CN1131576A - Method for treating discharge liquid of hexanolactam preparation technology - Google Patents
Method for treating discharge liquid of hexanolactam preparation technology Download PDFInfo
- Publication number
- CN1131576A CN1131576A CN 95110679 CN95110679A CN1131576A CN 1131576 A CN1131576 A CN 1131576A CN 95110679 CN95110679 CN 95110679 CN 95110679 A CN95110679 A CN 95110679A CN 1131576 A CN1131576 A CN 1131576A
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- CN
- China
- Prior art keywords
- caprolactam
- waste liquid
- comes out
- tower
- benzene
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
A process for treating high-connectration waste liquid generated during production of caprolactam to recover caprolactam, ammonium sulfate and hydroxyhexanoic acid includes mixing, concentration and demixing at 20-25 deg.C for recovering said usefull substances and also preventing environmental pollution. Its liquid phase density is 1.2-1.23 and the ammonium sulfate content in liquid phase is 30-40%.
Description
The present invention relates to a kind of method of handling preparing process of caprolactam moderate liquid.
The waste liquid kind that produces in the preparing process of caprolactam is more, mainly is the high-concentration waste liquid of the unsuitable biochemical treatment that produces from device techniques such as sulphur crystalline ammonium, cyclohexane oxidation, cyclohexanone oximate.For example, Yueyang Ying Shan petrochemical plant is introduced the waste liquid that is produced in 50,000 tons of caprolactam production apparatus technologies just to be had following several: waste liquid 4.10～6.12t/hr that come out from ion exchange tower (1), its composition: Na
+0.9wt%, NO3
-: 1.8wt%, PH=13, organic matter 0.45～2.25wt%; (2) the raffinate 0.0144～0.018t/hr that comes out from the benzene distillation tower, its composition: benzene 48.5%, caprolactam 11.42%, oligomer 40% reaches 120 tons every year; (3) caprolactam raffinate (coming out) from stripper, 3.71～4.32t/hr, its composition: (NH
4)
2SO
42.5%, organic matter (mainly being caprolactam) 2～3%; (4) A.S cleaning fluid, 0.638t/hr, it forms part: (NH
4)
2SO
4: benzene 20PPM 40%,, organic matter (mainly being caprolactam) 2.53%.At present, be that above waste liquid is handled with burning method, with decompression distillation the waste liquid organic matter is concentrated into about 50%, high temperature (more than 1000 ℃) organic matter decomposing oxidation down is transformed into solution salt Na
2SO
4, remove COD, combustion tail gas is sent into scrubbing tower fine particle is dissolved, and waste water enters the sewage-farm, and residual air enters atmosphere.For can be under the situation more than 1000 ℃ with above various waste liquids oxidation Decomposition, to consume 2700 tons of X oil every year, 600 tons of light oils, 400 tons of diesel oil, 30 tons of oil liquefied gas are worth greater than 9,000,000 yuan of coin, this has not only burnt some useful industrial chemicals, and from also uneconomical economically.
Burn above-mentioned waste liquid, in a conventional incinerator, carry out, at first light incinerator, furnace temperature is brought up to 1000 ℃, open each flue, above-mentioned several strands of waste liquids are mixed (PH neutrality) enter evaporimeter, advance living preheating and concentrate (hot-air), organic concentration reaches 10～15%, carries out gas-liquid separation then, send into another evaporimeter with discharge pump, use the 0.5MPa Steam Heating, be concentrated to 50～55%, carry out gas-liquid separation after, deliver to a storage tank and be equipped with burning, ventilate and situation that auxiliary fuel is combustion-supporting under, the concentrating spent liquor with 50～55% sprays into incinerator and burns, hot gas is used as thermal source, preheating evaporation and concentration liquid, waste water enters the sewage-farm.
The objective of the invention is to above-mentioned degree liquid not burnt, fuel savings, and the useful constituent in the waste liquid separated, both having made it turns waste into wealth, and does not cause the environment ring is dyed.
The invention is characterized in 1 part of A.S cleaning fluid (sulfur-bearing ammonium 30～40%) and add the waste liquid that comes out from ion exchange tower and the raffinate that comes out from the benzene distillation tower and concentrate after totally 3 parts of mixing from the raffinate that caprolactam stripping extraction tower comes out; Wait to be concentrated to water sulfur-bearing ammonium 30～40%, when density 1.20～1.23,25～30 ℃ of temperature, concentrate is layering well, contains caprolactam 25～30% in the oil phase, hydroxyl caproic acid 8～12%; Aqueous phase sulfur-bearing ammonium 35～42%.
The present invention has not only saved a large amount of fuel because of the described waste liquid of burning disposal not, and utility in the waste liquid is separated, and becomes useless and is the chamber, to efficent use of resources, prevents that its pollution to environment from all having very high value.
