CN102092883A - Method for treating DMP-30 wastewater - Google Patents

Method for treating DMP-30 wastewater Download PDF

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CN102092883A
CN102092883A CN2009102003516A CN200910200351A CN102092883A CN 102092883 A CN102092883 A CN 102092883A CN 2009102003516 A CN2009102003516 A CN 2009102003516A CN 200910200351 A CN200910200351 A CN 200910200351A CN 102092883 A CN102092883 A CN 102092883A
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waste water
wastewater
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CN102092883B (en
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曾勇强
张啸晨
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SHANGHAI SAN'AISI REAGENT CO Ltd
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SHANGHAI SAN'AISI REAGENT CO Ltd
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Abstract

The invention discloses a method for treating DMP-30 (2,4,6-tri[(dimethylamino) methyl] phenol wastewater, which comprises the following steps of: reacting 25 to 35 weight percent of NaOH solution and DMP-30, phenol, formaldehyde and dimethyl amine in the wastewater to reduce chemical oxygen demand (COD) and organic ammonia nitrogen compounds NH3-N in the wastewater, reacting for 5 hours at the temperature of between 70 and 80 DEG C under normal pressure, performing reclamation to obtain aqueous solution of dimethyl amine, filtering the reaction solution to obtain white sediment, dissolving the white sediment by using hydrochloric acid solution, performing separation to obtain a DMP-30 product, neutralizing the filtrate by using the hydrochloric acid solution, stirring the solution for 1 hour, and finishing the reaction. The method has low cost, simple operation and good effect, and accords with the environmentally-friendly requirement; and the removal rate of the COD is 90 percent, the removal rate of the NH3-N is 97.8 percent, and the treated wastewater can reach national secondary sewage discharge standards after biological treatment.

Description

A kind of DMP-30 wastewater treatment method
Technical field
The present invention relates to a kind of method of wastewater treatment, relate to a kind of DMP-30 wastewater treatment method or rather.
Background technology
Mainly containing DMP-30 in DMP-30 (2,4,6-three [(dimethylamino) methyl] phenol) waste water is impurity such as 24~27 weight %, phenol 4~6 weight %, dimethylamine 16~18 weight % and formaldehyde 8~11 weight %.
Phenol is a kind of colourless, poisonous, mordant crystal, is slightly soluble in water under the normal temperature, is soluble in organic solvent.
Formaldehyde is a kind of colourless, and the gas of strong impulse smell is arranged, boiling point-19.5 ℃.
DMP-30 is a kind of stiff yellow liquid, easily is dissolved in alcohol, benzene, acetone and the cold water, is slightly soluble in hot water.
Dimethylamine is a kind of colourless gas that irritating smell is arranged, and soluble in water, ethanol, ether, boiling point are 6.9 ℃.
Conventional treatment method ([1] Feng Yibiao " selection of high ammonia-nitrogen wastewater treatment technology method " China Academic Journal Electronic Publishing 2009.6 (30) about high ammonia-nitrogen wastewater; [2] be in ammonia nitrogen waste water, to add the double salt magnesium ammonium phosphate (MgNH that magnesium salts and phosphoric acid salt and ammonia nitrogen generate indissoluble Wang Huifang " research of ammonia nitrogen removal in chemical precipitation method denitrification process condition and the methylamine waste water " " contemporary chemical industry " 2008.6) 4PO 46H 2O), by gravitational settling magnesium ammonium phosphate is separated from waste water then, reached the purpose of removing ammonia nitrogen in the waste water.Yet this method is unsatisfactory to the effect of handling the organic ammonia nitrogen compound, and can't dispose materials such as phenol, formaldehyde simultaneously.
Summary of the invention
The present inventor has found a kind of with low cost, simple to operate, respond well and DMP-30 wastewater treatment method compliance with environmental protection requirements finally through after constantly exploring and testing.
The present invention realizes like this, at first DMP-30 waste water is added in the container, and connection gas receiving trap, this device is built-in with water, with water as gas absorbent, the NaOH solution that in waste water, adds 25~35 weight % concentration subsequently, be warmed to 70~80 ℃ under the normal pressure, impurity in the waste water was with NaOH reaction 5 hours, obtain the dimethylamine agueous solution that reclaims after the reaction, reaction solution obtains white depositions after filtration, white depositions with the dissolving with hydrochloric acid of 30 weight % after Separation and Recovery obtains solid DMP-30; Filtrate neutralizes with the hydrochloric acid of 30 weight %, under agitation reacts 1 hour, and reaction finishes.The DMP-30 waste water of the above-mentioned processing of process after biological treatment, can reach national B-grade sewage emission standard again.
Among the present invention, the volume ratio of DMP-30 waste water and 25~30 weight %NaOH solution is 2: 1~1.5.
Among the present invention, the quality of the white depositions of reaction gained is 1/6~1/5 of a used wastewater quality; The rate of recovery of DMP-30 is 5~6% of a used waste water weight.
Among the present invention, make the absorption agent of water as dimethylamine gas, specific absorption (in 40% dimethylamine agueous solution) is 10% of a used wastewater volume.
Chemical equation main among the present invention is as follows:
Figure G2009102003516D00021
CH 3-NH-CH 3+H 2O→CH 3-NH-CH 3·H 2O
2HCHO+NaOH→HCOONa+CH 3OH
C 6H 5OH+NaOH→C 6H 5ONa+H 2O
Figure G2009102003516D00031
Advantage of the present invention is simple to operate, with low cost, respond well, the COD clearance 90% in the DMP-30 waste water, NH 3-N clearance reaches 97.8%.
Embodiment
For the present invention is described better, as follows especially exemplified by embodiment, but the present invention is not subjected to the restriction of embodiment.
The content of impurity is that DMP-30 is 24~27 weight % in the DMP-30 waste water in following examples, phenol 4~6 weight %, dimethylamine 16~18 weight % and formaldehyde 8~11 weight %.
Embodiment 1: add 200ml DMP-30 waste water and 100ml 35 weight %NaOH solution in there-necked flask, and connect gas absorbing device, water absorbs evolving gas.Under the temperature of normal pressure and 70~80 ℃, reacted the dimethylamine agueous solution that obtains reclaiming (in 40 weight %) 18ml 5 hours.Obtain white precipitate after the filtration, weight of precipitate is 35 grams.Behind throw out usefulness 10ml 30 weight % dissolving with hydrochloric acid,, reclaim and obtain DMP-30 product 10g through separating.Hydrochloric acid soln with 30 weight % under filtrate is stirred neutralizes, and exhausts 50ml30 weight % hydrochloric acid soln altogether.Stir after 1 hour, reaction finishes.
Before the reaction: COD 98600mg/L NH 3-N 464.5mg/L
Reaction back: COD 10200mg/L NH 3-N 9.86mg/L
Clearance: COD 89.6% NH 3-N 97.8%.
Embodiment 2: add 200ml DMP-30 waste water and 120ml 35 weight %NaOH solution in there-necked flask, and connect gas absorbing device, water absorbs evolving gas.Under the temperature of normal pressure and 70~80 ℃, reacted the dimethylamine agueous solution that obtains reclaiming (in 40 weight %) 20ml 5 hours.Obtain white precipitate after the filtration, weight of precipitate is 36.2 grams.Behind throw out usefulness 10ml 30 weight % dissolving with hydrochloric acid,, reclaim and obtain DMP-30 product 10g through separating.Hydrochloric acid soln with 30 weight % under filtrate is stirred advances neutralization, exhausts 60ml30 weight % hydrochloric acid soln altogether.Stir after 1 hour, reaction finishes.
Before the reaction: COD 98600mg/L NH 3-N 464.5mg/L
Reaction back: COD 9930mg/L NH 3-N 7.93mg/L
Clearance: COD 89.6% NH 3-N 98.2%.
Embodiment 3: add 200ml DMP-30 waste water and 150ml 35 weight %NaOH solution in there-necked flask, and connect gas absorbing device, water absorbs evolving gas.Under the temperature of normal pressure and 70~80 ℃, reacted the dimethylamine agueous solution that obtains reclaiming (in 40 weight %) 21ml 5 hours.Obtain white precipitate after the filtration, weight of precipitate is 36.7 grams.Behind throw out usefulness 10ml 30 weight % dissolve with hydrochloric acid solution,, reclaim and obtain DMP-30 product 10g through separating.Hydrochloric acid soln with 30 weight % under filtrate is stirred neutralizes, and exhausts 80ml 30 weight % hydrochloric acid solns altogether.Stir after 1 hour, reaction finishes.
Before the reaction: COD 98600mg/L NH 3-N 464.5mg/L
Reaction back: COD 9720mg/L NH 3-N 6.18mg/L
Clearance: COD 90.1% NH 3-N 98.9%.

