CN1958481A - Chloroactic acid method for treating wastewater of glycine, and comprehensive utilization method - Google Patents
Chloroactic acid method for treating wastewater of glycine, and comprehensive utilization method Download PDFInfo
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- CN1958481A CN1958481A CN 200510117616 CN200510117616A CN1958481A CN 1958481 A CN1958481 A CN 1958481A CN 200510117616 CN200510117616 CN 200510117616 CN 200510117616 A CN200510117616 A CN 200510117616A CN 1958481 A CN1958481 A CN 1958481A
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Abstract
This invention is aimed to treating toxic wastewater from glycine production by chloroacetic acid method and recovering valuable resources from the wastewater. This invention utilizes evaporation, concentration, cooling and crystallization to remove amine, conversion to remove chloroacetic acid and dichloroacetic acid, alcohol-precipitation to remove glycine and iminodiacetic acid, extraction to remove acetic acid, monochloroacetic acid and dichloroacetic acid, and oxidative decomposition to completely decompose toxic substances in the wastewater. This invention provides a good method for environmental protection engineering and resource recycling.
Description
Technical field
Present technique relates to chloroactic acid method glycin waste water and method of comprehensive utilization, belongs to environmental protection and field of fine chemical.
Technical background
In recent years, along with the develop rapidly of glyphosate herbicidal in the world, the production as the sweet chloric acid of glyphosate main raw material has also obtained developing rapidly in China, and the enterprise that has develops into several kilotons from producing the hundreds of ton per year, develops into several ten thousand tons from several kilotons again.As China is with fastest developing speed at present, output is maximum, the also glycine overwhelming majority employing chloroactic acid method manufacturing of the main raw material of maximum glyphosate of export volume.The output of glycine has been up, but problem also brought, and originally is the production of a green product, but discharges a large amount of waste water, and one ton of product is discharged three tons of waste water.Contain a large amount of inorganic salt (ammonium chloride) and organic acid, salt in these waste water, COD content is very high, and some organism toxicity and corrodibility are all very big, as Mono Chloro Acetic Acid, formaldehyde, it is big all to belong to toxicity, the deep-etching material, be seriously to surpass discharging standards, do not add processing and do not allow to discharge.And a large amount of ammonium chlorides in the waste water and organic acid, salt are very valuable resources, and not adding recovery utilization is great waste.Patent 200510069080.7 patented technologies, with lime ammonium chloride is converted into calcium chloride, further make Snow Agent, though the part recovery resource, but the Mono Chloro Acetic Acid and the carcinogenic formaldehyde that can not thoroughly solve waste water pollution problem, particularly hypertoxic deep-etching fail to be handled completely and utilize.Purpose of the present invention just is thoroughly to solve chloroactic acid method glycine waste water pollution problems, accomplishes wastewater zero discharge, and reclaims resource as much as possible.
Summary of the invention
The present invention is characterized in, thoroughly solve waste water pollution problem, accomplish wastewater zero discharge.Principal character of the present invention also is to reclaim resource as far as possible, and ammonium chloride, glycine are derivative, and Mono Chloro Acetic Acid, dichloro acetic acid and acetate are all recycled to greatest extent.Principal character of the present invention also is severe toxicity, deep-etching material---Mono Chloro Acetic Acid and carcinogenic substance---, and formaldehyde has obtained thorough processing.
Embodiment
The present invention is achieved in that
One, takes off ammonium, (quality group is into about being: ammonium chloride accounts for 20% with 100 ℃ of dealcoholizing waste waters, glycine, iminodiethanoic acid 5.6%, urotropine accounts for 6%, and acetate, Mono Chloro Acetic Acid, dichloro acetic acid account for 4.4%, the rest is water), be cooled to normal temperature (about 30 ℃) and take off ammonium (ammonium chloride), once take off and will continue heating evaporation moisture content after ammonium is finished and concentrate waste water, ammonium (taking off ammonium for the second time) is taken off in cooling can also take off ammonium three times, takes off ammonium four times.
Two, solidify
Adding special composite high-molecular water-absorbing material (inhaling the nearly 200g/g of salt solution) in last mother liquor solidifies last mother liquor.
Three, transform, add water in above-mentioned solidified mother liquor, make it become solution, add Mono Chloro Acetic Acid again and be converted into the promotor of Padil in solution, promotor can be ammonia, urea, and at 50～60 ℃, PH ≈ 7～8 reacted 1-2 hour, must transform and finish liquid.
Four, alcohol is analysed
The conversion of Xiang Sanzhong is finished and is added alcohol (methyl alcohol or ethanol) in the liquid and carry out alcohol and analyse, and pure water ratio is about 3: 1, separates out Padil and iminodiethanoic acid, and it is told, and mother liquor removes to reclaim alcohol.
Five, acetate, Mono Chloro Acetic Acid, dichloro acetic acid are reclaimed in extraction.
Mother liquor in four is added water be made into chloroacetic acid solution, content adopts 20～40 (quality) % trialkylamine (7301), 10～30 (quality) % n-Octanol 40～60 (quality) % kerosene 5%～10%, forms the mixed twine mixture, extracts, and removes Mono Chloro Acetic Acid.
