sodium bicarbonate.
Furthermore, the wastewater after pH adjustment contains suspended matters, and a flocculating agent is added for flocculation and sedimentation, wherein the flocculating agent is one or the combination of two of polyaluminium chloride, polyaluminium sulfate and polyacrylamide, preferably the combination of polyacrylamide and polyaluminium chloride is used, and further preferably the polyacrylamide is used.
Furthermore, the phenol content of the clear water at the upper layer after the flocculation precipitation is less than or equal to 400ppm, the aldehyde content is less than or equal to 40ppm, the COD is less than or equal to 10000ppm, the pH value is 6-9, and the biochemical treatment can be directly carried out. The pH is not too low, and is preferably 6.5 to 8, and the pH exceeding the range is not favorable for flocculation and precipitation and also influences biochemistry.
Furthermore, the phenol content of the phenolic resin industrial wastewater obtained after pretreatment is 100-1000 ppm, the aldehyde content is 2000-8000 ppm, the COD is 6000-20000ppm, and the pH is 0.5-2.0.
In the process of producing phenolic resin, the phenolic resin industrial wastewater generated in the dehydration process has about 50000ppm of phenol, about 10000ppm of formaldehyde and about 200000ppm of COD, and is generally pretreated by a method of adding formaldehyde and an acid catalyst for secondary condensation. The content of formaldehyde in the pretreated wastewater is still more than thousands of ppm, and biochemical treatment cannot be directly carried out, the common treatment method is alkali treatment, usually sodium hydroxide is added for neutralization and aldehyde removal, formaldehyde is converted into other substances, the biological toxicity of the formaldehyde is reduced, but COD is basically unchanged.
Example 1
150kg of resorcinol residues are added into a reaction kettle filled with 10t of phenolic resin industrial wastewater (the phenol content is 322ppm, the formaldehyde content is 6545ppm, the COD is 17854ppm, and the pH value is 1.45), stirring paddles of the reaction kettle are started, the reaction kettle is heated by steam, the temperature in the reaction kettle reaches 85-100 ℃, the stirring reaction is carried out for 1 hour, and then the mixture is kept stand and precipitated. The low molecular weight resin begins to form and precipitate at the bottom of the reaction kettle, and the resin formed by the reaction is discharged from the bottom of the reaction kettle and recycled for secondary use. The phenol content of the waste water after removing the aldehyde from the resorcinol residue is 236ppm, the formaldehyde content is 42ppm, the COD is 13546ppm, and the pH is 1.4. Pumping the wastewater into an iron-carbon tower by a pump, adding hydrogen peroxide into a pipeline entering the iron-carbon tower according to the flow, and carrying out iron-carbon micro-electrolysis-Fenton oxidation reaction, wherein the use amount of the hydrogen peroxide is 0.6 per mill of the mass of water. After the wastewater flows out of the iron carbon tower, sodium hydroxide is added to adjust the pH value of the wastewater to 7.2, then polyacrylamide is added, and the wastewater flows to a sedimentation tank for sedimentation. The content of phenol in the supernatant after precipitation is 161ppm, the content of formaldehyde is 35ppm, the COD is 9868ppm, and the pH is 7.3.
Example 2
100kg of resorcinol residues are added into a reaction kettle filled with 10t of phenolic resin industrial wastewater (the phenol content is 126ppm, the formaldehyde content is 5466ppm, the COD is 15521ppm, and the pH is 1.35), a stirring paddle of the reaction kettle is started, steam is adopted to heat the reaction kettle, the temperature in the reaction kettle reaches 85-100 ℃, the reaction kettle is stirred for 1 hour, and then standing and precipitation are carried out. The low molecular weight resin begins to form and precipitate at the bottom of the reaction kettle, and the resin formed by the reaction is discharged from the bottom of the reaction kettle and recycled for secondary use. After the resorcinol residue was removed of aldehyde, the phenol content of the wastewater was 106ppm, the formaldehyde content was 38ppm, the COD was 11010ppm, and the pH was 1.32. Pumping the wastewater into an iron-carbon tower by a pump, adding hydrogen peroxide into a pipeline entering the iron-carbon tower according to the flow, and carrying out iron-carbon micro-electrolysis-Fenton oxidation reaction, wherein the use amount of the hydrogen peroxide is 0.6 per mill of the mass of water. After the wastewater flows out of the iron carbon tower, sodium hydroxide is added to adjust the pH value of the wastewater to 7.2, then polyacrylamide is added, and the wastewater flows to a sedimentation tank for sedimentation. The clear water on the upper layer after precipitation has the phenol content of 91ppm, the formaldehyde content of 35ppm, the COD of 7854ppm and the pH of 7.3.
Example 3
Adding 200kg of resorcinol residues into a reaction kettle filled with 10t of phenolic resin industrial wastewater (the phenol content is 322ppm, the formaldehyde content is 6545ppm, the COD is 17854ppm, and the pH value is 1.45), starting a stirring paddle of the reaction kettle, heating the reaction kettle by adopting steam to ensure that the temperature in the reaction kettle reaches 85-100 ℃, stirring for reaction for 1 hour, and standing for precipitation. The low molecular weight resin begins to form and precipitate at the bottom of the reaction kettle, and the resin formed by the reaction is discharged from the bottom of the reaction kettle and recycled for secondary use. After removing aldehyde from the resorcinol residue, the phenol content of the wastewater was 255ppm, the formaldehyde content was 12ppm, the COD was 13110ppm, and the pH was 1.42. Pumping the wastewater into an iron-carbon tower by a pump, adding hydrogen peroxide into a pipeline entering the iron-carbon tower according to the flow, and carrying out iron-carbon micro-electrolysis-Fenton oxidation reaction, wherein the use amount of the hydrogen peroxide is 0.6 per mill of the mass of water. After the wastewater flows out of the iron carbon tower, sodium hydroxide is added to adjust the pH value of the wastewater to 7.2, then polyacrylamide is added, and the wastewater flows to a sedimentation tank for sedimentation. The clear water on the upper layer after precipitation has the phenol content of 154ppm, the formaldehyde content of 10ppm, the COD content of 9852ppm and the pH value of 7.3.
