CN108689541A - The processing method of the waste water containing ammonium acetate - Google Patents
The processing method of the waste water containing ammonium acetate Download PDFInfo
- Publication number
- CN108689541A CN108689541A CN201810373576.0A CN201810373576A CN108689541A CN 108689541 A CN108689541 A CN 108689541A CN 201810373576 A CN201810373576 A CN 201810373576A CN 108689541 A CN108689541 A CN 108689541A
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- CN
- China
- Prior art keywords
- waste water
- ammonium acetate
- processing method
- containing ammonium
- water containing
- Prior art date
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Classifications
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F9/00—Multistage treatment of water, waste water or sewage
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/24—Sulfates of ammonium
- C01C1/242—Preparation from ammonia and sulfuric acid or sulfur trioxide
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/02—Treatment of water, waste water, or sewage by heating
- C02F1/04—Treatment of water, waste water, or sewage by heating by distillation or evaporation
- C02F1/046—Treatment of water, waste water, or sewage by heating by distillation or evaporation under vacuum produced by a barometric column
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F2001/5218—Crystallization
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/34—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
- C02F2103/343—Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32 from the pharmaceutical industry, e.g. containing antibiotics
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Inorganic Chemistry (AREA)
- Pyridine Compounds (AREA)
- Heat Treatment Of Water, Waste Water Or Sewage (AREA)
Abstract
This case is related to a kind of processing method of the waste water containing ammonium acetate, and processing method includes the following steps:1) waste water containing ammonium acetate obtains water and mother liquor through vacuum distillation dehydration, distillation;2) stream liquid feeding is added dropwise into the mother liquor in step 1), after completion of dropwise addition, 1~3h is stirred to react at 40~60 DEG C, obtains the first mixture;3) temperature of the first mixture obtained by step 2) is down to 10~20 DEG C, crystallisation by cooling, filtration drying obtains solid ammonium sulfate, and it is for use to collect filtration residue liquid;4) acetic acid solution is collected into the residual solution vacuum distillation obtained by step 3).Flow of the present invention is simple, technical maturity, is suitble to industrialized utilization, can be used for the processing of high ammonium acetate waste water in orthene;The ammonium sulfate and acetic acid solution of recycling are that enterprise creates economic benefit, are suitable for continuous production, are easy to industrially promote and apply.
Description
Technical field
The present invention relates to the processing method of industrial wastewater more particularly to a kind of processing methods of waste water containing ammonium acetate.
Background technology
Orthene also known as accephate belong to low toxic pesticide.Orthene is oral insecticide, has stomach toxicity and touches
The effect of killing, and can ovicidal, have certain fumigation action, be slow-acting type insecticide, be suitable for vegetables, tea tree, tobacco, fruit tree, cotton
The crops such as flower, rice, wheat, rape prevent a variety of chewing types, sucking pest and evil mite and sanitary insect pest.Currently, same
Industry is all perplexed by the difficult bottleneck of waste water, and wastewater flow rate is big and without processing recovery method, constrains the performance of production capacity, therefore,
It is very crucial to seek economic recovery method.
Invention content
For the technical problems in the prior art, this case provides a kind of environmental protection and economic orthene produced
The processing method of the waste water containing ammonium acetate generated in journey meets green, environmental requirement.
To achieve the above object, this case is achieved through the following technical solutions:
A kind of processing method of the waste water containing ammonium acetate, wherein the treating method comprises following steps:
1) waste water containing ammonium acetate obtains water and mother liquor through vacuum distillation dehydration, distillation;
2) stream liquid feeding is added dropwise into the mother liquor in step 1), after completion of dropwise addition, 1~3h is stirred to react at 40~60 DEG C,
Obtain the first mixture;
3) temperature of the first mixture obtained by step 2) is down to 10~20 DEG C, crystallisation by cooling, filtration drying obtains solid
It is for use to collect filtration residue liquid for ammonium sulfate;
4) acetic acid solution is collected into the residual solution vacuum distillation obtained by step 3).
Preferably, the processing method of the waste water containing ammonium acetate, wherein the vacuum degree of the step 1) vacuum distillation
For 0.02~0.05MPa, temperature 50 C~70 DEG C, the vacuum distillation time is 3~4h.
Preferably, the processing method of the waste water containing ammonium acetate, wherein the water distilled in the step 1) accounts for waste water
The 25~40% of quality.
Preferably, the processing method of the waste water containing ammonium acetate, wherein the stream liquid feeding includes acid and stabilizer.
Preferably, the processing method of the waste water containing ammonium acetate, wherein the acid is sulfuric acid, sulfuric acid and mother liquor
Mass ratio is 0.1~0.3:1.
