CN104874196A - Method for processing sodium and ammonium acetate-diazonium organic compound-methanol-water mixed solution - Google Patents
Method for processing sodium and ammonium acetate-diazonium organic compound-methanol-water mixed solution Download PDFInfo
- Publication number
- CN104874196A CN104874196A CN201510138385.2A CN201510138385A CN104874196A CN 104874196 A CN104874196 A CN 104874196A CN 201510138385 A CN201510138385 A CN 201510138385A CN 104874196 A CN104874196 A CN 104874196A
- Authority
- CN
- China
- Prior art keywords
- liquid
- organic matter
- diazonium
- side line
- sodium
- 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.)
- Granted
Links
Abstract
The invention provides a method for processing a sodium and ammonium acetate-diazonium organic compound-methanol-water mixed solution through the combination of the continuous extrinsic cycle reaction side stream distillation process and the liquid-liquid extraction process. A raw material mixed liquor and an alkali liquor are mixed up, and then the mixed liquor is added into a reaction lateral line rectifying column. During the extrinsic cycles of tower bottoms, an ammonium salt is converted into a sodium salt by the reaction side stream distillation, and then tail-gas ammonia and methanol can be separated. A mixture of sodium acetate, diazonium organic compound and water is obtained in a dust-settling compartment. After that, the mixture is subjected to the liquid-liquid extraction treatment with cyclohexane as an extraction agent, and then a sodium acetate aqueous solution and an organic phase can be obtained. The sodium acetate is obtained through the evaporation process of the sodium acetate aqueous solution. The diazonium organic compound is recycled through the flash evaporation of the organic phase, and the extraction agent after separation is recycled. At the same time, the tail gas is subjected to the sulphuric acid treatment to obtain ammonium sulfate. By means of the above method of the present invention, industrial grade sodium acetate, methanol with the concentration over 95 wt%, diazonium organic compound with the concentration over 97%, and ammonium sulfate, can be obtained respectively. The COD value of water after being separated is lower than 1000PPM. The method is simple in process and low in energy consumption during the separating process.
Description
Technical field
The present invention relates to a kind of multicomponent mixture treatment of Organic Wastewater and the technique be separated, be specifically related to the separation method of a kind of continuous external circulation reactive distillation and liquid-liquid extraction combination process sodium and ammonium acetate salt, diazonium organic matter, methyl alcohol and water mixed solution.
Background technology
Pymetrozine is novel heterocyclic efficient selective pesticide, has very strong interior absorption, can be absorbed by crops well, spreads to each position of crop by Uptake and translocation effect.Exactly because the mechanism of action of pymetrozine uniqueness, make it have selective (only effective to sucking mouthpart insect) of height, have good security to mammal, birds, fishes and shrimps, honeybee, non-target arthropod etc.
In pymetrozine production process, produce a large amount of waste water, wherein mainly comprise sodium and ammonium acetate salt, diazonium organic matter and methyl alcohol.The domestic and international recovery for above-mentioned salt-containing organic wastewater and processing method mainly contain physico-chemical process, biochemical process and chemical hydrolysis at present.Adopt biochemical process and chemical hydrolysis all can destroy active ingredient in waste water.The biochemical process processing time is long, degraded is not thorough, and in addition, diazonium organic matter can make microorganism poisoning, and cause extreme shock to biological treatment, disposal cost is high; Chemical method does not reach the object reclaiming salt and methyl alcohol, easily causes secondary pollution.
To above-mentioned mixed liquor as taked effective process and separation method, not only can obtain the high sodium acetate of added value and methyl alcohol, reaching the object of process waste water simultaneously, significantly reduce processing procedure cost, obtain good economic benefit.Adopt the above-mentioned salt-containing organic wastewater of conventional distil-lation method process, need repeatedly to distill, form saliferous organic solid castoff after process, the waste water COD after process reaches 40000PPM, still needs to carry out biochemical treatment, and processing procedure expense, energy consumption are higher.
