CN1371871A - Phenolic resin sewage treatment method - Google Patents
Phenolic resin sewage treatment method Download PDFInfo
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- CN1371871A CN1371871A CN 01133493 CN01133493A CN1371871A CN 1371871 A CN1371871 A CN 1371871A CN 01133493 CN01133493 CN 01133493 CN 01133493 A CN01133493 A CN 01133493A CN 1371871 A CN1371871 A CN 1371871A
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- raffinate
- phenolic resin
- sewage
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Abstract
The method for treating sewage product from production of phenolic resin includes the procedures of alkaline salt-forming reaction, vacu9um evaporation concentration, decomposition reaction and evaporatino crystallization. In the sewage the alkali is added until the pH value of sewage is 11-12, the they are stirred at normal temp., the sodium phenolate salt aqueous solution can be obtained, under the conditions of that its vacuum is 0.01-0.015 Mpa, and heated steam pressure is 0.15-0.3 Mpa the above-mentioned solution is concentrated, and its phenol content is 25-30%, then the dilute acid is added in the concentrate until its pH value is 1-3, reacted and stood still, the phenol and residue can be separated and recovered, the residue can be naturally evaporated, and the sodium sulfate can be separated, crystallized and recovered.
Description
Technical field
The present invention relates to a kind of sewage water treatment method, especially the treatment process of resol sewage.
Background technology
Resol is polymerized under certain condition by phenol and formaldehyde, and it is widely used in bakelite synthetic materials, impregnating material, wedding agent and paint etc.The sewage quantity of producing the resol generation is about 0.4T/
The T product, containing the phenol amount in the sewage is 8000～70000mg/
L sewage, above the 0.5mg/ of discharging standards defined
L sewageReach up to ten thousand times.There are nearly thousand families in the producer whole nation that produces resol, so how effectively, handling resol sewage economically is present problem demanding prompt solution.
To polluting so serious resol sewage, existing treatment technology mainly contains following several: one of null method is biochemical decomposition method, must can carry out biochemical treatment to the dilution of sewage hundreds of times earlier, and investment is big, per diem handles 3M
3Sewage calculates, and needs 600,000 yuan of investments, and one ton of sewage of average treatment needs 300 yuan of expenses, and the production cost height is also wasted a large amount of water resourcess simultaneously, and this is unallowed in China's national situation institute.Two of null method is chemical oxidization method (with potassium permanganate or ozone oxidation), its cost height, and the technical requirements height is difficult to promote.Phenol resource recycling method is example with the organic solvent extractionprocess, adopts coal tar distillate to make extraction agent, and percentage extraction is low, the highest less than 90%, processed waste water contains the phenol amount and exceeds standard and still reach thousands of times, also need carry out biological dephenolize and handle, complex technical process, cost height, treatment effect are also undesirable.
Summary of the invention
In view of the problems referred to above that exist, the objective of the invention is to seek that a kind of technology is reliable, technology simple, processing ease, cost are low, less investment, treatment effect is good, economic benefit is high, free from environmental pollution phenolic resin sewage treatment method.
For realizing purpose of the present invention, the technical measures of taking are a kind of phenolic resin sewage treatment methods of design, it is characterized in that it is by 1) add alkali salt-forming reaction, 2) vacuum-evaporation concentrates, 3) decomposition reaction, 4) the evaporative crystallization operation forms;
1) till adding solid alkali sodium hydroxide to the pH value of reacting back sewage is 11～12 in the resol sewage of 1 li of main reaction still, stirs generation sodium phenylate salt brine solution at normal temperatures;
2) be that the pressure of heating steam in 0.01～0.015Mpa, main reaction still 1 chuck is under the condition of 0.15～0.3Mpa in the vacuum tightness of main reaction still 1, Pyrogentisinic Acid's sodium-salt aqueous solution carries out vacuum-evaporation and is concentrated into that to contain the phenol amount in the concentrated solution be 25～30% (weight percentage);
3) adding concentration in main reaction still 1 in concentrated solution is that dilute sulphuric acid to the pH value of concentrated solution of 28～32% (weight percentage) is till 1～3, leaves standstill 2 hours after reacting again, and makes it layering, and the upper strata is a phenol, and lower floor is a raffinate;
4) in crystallizer tank 6, made the raffinate spontaneous evaporation 5～6 days, separate out sulfate crystal, the residue raffinate turns back in the former water basin 2 to be handled again.
