CN108689541A - The processing method of the waste water containing ammonium acetate - Google Patents

The processing method of the waste water containing ammonium acetate Download PDF

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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
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.)
Pending
Application number
CN201810373576.0A
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Chinese (zh)
Inventor
刘宇
张贤振
蒋磊
周全义
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
JIANGSU LANFENG BIOCHEMICAL CO Ltd
Original Assignee
JIANGSU LANFENG BIOCHEMICAL CO Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Application filed by JIANGSU LANFENG BIOCHEMICAL CO Ltd filed Critical JIANGSU LANFENG BIOCHEMICAL CO Ltd
Priority to CN201810373576.0A priority Critical patent/CN108689541A/en
Publication of CN108689541A publication Critical patent/CN108689541A/en
Pending legal-status Critical Current

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Classifications

    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F9/00Multistage treatment of water, waste water or sewage
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01CAMMONIA; CYANOGEN; COMPOUNDS THEREOF
    • C01C1/00Ammonia; Compounds thereof
    • C01C1/24Sulfates of ammonium
    • C01C1/242Preparation from ammonia and sulfuric acid or sulfur trioxide
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/02Treatment of water, waste water, or sewage by heating
    • C02F1/04Treatment of water, waste water, or sewage by heating by distillation or evaporation
    • C02F1/046Treatment of water, waste water, or sewage by heating by distillation or evaporation under vacuum produced by a barometric column
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/66Treatment of water, waste water, or sewage by neutralisation; pH adjustment
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F1/00Treatment of water, waste water, or sewage
    • C02F1/52Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
    • C02F2001/5218Crystallization
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2101/00Nature of the contaminant
    • C02F2101/30Organic compounds
    • C02F2101/38Organic compounds containing nitrogen
    • CCHEMISTRY; METALLURGY
    • C02TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02FTREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
    • C02F2103/00Nature of the water, waste water, sewage or sludge to be treated
    • C02F2103/34Nature of the water, waste water, sewage or sludge to be treated from industrial activities not provided for in groups C02F2103/12 - C02F2103/32
    • C02F2103/343Nature 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

The processing method of the waste water containing ammonium acetate
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.
CN201810373576.0A 2018-04-24 2018-04-24 The processing method of the waste water containing ammonium acetate Pending CN108689541A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
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

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Application publication date: 20181023

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