Summary of the invention
The reaction side line rectifying of a kind of continuous external circulation and liquid-liquid extraction is the object of the present invention is to provide to combine process sodium and ammonium acetate salt, diazonium organic matter, the technique of methyl alcohol and water mixed solution, first through the rectifying of primary first-order equation side line, ammonium salt is converted into sodium salt, and isolate tail gas ammonia and methyl alcohol, what obtain contains sodium acetate, diazonium organic matter and aqueous mixtures are again through liquid-liquid extraction, separation obtains sodium acetate aqueous solution and comprises diazonium organic matter, the organic phase of extractant, sodium acetate aqueous solution obtains fine chemicals sodium acetate through evaporation process, organic phase is through the recyclable diazonium organic matter of flash separation extractant, extractant can recycle, tail gas ammonia obtains ammonium sulfate through Waste Sulfuric Acid process.Said process obtains sodium acetate, methyl alcohol, diazonium organic matter and ammonium sulfate respectively, and after being separated, the COD of water is lower than 1000PPM, can enter industrial wastewater treatment system; Compared with traditional handicraft, it is simple that the present invention has processing step, the advantage that separation process energy consumption is low.
For achieving the above object, the present invention adopts following technical scheme:
Continuous external circulation reaction side line rectifying and liquid-liquid extraction combine a method for process sodium and ammonium acetate salt, diazonium organic matter, methyl alcohol and water mixed solution, comprise the following steps:
1) raw material sodium and ammonium acetate salt, diazonium organic matter, methyl alcohol and water mixed solution add from reacting side line rectifying column middle and lower part material inlet by reacting with alkali lye after mixing, reaction side line tower bottom of rectifying tower liquid carries out outer circulation by the recycle feed mouth above outer circulation pump pump to material inlet, through the rectifying of reaction side line, ammonium salt in material liquid is converted into sodium salt, reaction side line rectifying bottom discharge is to dust-settling compartment, dust-settling compartment discharging is for containing sodium acetate, diazonium organic matter and aqueous mixtures, reaction side line rectifying column side line, tower top obtains more than 95wt% methyl alcohol and tail gas ammonia respectively,
2) multistage liquid-liquid extraction tower is entered containing sodium acetate, diazonium organic matter and aqueous mixtures, take cyclohexane as extractant, through multiple stage of countercurrent liquid-liquid extraction, at the bottom of tower, tower top obtains sodium acetate aqueous solution respectively and comprises the organic phase of diazonium organic matter, extractant, obtain sodium acetate aqueous solution at the bottom of multistage liquid-liquid extraction tower and obtain technical grade acetic acid sodium through evaporation process, the Organic substance in water content of generation is lower than 0.1wt%;
3) multistage liquid-liquid extraction tower top is the organic phase primarily of extractant and diazonium organic matter composition, and through flash column process, tower top is extracted agent, is circulated to multistage liquid liquid counter-current extraction tower and recycles, obtain content >=97wt% diazonium organic matter at the bottom of tower.
The inventive method establishes the technique of the rectifying of a kind of successive reaction side line and liquid-liquid extraction combination, for sodium and ammonium acetate salt, diazonium organic matter, methyl alcohol and water mixed solution, through the rectifying of primary first-order equation side line, ammonium salt wherein can be converted into sodium salt, and isolate tail gas ammonia and methyl alcohol, obtain containing sodium acetate, diazonium organic matter and aqueous mixtures, again will containing sodium acetate, diazonium organic matter and aqueous mixtures are that extractant is through liquid-liquid extraction with cyclohexane, obtain sodium acetate aqueous solution respectively and comprise diazonium organic matter, the organic phase of extractant, sodium acetate aqueous solution obtains sodium acetate through evaporation process, organic phase uses through the recyclable diazonium organic matter circling of flash separation extractant, extractant after separation can recycle, meanwhile, the methyl alcohol obtained respectively and tail gas ammonia, methyl alcohol recycles as solvent, and tail gas ammonia obtains ammonium sulfate through Waste Sulfuric Acid process.Said process obtains sodium acetate, methyl alcohol, diazonium organic matter and ammonium sulfate respectively, and after being separated, the COD of water is lower than 1000PPM, can enter industrial wastewater treatment system; The inventive method simplifies the technological process of production, and separation process energy consumption is low.