The described churning time that adds in the alkali salt-forming reaction operation is 20～30 minutes, and stirring velocity is 70～90 rev/mins.
After described vacuum-evaporation enrichment process carries out a week, make concentrated solution collect 3M
3The time, send into main reaction still 1, concentrate the disaggregating treatment of carrying out next operation in a day.
Reaction times in the described decomposition reaction operation is 25～30 minutes.
In the described evaporative crystallization operation, in raffinate, add solid alkali sodium hydroxide to the pH value of raffinate and be till 10～12.
The present invention compares with existing treatment technology owing to take as above technical measures processing resol sewage, and its technology is reliable, and technology is simple, processing ease; Cost is low, less investment; Treatment effect is good, the economic benefit height; And realized zero release, free from environmental pollution.
Description of drawings
Accompanying drawing is the process flow sheet of phenolic resin sewage treatment method of the present invention.
Embodiment
Introduce technical characterictic of the present invention and principle of operation and process in detail below in conjunction with drawings and Examples.
In the accompanying drawing, 1 main reaction still, 2 former water basins, 3 concentrate flow container, 4 phenol basins, 5 condensation water pots, 6 crystallizer tanks, 7 condensers, 8 water of condensation grooves, 9 phenol scale tanks, 10 sour basins
As shown in drawings, resol sewage is incorporated into the main reaction still 1 from former water basin 2, add solid alkali sodium hydroxide to the pH value of reaction back sewage again and be till 11～12, at normal temperatures, stirred 20～30 minutes with 70～90 rev/mins speed, make phenol and sodium hydroxide reaction in the resol sewage generate the sodium phenylate salt brine solution.In the vacuum tightness of main reaction still 1 be in 0.01～0.015Mpa, main reaction still 1 chuck heating steam to press be under the condition of 0.15～0.3Mpa, Pyrogentisinic Acid's sodium-salt aqueous solution carries out vacuum-evaporation and is concentrated into that to contain the phenol amount in the concentrated solution be 25～30% (weight percentage).The water that steams enters condensate receiver 8 after condenser 7 condensations, send into condensation water tank 5 again, is used for batching at last and turns back to cooling water system recycling.Concentrated solution is delivered in the concentrated solution basin 3 and to be stored, so handle a week after, concentrated solution to be collected reaches 3M
3, deliver in the main reaction still 1 (or the acid corrosion-resistant splitter that sets up), concentrate the disaggregating treatment of carrying out next operation in a day.To come out from sour basin 10, through the concentration of sour scale tank 9 meterings be the dilute sulphuric acid of 28～32% (weight percentage) add the concentrated solution be 1～3 to the pH value of concentrated solution till, reaction times is 25～35 minutes, generate phenol and sodium sulfate salt solution (raffinate), leave standstill again and made it layering in 2 hours, the isolated phenol in upper strata is sent into phenol storage 4 and is reclaimed, and the isolated raffinate of lower floor is sent into crystallizer tank 6.In crystallizer tank 6, to adding in the raffinate till the pH value of solid alkali sodium hydroxide to raffinate be 10～12, make the reaction of phenol residual in the raffinate and sodium hydroxide generate nonvolatile phenol sodium salt, avoided the loss that causes because of the phenol volatilization like this and the pollution of air.Raffinate is separated out sulfate crystal through the spontaneous evaporation of 5～6 day time, it is pulled out again utilize, and the residue raffinate returns former water basin 2 and handles, has realized zero release, and is free from environmental pollution.
