CN102092883B - Method for treating DMP-30 wastewater - Google Patents
Method for treating DMP-30 wastewater Download PDFInfo
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- CN102092883B CN102092883B CN 200910200351 CN200910200351A CN102092883B CN 102092883 B CN102092883 B CN 102092883B CN 200910200351 CN200910200351 CN 200910200351 CN 200910200351 A CN200910200351 A CN 200910200351A CN 102092883 B CN102092883 B CN 102092883B
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- dmp
- weight
- waste water
- solution
- reaction
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- 239000002351 wastewater Substances 0.000 title claims abstract description 40
- AHDSRXYHVZECER-UHFFFAOYSA-N 2,4,6-tris[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC(CN(C)C)=C(O)C(CN(C)C)=C1 AHDSRXYHVZECER-UHFFFAOYSA-N 0.000 title claims abstract description 39
- 238000000034 method Methods 0.000 title claims abstract description 21
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims abstract description 39
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 32
- ROSDSFDQCJNGOL-UHFFFAOYSA-N Dimethylamine Chemical compound CNC ROSDSFDQCJNGOL-UHFFFAOYSA-N 0.000 claims abstract description 30
- 238000006243 chemical reaction Methods 0.000 claims abstract description 20
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 18
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000000706 filtrate Substances 0.000 claims abstract description 6
- 238000001914 filtration Methods 0.000 claims abstract description 6
- 239000000047 product Substances 0.000 claims abstract description 5
- 238000000926 separation method Methods 0.000 claims abstract description 3
- 239000010865 sewage Substances 0.000 claims abstract description 3
- 239000007789 gas Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- XKMRRTOUMJRJIA-UHFFFAOYSA-N ammonia nh3 Chemical compound N.N XKMRRTOUMJRJIA-UHFFFAOYSA-N 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 6
- 238000000151 deposition Methods 0.000 claims description 5
- 230000008021 deposition Effects 0.000 claims description 5
- 238000010521 absorption reaction Methods 0.000 claims description 4
- 238000011084 recovery Methods 0.000 claims description 4
- NFVPEIKDMMISQO-UHFFFAOYSA-N 4-[(dimethylamino)methyl]phenol Chemical compound CN(C)CC1=CC=C(O)C=C1 NFVPEIKDMMISQO-UHFFFAOYSA-N 0.000 claims description 2
- 238000013019 agitation Methods 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 claims description 2
- 238000006386 neutralization reaction Methods 0.000 claims description 2
- 229910017464 nitrogen compound Inorganic materials 0.000 claims description 2
- 238000003756 stirring Methods 0.000 abstract description 4
- 239000000126 substance Substances 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 239000000243 solution Substances 0.000 abstract 5
- 239000013049 sediment Substances 0.000 abstract 2
- CVTZKFWZDBJAHE-UHFFFAOYSA-N [N].N Chemical class [N].N CVTZKFWZDBJAHE-UHFFFAOYSA-N 0.000 abstract 1
- 239000007864 aqueous solution Substances 0.000 abstract 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 abstract 1
- 230000003472 neutralizing effect Effects 0.000 abstract 1
- 239000001301 oxygen Substances 0.000 abstract 1
- 229910052760 oxygen Inorganic materials 0.000 abstract 1
- 239000002244 precipitate Substances 0.000 description 6
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- 0 CC*C=C(CO)*NC Chemical compound CC*C=C(CO)*NC 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- BAVYZALUXZFZLV-UHFFFAOYSA-N Methylamine Chemical compound NC BAVYZALUXZFZLV-UHFFFAOYSA-N 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 229910052567 struvite Inorganic materials 0.000 description 2
- 238000004065 wastewater treatment Methods 0.000 description 2
- 229910017958 MgNH Inorganic materials 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- MXZRMHIULZDAKC-UHFFFAOYSA-L ammonium magnesium phosphate Chemical compound [NH4+].[Mg+2].[O-]P([O-])([O-])=O MXZRMHIULZDAKC-UHFFFAOYSA-L 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 159000000003 magnesium salts Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 150000003016 phosphoric acids Chemical class 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- -1 salt magnesium ammonium phosphate Chemical class 0.000 description 1
- HLBBKKJFGFRGMU-UHFFFAOYSA-M sodium formate Chemical compound [Na+].[O-]C=O HLBBKKJFGFRGMU-UHFFFAOYSA-M 0.000 description 1
- 235000019254 sodium formate Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
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- Removal Of Specific Substances (AREA)
- Physical Water Treatments (AREA)
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
Technical field
The present invention relates to a kind of method of wastewater treatment, relate to or rather a kind for the treatment of process of DMP-30 waste water.
Background technology
Mainly containing DMP-30 in DMP-30 (2,4,6-three (dimethylamino methyl) phenol) waste water is the impurity such as 24～27 % by weight, phenol 4～6 % by weight, dimethylamine 16～18 % by weight and formaldehyde 8～11 % by 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 yellow liquid of stiff, and is soluble in alcohol, benzene, acetone and 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), then by gravitational settling magnesium ammonium phosphate is separated from waste water, reached the purpose of removing ammonia nitrogen in the waste water.Yet the method is unsatisfactory to the effect of processing the organic ammonia nitrogen compound, and can't dispose simultaneously the materials such as phenol, formaldehyde.
Summary of the invention
The present inventor has found a kind for the treatment of process of DMP-30 waste water with low cost, simple to operate, respond well and that meet environmental requirement 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, with the NaOH solution that adds 25～35 % by weight concentration in the backward waste water, be warmed to 70～80 ℃ under the normal pressure, impurity in the waste water was with NaOH reaction 5 hours, the dimethylamine agueous solution that is recycled after the reaction, reaction solution obtains white depositions after filtration, and white depositions obtains solid DMP-30 with the dissolving with hydrochloric acid of 30 % by weight by Separation and Recovery; Filtrate neutralizes with the hydrochloric acid of 30 % by 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 % by 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 used wastewater quality; The rate of recovery of DMP-30 is 5～6% of used waste water weight.