In described method, in sodium and ammonium acetate salt, diazonium organic matter, methyl alcohol and water mixed solution, sodium and ammonium acetate salt weight percentage about 21.5 ~ 23.0%, diazonium organic matter about 2.0 ~ 2.5%, methyl alcohol 15.0 ~ 16.0%.
In described step (1), the tower top of successive reaction side line rectifying column and the temperature at the bottom of tower are respectively 41.4 ~ 43.1 DEG C and 100.2 ~ 102.7 DEG C.Preferably, the number of theoretical plate (N) of reaction side line rectifying column is 47, and material inlet position is at the 41st block of plate, and lateral line discharging position is at the 13rd block of plate, and recycle feed mouth position is at the 36th block of plate.
In described step (1), the preferred 50wt%NaOH solution of alkali lye, the mass ratio of material liquid and 50%NaOH alkali lye is 1: 0.146.
In described step (1), tail gas ammonia adopts sulfuric acid treatment to obtain ammonium sulfate.
In described step (2) multiple stage of countercurrent liquid-liquid extraction method, described extractant is industrial cyclohexane.Extractant with containing sodium acetate, diazonium organic matter and aqueous mixtures feed weight ratio is: 0.4 ~ 1.2: 1.
In described step (2) multiple stage of countercurrent liquid-liquid extraction method, multiple stage of countercurrent liquid-liquid extraction tower number of theoretical plate (N) is 4, and operating temperature is 10.5 ~ 29.5 DEG C.
In described step (3), flash column operating pressure is 0.10 ~ 0.15*10
5pa, tower top and the temperature at the bottom of tower are respectively 52.1 ~ 56.7 DEG C and 87.3 ~ 88.9 DEG C.Preferably, flash column number of theoretical plate (N) is 5, and feedstock position is at the 3rd block of plate.
Continuous external circulation reaction side line rectifying of the present invention and liquid-liquid extraction combine process sodium and ammonium acetate salt, diazonium organic matter, the method of methyl alcohol and water mixed solution, concrete grammar is as follows: ammonium and sodium acetate, diazonium organic matter, methyl alcohol and water mixed solution and 50%NaOH add in mixing channel in 1: 0.146 ratio, add in reaction side line rectifying column by reaction side line rectifying column middle and lower part charging aperture after mixing, tower bottoms by circulating pump outer circulation to recycle feed mouth, control reaction side line rectifying tower top, end temperature is respectively 41.4 ~ 43.1 DEG C and 100.2 ~ 102.7 DEG C, through the rectifying of reaction side line, ammonium salt in material liquid is converted into sodium salt, reaction side line rectifying tower top ammonia is absorbed by Waste Sulfuric Acid in absorption cell, and form ammonium sulfate, lateral line discharging is more than 95% methyl alcohol, the discharging of reaction side line rectifier bottoms is to liquid reducing chamber, diazonium organic wastewater containing sodium acetate in liquid reducing chamber enters in multiple stage of countercurrent liquid-liquid extraction tower middle and upper part, and extractant n-hexane adds in the middle and lower part of multiple stage of countercurrent liquid-liquid extraction tower, and extractant and liquid-liquid extraction tower charge ratio are 0.4 ~ 1.2: 1, after multiple stage of countercurrent liquid-liquid extraction, the discharging of liquid-liquid extraction top of tower is for containing the organic n-hexane of diazonium, and enter flash column containing the organic n-hexane of diazonium, operating pressure is 0.10 ~ 0.15*10
5pa, tower top and the temperature at the bottom of tower are respectively 52.1 ~ 56.7 DEG C and 87.3 ~ 88.9 DEG C, through flash column process, obtain content>=97% diazonium organic matter and n-hexane respectively, n-hexane recycle is to liquid-liquid extraction tower, and the discharging of multiple stage of countercurrent liquid-liquid extraction tower bottom is the aqueous solution containing sodium acetate, through evaporation and drying unit process, obtain 98% sodium acetate and industry water respectively, in industry water, COD is lower than 1000PPM, and industry water recycles as water for industrial use.