Embodiment 1. gets 100 gram A.S cleaning fluids and (contains (NH
4)
2SO
440%), waste liquid that adds the waste liquid that comes out from ion exchange tower and come out from the benzene distillation tower and the raffinate that comes out from caprolactam stripping extraction tower be totally 300 grams, insert in the 1000ml flask and concentrate, temperature is controlled at 27 ℃, water density is 1.21, and at this moment, oil phase and water layering are better, isolate the sulphur ammonium of aqueous phase 35～40% with conventional method, isolate the caprolactam of 25～30% in the oil phase and 8～12 hydroxycaproic acid.
Claims (4)
1. a method of handling waste liquid in the preparing process of caprolactam process is characterized in that adding the waste liquid that (1) ejects from ion exchange tower for 1 part with the A.S cleaning fluid.(2) raffinate that comes out from the benzene distillation tower.(3) raffinate that comes out from caprolactam stripping extraction tower concentrate after totally 3 parts of mixing, layering, reclaim 25～30% caprolactams and 35～42% sulphur ammoniums and 8～12% hydroxycaproic acids.
2. method according to claim 1 is characterized in that concentrating stratification temperature is 25～30% ℃, water density 1.20～1.23, aqueous phase sulfur-bearing ammonium 30～40%.
3. method according to claim 1 is characterized in that sulfur-bearing ammonium 30～40% in the A.S cleaning fluid.
4. according to the described method of claim, it is characterized in that:
(1) composition of A.S cleaning fluid: (NH
4)
2SO
4: 40%, benzene 20PPM, organic matter (mainly being caprolactam) 2.53%,
(2) waste liquid that ejects from ion exchange tower is formed:
Na
+0.9wt%, NO
31.8wt%PH=13, organic matter 0.45～2.25wt%,
(3) the waste liquid content that comes out from the benzene distillation tower is formed:
Benzene 48.5%, caprolactam 11.42%, oligomer 40%,
(4) waste liquid that comes out from caprolactam stripping extraction tower is formed: (NH
4)
2SO
42.5%, organic matter (mainly being caprolactam) 2～3%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 95110679 CN1131576A (en) | 1995-03-21 | 1995-03-21 | Method for treating discharge liquid of hexanolactam preparation technology |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 95110679 CN1131576A (en) | 1995-03-21 | 1995-03-21 | Method for treating discharge liquid of hexanolactam preparation technology |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1131576A true CN1131576A (en) | 1996-09-25 |
Family
ID=5078038
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 95110679 Pending CN1131576A (en) | 1995-03-21 | 1995-03-21 | Method for treating discharge liquid of hexanolactam preparation technology |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1131576A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1064930C (en) * | 1997-10-23 | 2001-04-25 | 巴陵石油化工公司鹰山石油化工厂 | Method and equipment for recovering sodium carbonate by incineration treatment of caprolactam saponification waste alkali liquor |
| CN102030434B (en) * | 2009-09-30 | 2012-05-30 | 中国石油化工股份有限公司 | Method for pretreating cyclohexanone ammoximation waste water |
| WO2015062189A1 (en) * | 2013-11-01 | 2015-05-07 | 华东理工大学 | Method and apparatus for recovering caprolactam in benzene distillation residue |
| CN111718058A (en) * | 2019-03-20 | 2020-09-29 | 中石化南京化工研究院有限公司 | Treatment method of caprolactam production waste liquid |
| CN112441599A (en) * | 2019-08-29 | 2021-03-05 | 中石化南京化工研究院有限公司 | Treatment method of caprolactam production waste liquid |
-
1995
- 1995-03-21 CN CN 95110679 patent/CN1131576A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1064930C (en) * | 1997-10-23 | 2001-04-25 | 巴陵石油化工公司鹰山石油化工厂 | Method and equipment for recovering sodium carbonate by incineration treatment of caprolactam saponification waste alkali liquor |
| CN102030434B (en) * | 2009-09-30 | 2012-05-30 | 中国石油化工股份有限公司 | Method for pretreating cyclohexanone ammoximation waste water |
| WO2015062189A1 (en) * | 2013-11-01 | 2015-05-07 | 华东理工大学 | Method and apparatus for recovering caprolactam in benzene distillation residue |
| CN111718058A (en) * | 2019-03-20 | 2020-09-29 | 中石化南京化工研究院有限公司 | Treatment method of caprolactam production waste liquid |
| CN112441599A (en) * | 2019-08-29 | 2021-03-05 | 中石化南京化工研究院有限公司 | Treatment method of caprolactam production waste liquid |
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| PB01 | Publication | ||
| C01 | Deemed withdrawal of patent application (patent law 1993) | ||
| WD01 | Invention patent application deemed withdrawn after publication |