In conclusion, the method utilizes the industrial waste resorcinol residues to remove high-concentration formaldehyde in the phenolic resin acidic industrial wastewater, and then carries out iron-carbon microelectrolysis-Fenton oxidation. Utilizing the acidic condition of the wastewater, generating small molecular resin by resorcinol residues and formaldehyde in the wastewater, discharging from the bottom after precipitation, further performing iron-carbon micro-electrolysis and Fenton oxidation on acidic upper clear water, and performing biochemical treatment after flocculation precipitation. The resorcinol residues can not only remove formaldehyde, but also recover resin, thereby realizing reasonable utilization of resources. The operation flow is reduced, and the production cost is reduced. The repeated acid-base blending process is reduced, so that the content of cations in the wastewater can be effectively reduced, the salinity in the wastewater is reduced, the pH value in the aerobic process is reduced, and the aerobic efficiency is improved. The anion content is reduced, and particularly the corrosion problem caused by chloride ions is avoided. The industrial solid waste resorcinol residues are adopted to remove formaldehyde in the wastewater, so that the resorcinol residues are effectively utilized, the formaldehyde is recovered, the removal rate of the formaldehyde reaches more than 92 percent, the COD in the wastewater is reduced, and the precipitated resin can be further recycled. The method has the advantages of simple and convenient operation, good treatment effect and low cost, and is beneficial to industrial application.
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all equivalent modifications made by the present invention in the specification or directly or indirectly applied to the related technical field are included in the scope of the present invention.
Claims (5)
1. A treatment method of phenolic resin industrial wastewater is characterized by comprising the following steps:
step 1: adding resorcinol residues into a reaction kettle filled with the phenolic resin wastewater, heating and continuously stirring;
step 2: standing and precipitating, and discharging bottom resin;
and step 3: pumping the upper clear water into an iron-carbon tower by using a pump, and adding hydrogen peroxide to perform iron-carbon micro-electrolysis-Fenton oxidation;
and 4, step 4: adjusting the pH value of the wastewater to 6-9 by using alkali, and then adding a flocculating agent for flocculation and precipitation to obtain upper clear water;
the phenolic resin wastewater has the phenol content of 100-1000 ppm, the formaldehyde content of 2000-8000ppm, the COD (chemical oxygen demand) of 6000-20000ppm and the pH value of 0.5-2.0;
in the step 3, the control indexes of the upper clear water are that the phenol content is less than or equal to 600ppm, the formaldehyde content is less than or equal to 50ppm, the COD is less than or equal to 15000ppm, and the pH is 0.6-2.5.
2. The method for treating the phenolic resin industrial wastewater according to claim 1, wherein the resorcinol residue is a residue remaining after the resorcinol is purified.
3. The method for treating the phenolic resin industrial wastewater as claimed in claim 1, wherein the dosage of the hydrogen peroxide is 0.5-3 per mill of the mass of water.
4. The method for treating phenolic resin industrial wastewater as recited in claim 1, wherein the alkali is one of sodium hydroxide, potassium hydroxide, calcium hydroxide, sodium carbonate or sodium bicarbonate.
5. The method for treating phenolic resin industrial wastewater as claimed in claim 1, wherein the flocculating agent is one or a combination of two of polyaluminium chloride, polyaluminium sulfate and polyacrylamide.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US3655047A (en) * | 1970-11-06 | 1972-04-11 | Corodex Nv | Process for the purification of waste water |
| GB1321625A (en) * | 1969-11-07 | 1973-06-27 | Corodex Nv | Process and apparatus for the purification of waste water |
| CN1927731A (en) * | 2006-09-27 | 2007-03-14 | 蓝星化工新材料股份有限公司无锡树脂厂 | Method of circulation utilizing phenol containing waste water in novolac epoxy preparing process |
| CN103496828A (en) * | 2013-10-18 | 2014-01-08 | 红板（江西）有限公司 | Printed circuit board high-concentration organic wastewater and acidic wastewater treating process |
| CN109111014A (en) * | 2017-06-26 | 2019-01-01 | 彤程化学（中国）有限公司 | A kind of resource utilization method of the aldehyde-containing sewage containing phenol |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| GB1321625A (en) * | 1969-11-07 | 1973-06-27 | Corodex Nv | Process and apparatus for the purification of waste water |
| US3655047A (en) * | 1970-11-06 | 1972-04-11 | Corodex Nv | Process for the purification of waste water |
| CN1927731A (en) * | 2006-09-27 | 2007-03-14 | 蓝星化工新材料股份有限公司无锡树脂厂 | Method of circulation utilizing phenol containing waste water in novolac epoxy preparing process |
| CN103496828A (en) * | 2013-10-18 | 2014-01-08 | 红板（江西）有限公司 | Printed circuit board high-concentration organic wastewater and acidic wastewater treating process |
| CN109111014A (en) * | 2017-06-26 | 2019-01-01 | 彤程化学（中国）有限公司 | A kind of resource utilization method of the aldehyde-containing sewage containing phenol |
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