Containing the phenol amount in the resol sewage of handling is 30000mg/L sewage, and processing power is 3M
3/ d.
In main reaction still 1, call in 3M
3Resol sewage adds solid alkali sodium hydroxide to reaction back sewage pH value again and is till 11～12, stirs 30 minutes generation sodium phenylate salts solution at normal temperatures with 80 rev/mins of speed.In the vacuum tightness of main reaction still 1 is that the pressure of heating steam in 0.01Mpa, main reaction still 1 chuck is under the condition of 0.2Mpa, Pyrogentisinic Acid's sodium-salt aqueous solution carries out vacuum-evaporation and is concentrated into concentrated solution to contain the phenol amount be 25～30% (weight percentage), after so handling a week, make concentrated solution collect 3M
3Send into main reaction still 1, concentrate the disaggregating treatment of carrying out next operation in a day.1 li of main reaction still, the dilute sulphuric acid that adds concentration and be 30% (weight percentage) in concentrated solution to the pH value of concentrated solution are 2 to end, and reacts 30 minutes, and the generation phenol and the sodium sulfate salt aqueous solution (raffinate) make it layering, and the upper strata is a phenol, and lower floor is a raffinate.In crystallizer tank 6, in raffinate, add solid alkali sodium hydroxide to the pH value of raffinate and be 12 and end, made the raffinate spontaneous evaporation again 5～6 days, separate out sulfate crystal and utilize again, remain raffinate and turn back to former water basin 2 and handle again, realized zero release.
Experimental data according to present embodiment is calculated, and handles 3M every day
3Sewage, total treatment capacity was 750M with calculating in 250 days in 1 year
3, total cost of production is 9.35 ten thousand yuan, and recyclable 22.5 tons of phenol in 6200 yuan of phenol per ton, can be made profits 13.95 ten thousand yuan, and net profit is 4.6 ten thousand yuan, does not comprise the value that environmental fines and sulfate crystal are recycled.
Claims (5)
1, a kind of phenolic resin sewage treatment method is characterized in that it is by 1) add alkali salt-forming reaction, 2) vacuum-evaporation concentrates, 3) decomposition reaction, 4) the evaporative crystallization operation forms;
1) till adding solid alkali sodium hydroxide to the pH value of reacting back sewage is 11～12 in the resol sewage of main reaction still (1) lining, stirs generation sodium phenylate salt brine solution at normal temperatures;
2) be that the pressure of heating steam in 0.01～0.015Mpa, main reaction still (1) chuck is under the condition of 0.15～0.3Mpa in the vacuum tightness of main reaction still (1), Pyrogentisinic Acid's sodium-salt aqueous solution carries out vacuum-evaporation and is concentrated into that to contain the phenol amount in the concentrated solution be 25～30% (weight percentage);
3) in main reaction still (1), the dilute sulphuric acid that adds concentration and be 28～32% (weight percentage) in concentrated solution to the pH value of concentrated solution is till 1～3, leaves standstill 2 hours after reacting again, and makes it layering, and the upper strata is a phenol, and lower floor is a raffinate;
4) in crystallizer tank (6), made the raffinate spontaneous evaporation 5～6 days, separate out sulfate crystal, the residue raffinate turns back in the former water basin (2) to be handled again.
2, phenolic resin sewage treatment method according to claim 1 is characterized in that 1) churning time that adds in the alkali salify operation is 20～30 minutes, stirring velocity is 70～90 rev/mins.
3, phenolic resin sewage treatment method according to claim 1 is characterized in that 2) after the vacuum-evaporation enrichment process carries out a week, make concentrated solution collect 3M
3Send into main reaction still (1) again, concentrate the disaggregating treatment of carrying out next operation in a day.
4, phenolic resin sewage treatment method according to claim 1 is characterized in that 3) reaction times in the decomposition reaction operation is 25～35 minutes.