The technique that the present invention adopts the rectifying of successive reaction side line and multiple stage of countercurrent liquid-liquid extraction to combine, process sodium and ammonium acetate salt, diazonium organic matter, methyl alcohol and water mixed solution, through the rectifying of primary first-order equation side line, ammonium salt wherein can be converted into sodium salt, and isolate tail gas ammonia and methyl alcohol, obtain containing sodium acetate, diazonium organic matter and aqueous mixtures, again will containing sodium acetate, diazonium organic matter and aqueous mixtures carry out multiple stage of countercurrent liquid-liquid extraction, obtain sodium acetate aqueous solution and diazonium organic matter respectively, extractant mixture, sodium acetate aqueous solution obtains fine chemicals sodium acetate through evaporation process, diazonium organic matter, extractant mixture flash separation, diazonium content of organics >=97%, the extractant that multiple stage of countercurrent liquid-liquid extraction adopts is n-hexane, can recycle.Obtain more than 95% methyl alcohol and tail gas ammonia respectively in reaction side line distillation process, 95% methyl alcohol recycles as solvent, and tail gas ammonia obtains ammonium sulfate through Waste Sulfuric Acid process simultaneously.Adopt the inventive method, above-mentioned processing procedure obtains sodium acetate, methyl alcohol, diazonium organic matter and ammonium sulfate respectively, and after being separated, the COD of water is lower than 1000PPM, can enter industrial wastewater treatment system; Simplify the technological process of production, separation process energy consumption is low.
Describe the present invention below in conjunction with specific embodiment.Protection scope of the present invention is not limited with detailed description of the invention, but is limited by claim.
Accompanying drawing explanation
Fig. 1 is the schematic flow sheet that continuous external circulation reaction side line rectifying and liquid-liquid extraction combine process sodium and ammonium acetate salt-diazonium nitrogen organic-methanol-water mixed solution.
Detailed description of the invention
Below by specific embodiment, technical solutions according to the invention are further described in detail, but are necessary to point out that following examples are only for the description to summary of the invention, do not form limiting the scope of the invention.
Continuous external circulation reaction side line rectifying of the present invention and liquid-liquid extraction combine the method for process sodium and ammonium acetate salt-diazonium nitrogen organic-methanol-water mixed solution, react side line rectifying and multiple stage of countercurrent liquid-liquid extraction coupling apparatus and technological process with reference to Fig. 1, wherein 1 is dashpot, 2 is liquid reducing chamber, 3 is reaction side line rectifying tower reactor, 4 is charging aperture, 5 is reaction side line rectifying column, 6 is recycle feed mouth, 7 is side line discharge, 8 is absorption cell, 9 is circulating pump, 10 is multiple stage of countercurrent liquid-liquid extraction tower, 11 is raw material, 12 is 50%NaOH solution, 13 is raw material and the mixed feeding of 50%NaOH solution, 14 eject material for reacting side line rectifying tower, 15 is Waste Sulfuric Acid, 16 is lateral line discharging, 17 is tower bottoms recycle feed, 18 is the charging of multiple stage of countercurrent liquid-liquid extraction tower, 19 is the discharging of multiple stage of countercurrent liquid-liquid extraction top of tower, 20 is the extractant of multiple stage of countercurrent liquid-liquid extraction tower, 21 is the discharging of multiple stage of countercurrent liquid-liquid extraction tower bottom, 22 is flash column, 23 is flash column bottom discharge, 24 is flash column top discharge, 25 is evaporation and drying unit, 26 is evaporation and drying unit bottom discharge, 27 is evaporation and drying unit top discharge.
The sodium adopting certain company to provide and ammonium acetate salt, diazonium organic matter, methyl alcohol and water mixed solution are raw material, the operation of reaction side line rectifying column is carried out at ambient pressure, tower internal diameter is 25mm, the stainless steel helices of in-built φ 3*3 θ type, through measuring by standards system, this height equivalent to one theoretical plate HETP=27mm, tower reactor coiled electrical heating, raw material, liquid-liquid extraction agent charging and each device discharging etc. are all with glass rotameter metering, and reaction side line rectifying column adopts exteenal reflux.