Among the present invention, make water as the absorption agent of dimethylamine gas, specific absorption (take 40% dimethylamine agueous solution) is 10% of used wastewater volume.
Chemical equation main among the present invention is as follows:
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
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 % by weight in the DMP-30 waste water in following examples, phenol 4～6 % by weight, dimethylamine 16～18 % by weight, and formaldehyde 8～11 % by weight.
Embodiment 1: add 200ml DMP-30 waste water and 100ml 35 % by 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 is recycled (in 40 % by weight) 18ml 5 hours.Obtain white precipitate after the filtration, weight of precipitate is 35 grams.Behind throw out usefulness 10ml 30 % by weight dissolving with hydrochloric acid, through separating, reclaim and obtain DMP-30 product 10g.Filtrate is stirred lower hydrochloric acid soln with 30 % by weight and is neutralized, and exhausts altogether 50ml30 % by weight hydrochloric acid soln.Stir after 1 hour, reaction finishes.
Before the reaction: COD 98600mg/L NH
3-N 464.5mg/L
After the reaction: 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 % by 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 is recycled (in 40 % by weight) 20ml 5 hours.Obtain white precipitate after the filtration, weight of precipitate is 36.2 grams.Behind throw out usefulness 10ml 30 % by weight dissolving with hydrochloric acid, through separating, reclaim and obtain DMP-30 product 10g.Filtrate is stirred lower hydrochloric acid soln with 30 % by weight and is advanced neutralization, exhausts altogether 60ml30 % by weight hydrochloric acid soln.Stir after 1 hour, reaction finishes.
Before the reaction: COD 98600mg/L NH
3-N 464.5mg/L
After the reaction: 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 % by 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 is recycled (in 40 % by weight) 21ml 5 hours.Obtain white precipitate after the filtration, weight of precipitate is 36.7 grams.Behind throw out usefulness 10ml 30 % by weight dissolve with hydrochloric acid solution, through separating, reclaim and obtain DMP-30 product 10g.Filtrate is stirred lower hydrochloric acid soln with 30 % by weight and is neutralized, and exhausts altogether 80ml 30 % by weight hydrochloric acid solns.Stir after 1 hour, reaction finishes.
Before the reaction: COD 98600mg/L NH
3-N 464.5mg/L
After the reaction: COD 9720mg/L NH
3-N 6.18mg/L
Clearance: COD 90.1% NH
3-N 98.9%.
Claims (5)
1. the treatment process of a DMP-30 waste water, it is characterized in that: the content of impurity is that DMP-30 is 24～27 % by weight in the DMP-30 waste water, phenol 4～6 % by weight, dimethylamine 16～18 % by weight and formaldehyde 8～11 % by weight, the method reacts to reduce COD and organic ammonia nitrogen compound N H in the DMP-30 waste water with the NaOH solution of 25～35 % by weight and the impurity in the DMP-30 waste water
3The content of-N, reaction was carried out 5 hours under normal pressure, 70～80 ℃ temperature, and water absorbs and reclaims evolving gas, obtains dimethylamine agueous solution; Reaction solution obtains white depositions after filtration, behind the dissolving with hydrochloric acid of white depositions with 30 % by weight, obtains the DMP-30 product through Separation and Recovery: during filtrate is under agitation carried out with 30 % by weight hydrochloric acid and after 1 hour, reaction finishes; The waste water of processing 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. the treatment process of a kind of DMP-30 waste water according to claim 1, it is characterized in that: the volume ratio of DMP-30 waste water and 25～35 % by weight NaOH solution is 2: 1.0～1.5.
3. the treatment process of a kind of DMP-30 waste water according to claim 1 is characterized in that: in the described method, the consumption that is used for 30 % by weight hydrochloric acid of neutralization is 1/2 of 25～35 % by weight NaOH liquor capacities by volume.
4. the treatment process of a kind of DMP-30 waste water according to claim 1, it is characterized in that: the rate of recovery of DMP-30 is 5～6% of used waste water weight.
5. the treatment process of a kind of DMP-30 waste water according to claim 1, when it is characterized in that the impurity reaction in 25～35 % by 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 % by weight dimethylamine agueous solutions.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910200351 CN102092883B (en) | 2009-12-11 | 2009-12-11 | Method for treating DMP-30 wastewater |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200910200351 CN102092883B (en) | 2009-12-11 | 2009-12-11 | Method for treating DMP-30 wastewater |
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|---|---|
| CN102092883A CN102092883A (en) | 2011-06-15 |
| CN102092883B true CN102092883B (en) | 2013-02-06 |
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|---|---|---|---|
| CN 200910200351 Expired - Fee Related CN102092883B (en) | 2009-12-11 | 2009-12-11 | Method for treating DMP-30 wastewater |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106008236A (en) * | 2016-05-19 | 2016-10-12 | 岳阳中展科技有限公司 | Preparation method of colorless DMP-30 |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101037278A (en) * | 2007-03-01 | 2007-09-19 | 江苏省环境科学研究院 | Combined technique for fluorobenzene production waste water treatment |
-
2009
- 2009-12-11 CN CN 200910200351 patent/CN102092883B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN101037278A (en) * | 2007-03-01 | 2007-09-19 | 江苏省环境科学研究院 | Combined technique for fluorobenzene production waste water treatment |
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| CN102092883A (en) | 2011-06-15 |
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