5, phenolic resin sewage treatment method according to claim 1 is characterized in that 4) in the evaporative crystallization operation, in raffinate, add solid alkali sodium hydroxide to the pH value of raffinate and be till 10～12.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011334932A CN1164505C (en) | 2001-11-26 | 2001-11-26 | Phenolic resin sewage treatment method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB011334932A CN1164505C (en) | 2001-11-26 | 2001-11-26 | Phenolic resin sewage treatment method |
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| Publication Number | Publication Date |
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| CN1371871A true CN1371871A (en) | 2002-10-02 |
| CN1164505C CN1164505C (en) | 2004-09-01 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB011334932A Expired - Fee Related CN1164505C (en) | 2001-11-26 | 2001-11-26 | Phenolic resin sewage treatment method |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101151217B (en) * | 2005-03-29 | 2011-06-08 | 住友化学株式会社 | Method for treating waste water containing oxygen-containing compound having phenol hydroxy group or carbonyl group |
| CN101481187B (en) * | 2008-01-15 | 2011-07-06 | 山东圣泉化工股份有限公司 | Method for processing phenolic resin phenolic wastewater |
| CN102126777A (en) * | 2011-02-11 | 2011-07-20 | 朱炜权 | Treatment method of phenol sodium salt waste water |
| CN102936075A (en) * | 2012-11-13 | 2013-02-20 | 常州大学 | Method for recycling industrial wastewater generated during alanine production |
| CN103159593A (en) * | 2013-03-18 | 2013-06-19 | 南京师范大学 | Method for preparing phenol sodium salt in aqueous phase |
| CN104998429A (en) * | 2015-08-17 | 2015-10-28 | 山东新华制药股份有限公司 | Dehydration technology and device for salicylic acid intermediate sodium phenoxide |
| CN106430768A (en) * | 2015-08-10 | 2017-02-22 | 彤程化学（中国）有限公司 | Treatment method of phenolic resin phenol and aldehyde wastewater |
-
2001
- 2001-11-26 CN CNB011334932A patent/CN1164505C/en not_active Expired - Fee Related
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101151217B (en) * | 2005-03-29 | 2011-06-08 | 住友化学株式会社 | Method for treating waste water containing oxygen-containing compound having phenol hydroxy group or carbonyl group |
| US8298378B2 (en) | 2005-03-29 | 2012-10-30 | Sumitomo Chemical Company, Limited | Method for treating waste water containing oxygen-containing compound having phenolic hydroxyl group of carbonyl group |
| CN101481187B (en) * | 2008-01-15 | 2011-07-06 | 山东圣泉化工股份有限公司 | Method for processing phenolic resin phenolic wastewater |
| CN102126777A (en) * | 2011-02-11 | 2011-07-20 | 朱炜权 | Treatment method of phenol sodium salt waste water |
| CN102126777B (en) * | 2011-02-11 | 2012-03-21 | 朱炜权 | Treatment method of phenol sodium salt waste water |
| CN102936075A (en) * | 2012-11-13 | 2013-02-20 | 常州大学 | Method for recycling industrial wastewater generated during alanine production |
| CN103159593A (en) * | 2013-03-18 | 2013-06-19 | 南京师范大学 | Method for preparing phenol sodium salt in aqueous phase |
| CN106430768A (en) * | 2015-08-10 | 2017-02-22 | 彤程化学（中国）有限公司 | Treatment method of phenolic resin phenol and aldehyde wastewater |
| CN106430768B (en) * | 2015-08-10 | 2019-07-19 | 彤程化学（中国）有限公司 | A kind of processing method of phenolic resin aldehyde-containing sewage containing phenol |
| CN104998429A (en) * | 2015-08-17 | 2015-10-28 | 山东新华制药股份有限公司 | Dehydration technology and device for salicylic acid intermediate sodium phenoxide |
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| Publication number | Publication date |
|---|---|
| CN1164505C (en) | 2004-09-01 |
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