Ammonium and sodium acetate, diazonium organic matter, methyl alcohol and water mixed solution 11 add mixing channel 1 with 50%NaOH solution 12 in 1: 0.146 ratio, add in reaction side line rectifying column 5 by reaction side line rectifying column 5 middle and lower part charging aperture 4 after mixing, in tower reactor 3, solution is circulated to recycle feed mouth 6 by circulating pump 9, control reaction side line rectifying column 5 tower top, end temperature are respectively 41.4 ~ 43.1 DEG C and 100.2 ~ 102.7 DEG C, control tower top reflux ratio 1.5: 1, reaction side line rectifying tower top discharging 14 is ammonia, absorbed by Waste Sulfuric Acid in absorption cell 8, and form ammonium sulfate, lateral line discharging 16 is more than 95% methyl alcohol, and from side line discharge 7 extraction of reaction side line rectifying column 5, at the bottom of reaction side line rectifying tower, discharging is to liquid reducing chamber 2, multiple stage of countercurrent liquid-liquid extraction tower charging 18 is from the diazonium organic wastewater containing sodium acetate in liquid reducing chamber 2, enter in multiple stage of countercurrent liquid-liquid extraction tower 10 middle and upper part, extractant n-hexane 20 adds in multiple stage of countercurrent liquid-liquid extraction tower 10 middle and lower part, extractant is 1: 1 with the diazonium organic wastewater charge ratio containing sodium acetate, after liquid-liquid extraction, extraction tower 10 top discharge 19 is for containing the organic n-hexane of diazonium, process through flash column 22 containing the organic n-hexane of diazonium, flash column bottom discharge 23 and top discharge 24 obtain diazonium organic matter and n-hexane respectively, n-hexane and top discharge 24 are circulated to liquid-liquid extraction tower 10, multiple stage of countercurrent liquid-liquid extraction tower 10 bottom discharge 21 is the aqueous solution containing sodium acetate, process through evaporation and drying unit 25, bottom discharge 26 and top discharge 27 obtain 98% sodium acetate and industry water respectively, and in industry water, COD is lower than 1000PPM, and industry water can be used as water for industrial use and recycles.
The rectifying of described reaction side line and the preferred process conditions of liquid-liquid extraction separation process as follows:
Top, end temperature, reflux ratio, feed entrance point and the numbers of plates such as reaction side line rectifying column 5, multistage liquid-liquid extraction tower 10 and flash column 22 are shown in Table 1.
Table 1 reacts side line rectifying and liquid-liquid extraction separation process conditions
Analyze through HP chromatograph, continuous external circulation reaction side line rectifying and liquid-liquid extraction combine process sodium and the results are shown in Table shown in 2 of ammonium acetate salt-diazonium nitrogen organic-methanol-water mixed solution.
The reaction side line rectifying of table 2 continuous external circulation and liquid-liquid extraction combine the result of process sodium and ammonium acetate salt-diazonium nitrogen organic-methanol-water mixed solution
Table 2 (Continued)
Claims (8)
1. continuous external circulation reaction side line rectifying and liquid-liquid extraction combine a method for process sodium and ammonium acetate salt, diazonium organic matter, methyl alcohol and water mixed solution, comprise the following steps:
1) raw material sodium and ammonium acetate salt, diazonium organic matter, methyl alcohol and water mixed solution add from reacting side line rectifying column middle and lower part material inlet by reacting with alkali lye after mixing, reaction side line tower bottom of rectifying tower liquid carries out outer circulation by the recycle feed mouth above outer circulation pump pump to material inlet, through the rectifying of reaction side line, ammonium salt in material liquid is converted into sodium salt, reaction side line rectifying bottom discharge is to dust-settling compartment, dust-settling compartment discharging is for containing sodium acetate, diazonium organic matter and aqueous mixtures, reaction side line rectifying column side line, tower top obtains more than 95wt% methyl alcohol and tail gas ammonia respectively,
2) multistage liquid-liquid extraction tower is entered containing sodium acetate, diazonium organic matter and aqueous mixtures, take cyclohexane as extractant, through multiple stage of countercurrent liquid-liquid extraction, at the bottom of tower, tower top obtains sodium acetate aqueous solution respectively and comprises the organic phase of diazonium organic matter, extractant, obtain sodium acetate aqueous solution at the bottom of multistage liquid-liquid extraction tower and obtain technical grade acetic acid sodium through evaporation process, the Organic substance in water content of generation is lower than 0.1wt%;
3) multistage liquid-liquid extraction tower top is the organic phase primarily of extractant and diazonium organic matter composition, and through flash column process, tower top is extracted agent, is circulated to multistage liquid liquid counter-current extraction tower and recycles, obtain content >=97wt% diazonium organic matter at the bottom of tower.