Preferably, the processing method of the waste water containing ammonium acetate, wherein the stabilizer includes 25~28wt% second
Acid anhydride, 16~18wt% dimethyl suflfates, 30~34wt%N- methyl pyrrolidones and 22~24wt%N- picolines.
Preferably, the processing method of the waste water containing ammonium acetate, wherein the mass ratio of the stabilizer and mother liquor is
0.01~0.02:1.
Preferably, the processing method of the waste water containing ammonium acetate, wherein in the step 2) time for adding be 1~
2h。
Preferably, the processing method of the waste water containing ammonium acetate, wherein the step 3) drying temperature be 100~
120 DEG C, drying time is 6~8h.
Preferably, the processing method of the waste water containing ammonium acetate, wherein the vacuum being evaporated under reduced pressure in the step 4)
Degree is 0.04~0.07MPa, 90 DEG C~100 DEG C of temperature.
The beneficial effects of the invention are as follows:
(1) flow of the present invention is simple, technical maturity, is suitble to industrialized utilization, can be used for high acetic acid in orthene
The processing of ammonium waste water;
(2) ammonium sulfate and acetic acid solution recycled is that enterprise creates economic benefit, is suitable for continuous production, is easy in industry
Upper popularization and application;
(3) present invention has economical and environmentally friendly double effects, has good social benefit and environmental benefit;
(4) the stream liquid feeding including acid and stabilizer is gradually added dropwise into mother liquor, improves the conversion ratio of ammonium acetate, from
And improve the yield of product;Stabilizer acetic anhydride, dimethyl suflfate, N-Methyl pyrrolidone and the collaboration of N- picolines use,
The stability for effectively increasing reaction system reduces the generation of by-product.
Specific implementation mode
With reference to embodiment, the present invention is described in further detail, to enable those skilled in the art with reference to specification
Word can be implemented according to this.
Embodiment 1
With mechanical agitation, Industry Waste is added in the 1000ml reaction bulbs of addition funnel and reflux condenser in thermometer
Water 600g opens stirring and positive empty pump, flask is heated to 50 DEG C, starts vacuum distillation dehydration, vacuum degree 0.02MPa, dehydration
3h deviates from water 160g, remaining as mother liquor, stops heating and changes back stream, stream liquid feeding is added dropwise into mother liquor, flow liquid feeding include 85g sulfuric acid,
2.1g acetic anhydrides, 1.6g dimethyl suflfates, 2.7gN- methyl pyrrolidones and 1.5gN- picolines.Time for adding 1.5h, then
Flow back 1h at 50 DEG C, is cooled to 10 DEG C and filters to obtain ammonium sulfate solids 156g, filtrated stock 190g, and mother liquor collection is depressurized
The vacuum degree of distillation, vacuum distillation is 0.05MPa, and 90 DEG C of temperature obtains acetic acid solution 84g.
Embodiment 2
With mechanical agitation, Industry Waste is added in the 1000ml reaction bulbs of addition funnel and reflux condenser in thermometer
Water 600g opens stirring and positive empty pump, flask is heated to 40 DEG C, starts vacuum distillation dehydration, vacuum degree 0.03MPa takes off
Water 3.5h deviates from water 170g, remaining as mother liquor, stops heating and changes back stream, and stream liquid feeding is added dropwise into mother liquor, and stream liquid feeding includes being added dropwise
90g sulfuric acid, 2.85g acetic anhydrides, 2.27g dimethyl suflfates, 2.97gN- methyl pyrrolidones and 1.9gN- picolines, when dropwise addition
Between 1.8h, then flow back at 40 DEG C 2h, is cooled to 15 DEG C and filters to obtain ammonium sulfate solids 197g, filtrated stock 215g, by mother liquor
Collection is evaporated under reduced pressure, and the vacuum degree of vacuum distillation is 0.06MPa, and 90 DEG C of temperature obtains acetic acid solution and obtains 75g.
Embodiment 3
With mechanical agitation, Industry Waste is added in the 1000ml reaction bulbs of addition funnel and reflux condenser in thermometer
Water 600g opens stirring and positive empty pump, flask is heated to 60 DEG C, starts vacuum distillation dehydration, vacuum degree 0.05MPa, dehydration
4h deviates from water 200g, stops heating and changes back stream, and stream liquid feeding is added dropwise into mother liquor, and it includes 95g sulfuric acid to flow liquid feeding, 3.42g acetic anhydrides,
Then 2.72g dimethyl suflfates, 3.8gN- methyl pyrrolidones and 2.1gN- picolines, time for adding 2h add at 60 DEG C
Heat reflux 2h, is cooled to 10 DEG C and filters to obtain ammonium sulfate solids solid 222g, filtrated stock 206g, and mother liquor collection is carried out decompression steaming
It evaporates, the vacuum degree of vacuum distillation is 0.07MPa, and 100 DEG C of temperature obtains acetic acid solution 87g.