Claims (5)

1. DMP-30 wastewater treatment method, it is characterized in that: the content of impurity is that DMP-30 is 24~27 weight % in the DMP-30 waste water, phenol 4~6 weight %, dimethylamine 16~18 weight % and formaldehyde 8~11 weight %, this method is reacted COD and the organic ammonia nitrogen compound N H that reduces in the DMP-30 waste water with NaOH solution and the impurity in the DMP-30 waste water of 25~35 weight % 3The content of-N is reflected under normal pressure, 70~80 ℃ the temperature and carried out 5 hours, and water absorbs evolving gas, reclaims to obtain dimethylamine agueous solution; Reaction solution obtains white depositions after filtration, behind the dissolving with hydrochloric acid of white depositions with 30 weight %, obtains the DMP-30 product through Separation and Recovery; During filtrate is under agitation carried out with 30 weight % hydrochloric acid and after 1 hour, reaction finishes; The waste water of handling through aforesaid method can reach national B-grade sewage emission standard again after biological treatment; Described DMP-30 is 2,4,6-three [(dimethylamino) methyl] phenol.
2. a kind of DMP-30 wastewater treatment method according to claim 1 is characterized in that: the volume ratio of DMP-30 waste water and 25~35 weight %NaOH solution is 2: 1.0~1.5.
3. a kind of DMP-30 wastewater treatment method according to claim 1 is characterized in that: in the described method, the consumption by volume that is used for neutral 30 weight % hydrochloric acid is 1/2 of 25~35 weight %NaOH liquor capacities.
4. a kind of DMP-30 wastewater treatment method according to claim 1 is characterized in that: the rate of recovery of DMP-30 is 5~6% of a used waste water weight.
5. a kind of DMP-30 wastewater treatment method according to claim 1, when it is characterized in that the impurity reaction in 25~35 weight %NaOH solution and the DMP-30 waste water, water is as the absorption agent of dimethylamine gas, and specific absorption is counted 10% of wastewater volume with 40 weight % dimethylamine agueous solutions.
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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106008236A (en) * 2016-05-19 2016-10-12 岳阳中展科技有限公司 Preparation method of colorless DMP-30

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SU685634A1 (en) * 1976-04-14 1979-09-15 Уральский лесотехнический институт Method of porifying waste water in phenolformaldehyde resin production
US6113790A (en) * 1998-12-18 2000-09-05 Basf Corporation Process for removing water-soluble organics from waste streams
CN100488898C (en) * 2007-03-01 2009-05-20 江苏省环境科学研究院 Combined technique for fluorobenzene production waste water treatment

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106008236A (en) * 2016-05-19 2016-10-12 岳阳中展科技有限公司 Preparation method of colorless DMP-30

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