2. continuous external circulation reaction side line rectifying according to claim 1 and liquid-liquid extraction combine the method for process sodium and ammonium acetate salt, diazonium organic matter, methyl alcohol and water mixed solution, it is characterized in that: in described sodium and ammonium acetate salt, diazonium organic matter, methyl alcohol and water mixed solution, weight percentage is sodium and ammonium acetate salt 21.5 ~ 23.0%, diazonium organic matter about 2.0 ~ 2.5%, methyl alcohol 15.0 ~ 16.0%.
3. continuous external circulation reaction side line rectifying according to claim 1 and 2 and liquid-liquid extraction combine the method for process sodium and ammonium acetate salt, diazonium organic matter, methyl alcohol and water mixed solution, it is characterized in that: in described step (1), the tower top of successive reaction side line rectifying column and the temperature at the bottom of tower are respectively 41.4 ~ 43.1 DEG C and 100.2 ~ 102.7 DEG C.
4. continuous external circulation reaction side line rectifying according to claim 1 and 2 and liquid-liquid extraction combine the method for process sodium and ammonium acetate salt, diazonium organic matter, methyl alcohol and water mixed solution, it is characterized in that: in described step (1), the number of theoretical plate of reaction side line rectifying column is 47, material inlet position is at the 41st block of plate, lateral line discharging position is at the 13rd block of plate, and recycle feed mouth position is at the 36th block of plate.
5. continuous external circulation reaction side line rectifying according to claim 1 and 2 and liquid-liquid extraction combine the method for process sodium and ammonium acetate salt, diazonium organic matter, methyl alcohol and water mixed solution, it is characterized in that: in described step (1), alkali lye is 50wt%NaOH solution, and the mass ratio of material liquid and 50wt%NaOH alkali lye is 1: 0.146.
6. continuous external circulation reaction side line rectifying according to claim 1 and 2 and liquid-liquid extraction combine the method for process sodium and ammonium acetate salt, diazonium organic matter, methyl alcohol and water mixed solution, it is characterized in that: in described step (2), extractant with containing sodium acetate, diazonium organic matter and aqueous mixtures feed weight ratio is: 0.4 ~ 1.2: 1.
7. continuous external circulation reaction side line rectifying according to claim 1 and 2 and liquid-liquid extraction combine the method for process sodium and ammonium acetate salt, diazonium organic matter, methyl alcohol and water mixed solution, it is characterized in that: in described step (2) multiple stage of countercurrent liquid-liquid extraction method, multiple stage of countercurrent liquid-liquid extraction tower number of theoretical plate is 4, and operating temperature is 10.5 ~ 29.5 DEG C.
8. continuous external circulation reaction side line rectifying according to claim 1 and 2 and liquid-liquid extraction combine the method for process sodium and ammonium acetate salt, diazonium organic matter, methyl alcohol and water mixed solution, it is characterized in that: in described step (3), flash column operating pressure is 0.10 ~ 0.15*10
5pa, tower top and the temperature at the bottom of tower are respectively 52.1 ~ 56.7 DEG C and 87.3 ~ 88.9 DEG C; Flash column number of theoretical plate is 5, and feedstock position is at the 3rd block of plate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510138385.2A CN104874196B (en) | 2015-03-26 | 2015-03-26 | A kind of method processing sodium and ammonium acetate salt-diazonium Organic substance-methanol-water mixed solution |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510138385.2A CN104874196B (en) | 2015-03-26 | 2015-03-26 | A kind of method processing sodium and ammonium acetate salt-diazonium Organic substance-methanol-water mixed solution |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104874196A true CN104874196A (en) | 2015-09-02 |
| CN104874196B CN104874196B (en) | 2016-09-14 |
Family
ID=53942032