Although the embodiments of the present invention have been disclosed as above, but its is not only in the description and the implementation listed
With it can be fully applied to various fields suitable for the present invention, for those skilled in the art, can be easily
Realize other modification, therefore without departing from the general concept defined in the claims and the equivalent scope, the present invention is simultaneously unlimited
In specific details.
Claims (10)
1. a kind of processing method of waste water containing ammonium acetate, which is characterized in that the treating method comprises following steps:
1) waste water containing ammonium acetate obtains water and mother liquor through vacuum distillation dehydration, distillation;
2) stream liquid feeding is added dropwise into the mother liquor in step 1), after completion of dropwise addition, 1~3h is stirred to react at 40~60 DEG C, obtains the
One mixture;
3) temperature of the first mixture obtained by step 2) is down to 10~20 DEG C, crystallisation by cooling, filtration drying obtains solid sulphuric acid
It is for use to collect filtration residue liquid for ammonium;
4) acetic acid solution is collected into the residual solution vacuum distillation obtained by step 3).
2. the processing method of the waste water containing ammonium acetate as described in claim 1, which is characterized in that the step 1) vacuum distillation
Vacuum degree is 0.02~0.05MPa, and temperature 50 C~70 DEG C, the vacuum distillation time is 3~4h.
3. the processing method of the waste water containing ammonium acetate as described in claim 1, which is characterized in that the water distilled in the step 1)
Account for the 25~40% of wastewater quality.
4. the processing method of the waste water containing ammonium acetate as described in claim 1, which is characterized in that the stream liquid feeding includes sour and steady
Determine agent.
5. the processing method of the waste water according to any one of claims 1-4 containing ammonium acetate, which is characterized in that the acid is sulphur
The mass ratio of acid, sulfuric acid and mother liquor is 0.1~0.3:1.
6. the processing method of the waste water according to any one of claims 1-4 containing ammonium acetate, which is characterized in that the stabilizer packet
Include 25~28wt% acetic anhydrides, 16~18wt% dimethyl suflfates, 30~34wt%N- methyl pyrrolidones and 22~24wt%N-
Picoline.
7. the processing method of the waste water according to any one of claims 1-4 containing ammonium acetate, which is characterized in that the stabilizer with
The mass ratio of mother liquor is 0.01~0.02:1.
8. the processing method of the waste water containing ammonium acetate as described in claim 1, which is characterized in that time for adding in the step 2)
For 1~2h.
9. the processing method of the waste water containing ammonium acetate as described in claim 1, which is characterized in that the step 3) drying temperature is
100~120 DEG C, drying time is 6~8h.
10. the processing method of the waste water containing ammonium acetate as described in claim 1, which is characterized in that decompression is steamed in the step 4)
The vacuum degree evaporated is 0.04~0.07MPa, 90 DEG C~100 DEG C of temperature.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN111689635A (en) * | 2020-06-10 | 2020-09-22 | 南京工业大学 | Method for treating waste water containing ammonium acetate |
Citations (4)
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CN101050224A (en) * | 2007-05-21 | 2007-10-10 | 鄂州海丰化工实业有限公司 | Technique for extracting and recovering wastewater of acephate pesticide |
CN101215063A (en) * | 2007-12-27 | 2008-07-09 | 沙隆达集团公司 | Integral treatment method for waste water of acephate producing process |
JP2014144440A (en) * | 2013-01-30 | 2014-08-14 | Keiichiro Asaoka | Treating method of harmful waste, producing method of compost using the treating method and treating system of harmful waste |
CN104909993A (en) * | 2015-06-15 | 2015-09-16 | 江苏蓝丰生物化工股份有限公司 | Industrial synthesis method of dicamba key intermediate 2,5-dichlorophenol |
-
2018
- 2018-04-24 CN CN201810373576.0A patent/CN108689541A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN101050224A (en) * | 2007-05-21 | 2007-10-10 | 鄂州海丰化工实业有限公司 | Technique for extracting and recovering wastewater of acephate pesticide |
CN101215063A (en) * | 2007-12-27 | 2008-07-09 | 沙隆达集团公司 | Integral treatment method for waste water of acephate producing process |
JP2014144440A (en) * | 2013-01-30 | 2014-08-14 | Keiichiro Asaoka | Treating method of harmful waste, producing method of compost using the treating method and treating system of harmful waste |
CN104909993A (en) * | 2015-06-15 | 2015-09-16 | 江苏蓝丰生物化工股份有限公司 | Industrial synthesis method of dicamba key intermediate 2,5-dichlorophenol |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN111689635A (en) * | 2020-06-10 | 2020-09-22 | 南京工业大学 | Method for treating waste water containing ammonium acetate |
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