Six, oxygenolysis poisonous substance
Add in the extracting phase of Xiang Wuzhong (last waste water) contriver's patented product percarbonic acid amine (patent No.: 02104415.5) or middle section aldehyde do not have Mono Chloro Acetic Acid and formaldehyde in the shadow formaldehyde scavenger oxygenolysis waste water, reaching can reuse.
Embodiment one, gets 100ml dealcoholizing waste water (30 ℃) and is heated to about 105 ℃, and the evaporation concentration dehydration steams 10 gram water, is cooled to 30 ℃ and separates out ammonium chloride, and filtering separation gets ammonium chloride 4 grams.
Embodiment two, and getting 100ml Mono Chloro Acetic Acid concentration (quality) is 5% usefulness 30%TOA/20% n-Octanol/50% kerosene extraction, and the Mono Chloro Acetic Acid percentage extraction is more than 95%.
Embodiment three, cross phosphinylidyne ammonium exhaustive oxidation with patented product and decompose Mono Chloro Acetic Acid and formaldehyde, and formaldehyde in the last sewage and Mono Chloro Acetic Acid reach can reuse.
Claims (1)
1, the sweet ammonia waste water of a kind of chloroactic acid method is handled and method of comprehensive utilization, it is characterized in that, with waste water after the dealcoholysis of chloroactic acid method glycine is raw material, adopt 1, take off ammonium, (quality group is into about being: ammonium chloride accounts for 20% with 100 ℃ of dealcoholizing waste waters, glycine, iminodiethanoic acid 5.6%, urotropine accounts for 6%, acetate, Mono Chloro Acetic Acid, dichloro acetic acid accounts for 4.4%, the rest is water), be cooled to normal temperature (about 30 ℃) and take off ammonium (ammonium chloride), once take off and to continue the concentrated waste water of heating evaporation moisture content after ammonium is finished, ammonium (take off for the second time ammonium) is taken off in cooling, can also take off ammonium three times, takes off ammonium four times; 2, solidify, in last mother liquor, add special composite high-molecular water-absorbing material (inhaling the nearly 200g/g of salt solution) last mother liquor is solidified; 3, transform, add water in above-mentioned solidified mother liquor, make it become solution, add Mono Chloro Acetic Acid again and be converted into the promotor of Padil in solution, promotor can be ammonia, urea, and at 50～60 ℃, PH ≈ 7～8 reacted 1-2 hour, must transform and finish liquid; 4, alcohol is analysed, and the conversion in 3 is finished and added alcohol (methyl alcohol or ethanol) in the liquid and carry out alcohol and analyse, and pure water ratio is about 3: 1, separates out Padil and iminodiethanoic acid, and it is told, and mother liquor removes to reclaim alcohol; 5, acetate, Mono Chloro Acetic Acid, dichloro acetic acid are reclaimed in extraction; Mother liquor in 4 is added water be made into chloroacetic acid solution, content adopts 20～40 (quality) % trialkylamine (7301), 10～30 (quality) % n-Octanol 40～60 (quality) % kerosene 5%～10%, forms the mixed twine mixture, extracts, and removes Mono Chloro Acetic Acid; 6, oxygenolysis poisonous substance, add in the extracting phase in 5 (last waste water) contriver's patented product percarbonic acid amine (patent No.: 02104415.5) or middle section aldehyde do not have the shadow formaldehyde scavenger, Mono Chloro Acetic Acid in the oxygenolysis waste water and formaldehyde, reaching can reuse.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510117616 CN1958481A (en) | 2005-11-04 | 2005-11-04 | Chloroactic acid method for treating wastewater of glycine, and comprehensive utilization method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510117616 CN1958481A (en) | 2005-11-04 | 2005-11-04 | Chloroactic acid method for treating wastewater of glycine, and comprehensive utilization method |
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| Publication Number | Publication Date |
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| CN1958481A true CN1958481A (en) | 2007-05-09 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 200510117616 Pending CN1958481A (en) | 2005-11-04 | 2005-11-04 | Chloroactic acid method for treating wastewater of glycine, and comprehensive utilization method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108558689A (en) * | 2018-05-28 | 2018-09-21 | 河南红东方化工股份有限公司 | It is a kind of industry amion acetic acid by-product ammonium chloride without haline water solution processing methods |
| CN109650646A (en) * | 2018-11-21 | 2019-04-19 | 河北东华冀衡化工有限公司 | A kind of processing method of glycine production waste water |
-
2005
- 2005-11-04 CN CN 200510117616 patent/CN1958481A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108558689A (en) * | 2018-05-28 | 2018-09-21 | 河南红东方化工股份有限公司 | It is a kind of industry amion acetic acid by-product ammonium chloride without haline water solution processing methods |
| CN109650646A (en) * | 2018-11-21 | 2019-04-19 | 河北东华冀衡化工有限公司 | A kind of processing method of glycine production waste water |
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