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510138385.2A Active CN104874196B (en) | 2015-03-26 | 2015-03-26 | A kind of method processing sodium and ammonium acetate salt-diazonium Organic substance-methanol-water mixed solution |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104874196B (en) |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105417815A (en) * | 2015-11-06 | 2016-03-23 | 南京师范大学 | Method for treating salt-containing organic wastewater during production of cationic golden yellow dye X-GL |
| CN108059291A (en) * | 2017-10-26 | 2018-05-22 | 淄博鑫泉医药技术服务有限公司 | The recovery method of DMF and inorganic salts in cefotaxime side chain acid esters waste water |
| CN112499868A (en) * | 2020-11-30 | 2021-03-16 | 安道麦安邦(江苏)有限公司 | Method for recycling pymetrozine concentrated mother liquor |
| CN113968782A (en) * | 2021-11-24 | 2022-01-25 | 南通醋酸纤维有限公司 | Method for removing impurities in recycled acetic acid |
| CN114288699A (en) * | 2021-12-02 | 2022-04-08 | 徐州砥研医药科技有限公司 | Rectification device for preparing benzene-containing medical intermediate and working method thereof |
| CN116999883A (en) * | 2023-08-07 | 2023-11-07 | 江苏诺恩作物科学股份有限公司 | System and method for producing dichlormid |
| CN116999883B (en) * | 2023-08-07 | 2024-04-19 | 江苏诺恩作物科学股份有限公司 | System and method for producing dichlormid |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63156744A (en) * | 1986-12-22 | 1988-06-29 | Toray Ind Inc | Recovery of acetic acid |
| CN101148407A (en) * | 2007-10-16 | 2008-03-26 | 南京师范大学 | Method for extracting ethyl acetate from ketoconazole production by continuous side line discharging method |
| CN101148398A (en) * | 2007-10-19 | 2008-03-26 | 南京师范大学 | Method for separating Ethylene glycol monomethyl ether, methanol and water by rectification and azeotropy |
| CN101759569A (en) * | 2010-01-12 | 2010-06-30 | 南京师范大学 | Method for extracting high purity para-nitrochlorobenzene and ortho-nitrochlorobenzene by synthesis method of multistrand side track discharging rectification and continuous crystallization |
| CN203090515U (en) * | 2013-02-06 | 2013-07-31 | 南京师范大学 | External circular-reaction extractive distillation integrated device |
| CN103772230A (en) * | 2014-02-13 | 2014-05-07 | 南京师范大学 | Method for separating mixing solution of sodium salt, dimethyl formamide, methylbenzene and water through integration of azeotropic/extractive distillation and liquid-liquid stratification |
| CN103880786A (en) * | 2014-03-18 | 2014-06-25 | 南京师范大学 | Method for recovering useful constituents in mixed waste solvent during glufosinate ammonium production process |
-
2015
- 2015-03-26 CN CN201510138385.2A patent/CN104874196B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS63156744A (en) * | 1986-12-22 | 1988-06-29 | Toray Ind Inc | Recovery of acetic acid |
| CN101148407A (en) * | 2007-10-16 | 2008-03-26 | 南京师范大学 | Method for extracting ethyl acetate from ketoconazole production by continuous side line discharging method |
| CN101148398A (en) * | 2007-10-19 | 2008-03-26 | 南京师范大学 | Method for separating Ethylene glycol monomethyl ether, methanol and water by rectification and azeotropy |
| CN101759569A (en) * | 2010-01-12 | 2010-06-30 | 南京师范大学 | Method for extracting high purity para-nitrochlorobenzene and ortho-nitrochlorobenzene by synthesis method of multistrand side track discharging rectification and continuous crystallization |
| CN203090515U (en) * | 2013-02-06 | 2013-07-31 | 南京师范大学 | External circular-reaction extractive distillation integrated device |
| CN103772230A (en) * | 2014-02-13 | 2014-05-07 | 南京师范大学 | Method for separating mixing solution of sodium salt, dimethyl formamide, methylbenzene and water through integration of azeotropic/extractive distillation and liquid-liquid stratification |
| CN103880786A (en) * | 2014-03-18 | 2014-06-25 | 南京师范大学 | Method for recovering useful constituents in mixed waste solvent during glufosinate ammonium production process |
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105417815A (en) * | 2015-11-06 | 2016-03-23 | 南京师范大学 | Method for treating salt-containing organic wastewater during production of cationic golden yellow dye X-GL |
| CN108059291A (en) * | 2017-10-26 | 2018-05-22 | 淄博鑫泉医药技术服务有限公司 | The recovery method of DMF and inorganic salts in cefotaxime side chain acid esters waste water |
| CN108059291B (en) * | 2017-10-26 | 2020-09-04 | 山东鑫泉医药有限公司 | Method for recovering DMF (dimethyl formamide) and inorganic salt in ceftazidime side chain acid ester wastewater |
| CN112499868A (en) * | 2020-11-30 | 2021-03-16 | 安道麦安邦(江苏)有限公司 | Method for recycling pymetrozine concentrated mother liquor |
| CN113968782A (en) * | 2021-11-24 | 2022-01-25 | 南通醋酸纤维有限公司 | Method for removing impurities in recycled acetic acid |
| CN114288699A (en) * | 2021-12-02 | 2022-04-08 | 徐州砥研医药科技有限公司 | Rectification device for preparing benzene-containing medical intermediate and working method thereof |
| CN116999883A (en) * | 2023-08-07 | 2023-11-07 | 江苏诺恩作物科学股份有限公司 | System and method for producing dichlormid |
| CN116999883B (en) * | 2023-08-07 | 2024-04-19 | 江苏诺恩作物科学股份有限公司 | System and method for producing dichlormid |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104874196B (en) | 2016-09-14 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104874196A (en) | Method for processing sodium and ammonium acetate-diazonium organic compound-methanol-water mixed solution | |
| CN105001087A (en) | Method and apparatus for producing formic esters by comprehensively utilizing metronidazole hydroxylation synthesis wastewater | |
| CN105417815A (en) | Method for treating salt-containing organic wastewater during production of cationic golden yellow dye X-GL | |
| CN103992206B (en) | The method and system of prenol are prepared in a kind of ester exchange | |
| CN107311878B (en) | Device for recycling glycine waste liquid and method for recycling glycine waste liquid | |
| CN108128826B (en) | Nitric acid-containing wastewater treatment device and treatment method | |
| CN104193751A (en) | Method for treating mother liquid discharged in glycine production | |
| CN104761452B (en) | A kind of purification process of butyl acrylate coarse product | |
| US20160185711A1 (en) | Process and Device for Recycling Waste Acid Produced in Process of Producing Zoalene | |
| CN106008186B (en) | A kind of separation method of isopropanol, acetone and water mixed solution | |
| CN102530893B (en) | Nitric acid extraction and concentration method | |
| CN104193634A (en) | Method for separating mixed crystals of glycine and ammonium chloride | |
| US11767304B2 (en) | System and method for continuously preparing furfural using lignocellulosic raw material | |
| CN108658051A (en) | Recovery method, device and its sulfuric acid of recycling of nitrating wasting acid | |
| CN103214045A (en) | Furfural wastewater treatment method | |
| CN103304442A (en) | Process for synthesizing diacetylmonoxime ethyl ether by continuous reactions in microtube | |
| CN105859580A (en) | Novel process for recycling sulfuric acid in production of 2-cyano-4-nitroaniline | |
| CN104844416A (en) | Method for multistage extracting and absorpting dichloromethane and monochloroacetone in MCPa synthetic tail gas | |
| CN109607915A (en) | A kind of processing method of Benzotriazole Ultraviolet Stabilizer production waste water | |
| CN102107924A (en) | Method for comprehensively recovering and treating furfural industrial wastewater | |
| CN111533683B (en) | Method and device for preparing vinyl pyridine by continuous dehydration of hydroxyethyl pyridine | |
| CN105329864A (en) | Resourceful treatment method of waste acid solution in nitrobenzene production process | |
| CN102731299A (en) | Liquid-liquid extraction separation method of methyl propionate-methanol-water azeotropic system | |
| CN102659515A (en) | Method for recovering 1,4-butanediol from waste liquor generated in production of 1,4-butanediol through Reppe method | |
| CN106831336B (en) | Ethyl alcohol and the recycling of hydrazine hydrate mixed liquor and circulation utilization method in a kind of production of pyraclostrobin |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| EXSB | Decision made by sipo to initiate substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |